A Handbook for Cane-Sugar Manufacturers and Their Chemists 1000763605

1 HANDBOOK A CANE-SUGAR MANUFACTURERS IMD THKUI CHEMISTS. l: GUILFORD 7AiV Chemui in Chargt of JPENCEE, The

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1 HANDBOOK

A

CANE-SUGAR

MANUFACTURERS IMD

THKUI

CHEMISTS.

l:

GUILFORD 7AiV

Chemui

in

Chargt

of

JPENCEE,

The Manujjaeluret

D.So.,

Cuban-Ameriean

(Chaparra^DHicias, Tinffuaro, Conataneia, MercedUat and Vniaadt CardenoB Oramercy Refineries); Formerly

Company

Chief of Suffor Laboratory^ U. S. Department if AgriaUturt, WaahingUm, etc.

SIXTH

EDITION,

SECOND

ENLARGED,

IMPRESSION, TOTAL

ISSUE,

NEW

JOHN

WILEY

London:

CHAPMAN

TEN

CORRECTED. THOUSAND

YORK:

" "

SONS,

Inc.

HALL,

Limited

Sugar

Copyright,

1916.

1905.

1889,

1917,

BT

JOHN

WILEY

PRfeM

"RAUNWORTH

sM

BOOK

Inc.

SONS,

"

OF

*

CO.

MANUFAOTURCBe

"ROOKLVN,

N.

V.

^

I

" I

9

DEDICATED IN

BONOB

GRATTTUDB

AND TO

M.

CH.

GALLOIS AND

M.

DUPONT

FBAN9OIB PAST

PRESIDENTS OF

ABSOaATION

CHIMISTES

DES BT

THE

THE

AUTHOR

411603

DE

FBANCB

/"

edition is enlargedto include

This

EDITION.*

SIXTH

THE

TO

PREFACE

a

chapteron Evaporation

Heating, by Prof. W. H. P. Creighton,Dean of the Department of Technology, The, Tulane University, Prof. Creighton's long experience as an New Orleans,La. States Navy, and in teachingin the officer in the United engineeringdepartments of Purdue and Tulane Universities, and

has

Juice

eminently fitted him

I extend

A

thanks

my

for the

this article.

to him.

have been

errors typographical

few

preparationof

slightchanges have been made clearly. descriptionsmore

to

corrected and

bring out certain

some

process

G. L. Spsnceb.

Mass., 1917.

Cambbidob,

PREFACE

The

THE

TO

FIFTH

EDITION.

section devoted to ijiemanufacture

enlargedin of

this edition. raw,

The

processes

plantationwhite

and

in

has been greatly use

in the

refined

facture manu-

sugar

are

described.

Through the courtesy of Mr. George P. Meade, Superintendent Cardenas the include of (Cuba) Refinery,I a control as is practised and refinery chapter on sugar refining in the United The

book

States. has been

largelyrewritten.

has been revised to meet factories and

now

in

operation.

several of the older

ones

The

chemical

tion sec-

the conditions of the very large Additional tables are included have

("eenreplaced by

recent

tables. G. L. Spenceb.

Washington, D. C, 1915. "",

vii

'

i

r

PREFAC3E

edition

first

The

few

been

book

with

industry in

available

a

addition

to

of

control

proper

requires

knowledge a

of

of

of

chemical

this

the

cane-

is

book.

this

by

methods

training.

of

this

For

manufacturing

the

of

material

more

sugar-factory

a

little

branch,

in

much

that

result

when

but

engaged

now

time

a

and

concerning are

the

at

chemists

English,

preparation

the

written

was

employed

chemists

Many

The

this

in

written,

sugar-work.

sugar

of

EDITION.

FOURTH

factories

cane-sugar

had

THE

TO

processes

chemist

the

in

manufacture,

reason

a

is

included

of

manufacture

brief

scription de-

in

this

edition.

With

the

and

the

sugar,

competent

the

large

past

few

increase the

years,

tendency

in

toward

whether

raw

chemist

or

in

the

scale

complexity

greater the

the

of

production

refined,

factory

the

of

of

becoming

processes,

grade

one

necessity is

ing dur-

having generally

recognized. G.

WAsmNOTOir,

D.

C,

1005.

L.

Spencer.

of

a

r

r

CONTENTS,

MANUFACTURE

CANE-SUGAR

OF

FAcn

R"w

Material

Extraction Steam

1 the

of

Plant

Outline

of

Juice

and

Fuel

Raw

Purification

32

Sugar

of

0

:

the

Manufacture

36

Juice

38

Defecation

and

Defecation

using

Closed

Heaters

and

Open

Defecation

using

Closed

Heaters

and

Closed

Clarification

Sulphitation

Process

Sulphitation

after

Carbonation

Processes

Harloff's

Acid

Sulphur

Stoves

Carbonation

of

Tanks

Open

39 Settlers

43

Settlers

45

Louisiana

47

Liming

49 50

'.

Thin-juice and

55

Process

Sulphitors

58

Tanks

60

Kilns

Lime Filtration Chemical

61

Processes

and

Reagents

used

Evaporation

of

Preservation

of

Boiling

the

in

Purifying

63 the

Juice

72 77

and

Juice

Sirup

83

Sugar

85

Sugar

86

Crystallization and

Purging

Machinery

Juice

of the

Crystallization

in

Motion

94

the

99

Curing

Classification

of

Raw

Classification

of

White

Deterioration

of

Sugars

of

Warehousing Sugar

in

Raw

Sugar Sugars

102

.'

Sugars

103 103

Sugars

103

Refining

Raw

106

Materials

107 109

Defecation

!

Filtration Char

112

115

Revivification of

Crystallization Drying Technical

and

the

Finishing and

Chemical

118

Sugar the

120

Products

123

Control XI

CONTENTS.

XU

SUGAR

ANALYSIS PAQB

Sugars

and

Optical

other

Constituents

Methods

of

of

Sugar

the

Cane

and

Analysis

Its

Products

134 141

^ "

Chemical

Methods

of

Density

Determinations

General

Analytical

109

Averaging

199

of

the

Sugar-cane

Analysis

of

the

Juice

Analysis

of

Sirup,

Analyras

of

Sugars

Analysis

of

Filter-press

Analysis

of

Bagasse

and

Analysis

of

Factory

Wastes

Analysis

of

Molasses

214

:

221

Massecuites

and

Molasses

259 274

;

and

Cake

280

of

Sugar-house Evaporating

and

282 294

Cattle

Calculations

Chips

Exhausted

Food of

Applications

Control

Chemical

187 191

Analysis

Definitions

Analysis

Work

and

Sampling

Sugar

298

used

Expressions

in

Sugar

Work

Sugar-house

Work.

301 310 340

Juice

Heating

350 ,

of

Purchase

Analysis

of

Quality

on

Limestone,

a

Basis

Lime,

of

its

Sulphur

Analysis

382

and

Sulphurous

of of

Flue-gases the

Reference

Reagents Tables

386 390

Water

403

Supply,

Treatment

of

Fermentation

Special

Acid

Oils

Lubricating Analysis

Cane

\

Impure

Water

407

".

409 410 423

LIST

ILLUSTRATIONS.

OF

PAGB

VlGTTRa

Central

Delicias,

1.

Cane-shredder

2.

ProntUpiece

Cuba

10

Krajewski

Crusher

11

3.

Krajewski

Crusher-roll

11

4.

Fulton

Crusher

12

5.

Fulton

Crusher-rolls

12

6.

Puunene

Housing

13

7.

Fulton

8.

Meiaschaert's

9.

Mill

Housing

14

\

Grooves

Juice

16

Settings

10.

Diagram

11.

Draw-down

12.

Diagram

13.

Vivien

14.

Sulphur

18 Saturation

Compound

of

for

Pipes

20

Defecators

44 ^

Closed

Deming's

of

Settling-tank

46

Tube

56

Stove

15.

KeUy

16.

Sweetland

17.

Hersey

18.

Nicol

19.

Half-shadow

59

Press.'!

Filter

Filter

68

Press

69

Granulator

121

(diagram)

Prism

141

Compensating

Single

Compensating

20.

Double

21.

Half-shadow

Polariscope

Polariscope (Josef

Polariscope

(Schmidt

143 "

Haensch)

144

Jan-Fric)

146 ,.,...

22.

Half-shadow

23.

Triple-field Polariscope

24.

Arrangement

(Julius

Polariscope

of

Peters)

147 148

in

Prisms

Triple-field

Polariscope

(diagram)

149 .

..

Polariscope

25.

Laurent

26.

Compensating

27.

Transition

28.

Cane-sugar

150

Attachment Tint

for

Laurent

Polariscope.

151

Polariscope

Scale,

152 Scale

Ventske

154 ^

29.

Control

Tube

for

30.

Polariscope

Tubes,

31.

Polariscope

Tube

32.

Bates'

33.

Polariscope

34.

Pellet's

Continuous

35.

Pellet's

Continuous

36.

Landolt's

Polariscope Tube

Polariscopes Ordinary with

158 Forms

158

End

Enlarged

159

Tube with

159

Tubule

Side

Polariscope

160

Tube

160

.

Tube,

Modified

Form

161 ._

Inversion

Tube

162 ,.

37.

Wiley's

Desiccator

Caps

for

Landolt's

Tube

162 ^

,

"

"

"

LIST

XIV

OF

ILLUSTRATIONS.

flOUBB

38.

PAGS

Sugar

40.

Capsule FilteringDevices Sugar Flasks, Diagram

41.

Pellet's Conical

42.

Sugar Balance

43.

Decimal

44.

Balance

45.

Norma

46.

Brix

39.

166 166 ^

of

Types

167

Flasks

168 170 ,

Balance for Rough Alcohol

Weighings

173

49. 60.

Calumet

48.

172

Stove

Hydrometer Reading the Hydrometer Westphal Balance Pyknometers

47.

171

."

193 ,

Scale

193 ,

195 197

Sampler '51. Coombs* Drip Sampler 52. Horsin-Dton's Sampler 63. Press-cake Sampler 54. Sample Box for Sugar

203

Trier

213

205 206 209 212

66.

Sugar

66.

Hyatt Cane-reducer

57.

Extractor

58.

Vacuum

Drying

Apparatus

69.

Vacuum

Drying

or

60.

Abbe

61.

Immersion

62.

Sugar

63.

Sucrose

64.

Funnel

,

214

for Use

in Fiber

Tests

218 223

Distilling Apparatus

224

Refractometer

227

Refractometer

228

Refractometer

229 231

Pipette for Alundum

Holder

65.

Sargent's Alundum

66.

Filtering Apparatus.

Crucible

67.

Alcohol

68.

Current

69.

Soxhlefs

Crucibles

238

Holder

238 239

Burner

241 for

Regulator

ElectrolyticWork

243

Filter Tube Burette

70. Squibb's Automatic and

Knorr

244 248

Tubes

Filter

248

71.

Wiley

72.

Muffle

for Incinerations

255

73.

Muffle

for Incinerations

255

74.

Muffle

for Incinerations

75.

Apparatus

for

76.

Inversion

Flask

77.

Karcs's

78.

Kohlrausch

79.

Bagasse

80. Bagasse 81. 82.

Volume

262 269

."

Apparatus

for

Crystal

Content

Flask

with

271 281

Chopper, Boot Chopper,

of Massecuite

"

Krantz

Athol

283 283

Induced

Draft

285

Bagasse

Oven

Bagasse

Oven

288

Digester

290

Digester, Norris

291

83. Bagasse 84.

255

Weighing a'Unit

Bagasse

85.

Knorr-Soxhlet

86.

Hors6n-D6on's

Extraction Control

Apparatus Device

298 318

LIST

ILLUSTRATIONS.

OP

XV m

FIOVBB

PAOB

87.

Lftboratory

88.

Massecuite

89.

Diagram

326

CeHtrifugals Funnel

(CobensI) of

90.

Diagram

91.

Vacuum

Pan

92.

Vapor

Distribution

93.

Elevation

94.

Knorr's

95.

Schroetter's

96.

Engler's

97.

Orsat's

of

CO2

Calculating

for

Effect

Multiple

"

Molasses

Mixtures

Evaporator

326 347 355 356

in

Effect

Multiple

a

Horisontal

T3ri)e

of

Evaporator

358 359 392

Apparatus Alkalimeter

393

Viscosimeter

Gas

the

Separating

for

400

404

Apparatus .

.

.

^

)

/

THE

MATERIAL.

RAW

Sugar-cane.

1.

is

Cane

"

The

Saccharum.

genus

sterile. the

The

recent

have

arrows

been

conditions.

freely every

in Louisiana

with within

believed

were

the

varies Until

blossoms

or

not

noted

growth

its flowers

years

then

its

of

cultural

plant "arrows"

Tropics and

large grass, belongingto

a

mode

variety, climate, soil and comparatively

CANE-SUGAR.

OF

MANUFACTURE

be

to

usually only in A

year.

few

very

exceptionallymild

in

years.

Large numbers stations new

varieties.

and

with

in various The

parts of the world

seedUngs

are

crossed

which

are

for

now

in broad

in the

with

resistance

search

other

for

seedUngs

in several varieties

resulted

culture.

The

varieties

new

particular qualities such

some

ment experi-

teristics. develop certain charac-

to

experiments have

in

produced

now

existingvarieties in order These

selected

seedlingsare

of

as

are

richness

in

disease, persistence of type, time of The most ripening, milling qualities,fuel value, color, etc. sucrose,

extensive of the

seedling varieties

of

use

old varieties

It is

to

generally believed freely is

cane

arrows

cane,

however, is often

sugar

content.

months

deteriorates

begins. plant

The

grows

in Cuba

usually

very

rich

regards

yield of

the

cane,

littletaller and

in

in its

flowering, and, as

that

not

It increases

after

Java.

There

few

in which

the

cultivated.

now

are

is in

as

^*ery sucrose

sucrose

year

productive. content

for several

with

other

when

the

rainy

however,

may

after

Such

an?l of low invert-

is true

sugar

heavier

a

canes, season

small,since flowering. be

the

2

MATERIAL.

RAW

"

Sugar-Ksanevaries greatlyin richness in differentcountries and

in the

even

attain

even

a

It does

country.

same

of 17 per

content

sucrose

cent

surpassed in other countries.

is sometimes

containing

12

of

cent

per

often exceed

not

in

Cuba, but this

A

cane

iana in Louis-

is considered

sucrose

or

very

rich.

Sugar-cane is propagated by located

nodes.

the

at

planted with

a

Pieces

that

cuttingsof the

or

covering of soil

shallow

very

of the buds

means

cane

are are

in certain

or

only partly covered, but in this latter event irrigated.Each bud produces a plant and from each of

localities are

these

are

there

clump

several

are

stool of

or

shoots

or

The

cane

canes.

These

suckers.

form

a

suitable soil and

under

in several usually planted but once New "ratoons," spring up from the plants, termed years. stubble,after harvesting the crop, and produce a second climatic

conditions

and

crop

Fiscal

on.

so

limit the crop two

or

is

to

soil and

or

climatic

"plant-cane"

or

to

conditions

times some-

plant-caneand

one

ratoons.

Dark-colored

usually produced in sub-tropical the light-colored, greenish or yellow canes r^ons.and in the Tropics. The Tropics,however, will produce canes of is the "cristalina" variety. The usual Cuban cane any variety and is of a lightcolor. Normal

They and

varieties

sugar-canes

are

are

hollow

never

partially so.

or

contain

approximately from 87 to 90 per cent of juice uents some water, in composition with certain plant constitlittle or (colloid water), that contains no sugar.

Canes other of such

that

abnormal

ar"

conditions

are

on

climatic

some

hollow, but

sometimes

is usually very

cane

of

account

the

or

proportion

small.

The

with the approach of cool or dry weather. plant matures Harvesting usually begins long before the cane is considered to be ripe, in order to obtain If a long working season. the factory is in an irrigateddistrict, the distribution of water is suspended a few weeks before the cane is to be harvested, to

promote

increases

and

ripening. The the

reducing approaches maturity. The

stalks

are

cut

sucrose

sugars

off close

to

content

of

decrease

as

the

ground

the the

stalks

plant

in harvest^

4

HAVf

MATERIAL. "

be harvested

by burning, but it must loss

The

The

includingfive days

but

in the

The

purificationof the juice is with of the

carbon

with

as

in

cane

to

up

from

the

price,

it at

any

time.

plished usually so readily accomfaces cane, and the heating-sur-

not

sound

foul

evaporator

refuse

may

rain

agrees

burned

deduction

without

of rainfall he

burned

should

manufacturer

receive

to

and

event

ing. by the burn-

is greatlyincreased

rate of deterioration

fall upon the burned cane. Cuban most contracts cane

The

sooner.

particlesof

fine

persist through the manufacture in the sugar. It is preferableto grind

and

sometimes

finallyappear of sound

and

burned

alone, since the mixed The

method

with

local

their

cane

juicesare

in

carts

at

all in Cuba.

small

railway in Cuba in the Island

The

in bullock

of Hawaii The

in punts.

burned

cane

to the

cane

factory varies

factories

Small

or

ture mix-

a

readilypurified.

more

of transport of the conditions.

than

rather

cane

largelyused in the Hawaiian not

is accelerated

through deterioration,which

to avoid

promptly

very

usually transport Portable railways are

cars.

Islands is

cane

and

in

brought

Java, but almost to

the

factory

or

It is

carts.

and

in British

use

of flumes

the

the factories fiumedj" ported transGuiaiJS^|nisually and

complicates ptu^is mills. jui3B|^the

estimating of the percentage yield of Inferential methods, based the analyjpHKjthe cane upon ^en become the weight of the latter,may and juice and

necessary.

Sugar-cane is usually sold to

its richness to devise a

upon

The of

in sugar an

or

to

the

the factories without

regard

cult purity of its juice. It is diffi-

equitablemethod

for the

purchase of

cane

basis of its

analysis. (See page 382.) following table showing the composition of the stalks

Louisiana

December,

cane

at

is inserted

the

time

of

through the

harvesting, Novembercourtesy

of Dr.

C.

A.

of the New York Sugar Trade Laboratory Browne, Chemist and formerly of the Louisiana Sugar Experiment Station. The figuresare condensed from many analyses of the purple The varies composition of the cane variety of the cane. climatic conditions, character of the soil, with of manner fertilization and and its cultivation,the age of the cane

variety:

SUGAR-CANE.

COMPOSITION

OP

Wa""r.

SUGAR-CANE.

LOUISIANA

74.60%

74.60% SiUca.

Si02. Potash. KjO

Ash.

0.25 0.12

Soda"Na^

0.01

Lime.

0.02 0.01

CaO

Magnesia, ACgO Iron, FeaOa Phosphoric acid, P^" Sulphuric acid, SOs.

O.fiO

Trace 0.07

0.02 Trace

Chlorine, Q.

Fiber.

Cellulose Pentosans.

10.00

14.00

Siiears

6.60 .

i Xylan fAiaban

"

(Cane-gum) Lignin bodies, etc

2 .00 60

2.00

Sucrose Dextrose

12. 60

(

90 60

Levulose

Nitrogenous bodies 06%) (Total N-.

0.40

.

Fat and wax. Pectin (ffums). Free adds Combined acids. .

..

..

that

.

the

.

0 .

20

0.01

T^ace Trace 0.20

0.20 0.08

0.20

(Malic, succinic,etc.) ) " *"

"*

0.08

""

0.12

100.00%

juice of

0^ 12 0.07

0.20

0.12

Total

The

Albuminoids Amids (as asparagin) acids (as aspartio) Amido Nitric acid Ammonia bodies Xanthin

cane

100.00%

contains

nitrogenous substances

objectionable in the manufacture. ^ isolated Fritz Zerban asparagin,glutamin and tyrosin. A part of the asparagin and a stillgreater part of the glutamin are

more

broken

are

up

or

less

in the manufacture

the result that asparin the molasses along with

with

glutamic acids accumulate undecomposed asparagin and glutamin. These amids are given off during the largely responsible for the ammonia are evaporation of the juice. Acid amids and aminoacids positivemolasses-makers. A small amount of cane-gums (pentosans) and of fat and find their way into the juice during milling;these together wax with the pectin acids and nitrogenous bodies make up the organic solids,not sugar of the juice. The of amount these organic impuritiesdepends upon the age and variety of tic and

the

cane

Their and

and

also

upon

the

pressure

of

the

mill-rollers.

higher in the juicefrom the second in the juice from the first mill;* their

percentage is much third mills than Int. Congress

Chem.

8, 103.

*

Eighth

s

Cane-sugar, Prinsen-Geerligs,2d edition, 31.

1904, 3S, 49.

App.

Browne,

La.

Planter,

b

RAW

MATERIAL.

sion-batter higher in the juicefrom the diffu-

relative percentage is also than

in

mill-juice. The fat and of albuminoids, and part of the gums amount removed during the clarification. Hie

the

purityof

of the

content

sucrose

juicevary that

purity than exists between NoSl

the

has

on

"Uid upper

the

following table

three

for

similar

A

lower

difference

halves of the stalk. the

canes,

in each

sucrose

and

content

intemodes.

the

percentage basis. ^

a

juiceare

also the coefficient of

sucrose

analyzed whole

has referred

cane

is of lower

the lower

Deerr

node, and whole

of

of the

greatly in different parts of the stalk.

juice of the nodes

The

and

cane

the greater

wax,

His

varieties

pith, rind and to that

part

in the

figuresare

given in

of Hawaiian

canes.

using these figuresit should be considered that the separation into pith,rind and node can be made approximately only:

In

The

cane

contains

coloring matters

anthocyanin and saccharetin insoluble

such

of Steuerwald.

'

as

chlorophyll,

Chlorophyllis

is therefore

in the readily removed purificationof the juice. Anthocyanin is precipitatedin the in the carbonaof excess of lime, hence is removed presence tion process. It is partiallybleached by sulphurous acid. charetin Anthocyan ' is very soluble and decomposes rapidly. Sacin water

and

is present in the

Steuerwald lime and

and

it turns

fiber of the

yellow and

oliier alkalis and

cane.

to

is soluble

is not

in the presence of altered in the carbonation unites

Saccharetin

processes. sulphitation

According

with

iron to

Such saccharetin is as intensely black compound. of juice passes through all the processes present in the raw

form

an

30, Haw.

1

Bui.

"

Int. Sugar

*

C.

Sugar

Journ.,

Mftller, Bull.

Planters'

14,

Assoc,

Exp't Sta.,

36.

53.

des

Chimistes

de

France,

31, 849*

f

and

manufacture

7

SEASON.

MANUFACTURING

in

finallyappears

the

molasses.

Sao-

prevented from entering the manufacture by thoroughly strainingthe juice as it flows from the mills and by the non-use of alkaline imbibition water. Sugar-cane usuallycontains three sugars,^sucrose/ dextrose and levulose (d-Fructose,Fruit sugar). The dextrose and levulose are plant in nearly present in the very immature charetin

should

be

these equal proportions, i.e., in the proportionsin which is inverted by acids. As the formed when sucrose are sugars the levulose

matures

cane

iisappears. Levulose This

molasses. the dextrose

again always

its solutions

sometimes

however, in the isomeric changes in

to

heated

are

and

appears,

is due

reappearance

when

decreases

content

in the presence

of

earths, notably potassium of Cuban salts. The content cane-juice, reducing sugar the "glucose" in the cane levulose and dextrose,termed alkalis and

salts of the

alkaline

between 0.4 and 1.35 per cent. industry, usually ranges almost or quite absent The reducing sugars are sometimes from cane-juices. This condition existed for several weeks in the writei's experienceat Magnolia Plantation, season one Louisiana.

The 0.25 of the ash

K3O, about

25

The year

able. cane-juiceis quitevaritween in the author's Cuban experience is berange and 0.6 per cent in the juice. The composition is also very variable. Potassium, figuredas potash, from abundant the most constituent,ranges

mineral

The

ash content

or

to 45 per

cent

of the

of the ash.

composition of the ash .of the juice also varies from be noted in the table on page 8, colto year, as may "A":

unms

Season. The season begins at Manufacturing In the greatly varying^dates in various parts of the world. almost rainless districts where ing irrigationis practised,grindbe prosecutedduring nearly or quite the entire year. may %.

This The

"

is true

not

Pellet been

France,

in parts of the Hawaiian

and

Peru

Islands.

begins in October and November and lasts through December and often into Jan-

of manufacture

season

in Louisiana 1

in

reported raffinose in confirmed

14, 139;

see

by

other

also

Deut.

cane

chemists

but

its

presence

(Bull. Assoc,

des

Chimistes

molasses,

Zuckerind., 9(3, 1439).

has de*

8

RAW

ANALYSES

OF

MATERIAL.

THE

of

(Percentages

and

Factory

Crop

CUBAN

OF

ASH

CANE

JUICES

Ash)

the

Year

B .

.

(1912) SiOs

Silica,

and

Iron

6.46

Alumina,

FesOs^

AliOj

3.00

CaO

Lime,

4.70

MgO

Magnesia,

5.01

KsO

Potash,

46.28

Na"0..

Soda,

1.36

PiOt.

Add,

Phosphoric

4.21 .

.

Chlorine,

CI

Carbonic

Acid,

in

COt

northeast

is

months,

the

of

nearly The the

a

with

the

of

the

with

the

its growth

This

the

the

on

count ac-

ian Hawai-

The

about

The

dry

six of

parts

many

the

during

the

factories

monsoon,

or

corresponds

in

determines

season

the

expense

The

Tropics. of

transportation at

parts

very

season.

rainy

period

of

season.

November.

Argentine

advent

in

longer

grind

in

continues

and

the

grinding

months.

following

of

interruption

frequent

uary Jan-

though

longer

even

with

much

into

May

June,

conditions

Indies

East

or

in

period

manufacturing until

the

and

Cuba

in

November

very

manufactunng

interfere renew

in climatic

permit Dutch

and

May

though

about

from

Cuba,

begins

season

usual

September

of in

December

December

into

rains

in

The

from

coast

of

Islands

begins

Rico,

Porto

continue

may

10.53

season

Indies

West

4.08 12.90

The

uary.

.

SOt

Acid,

Sudphuiic

of

the

its

cane,

sucrose

the rains but

close not

cause

content.

of

only it

to

EXTRACTION

Milling

3.

is unloaded in

devices

from

in

are

Where

the

in

little These

and

a

the

In

devices

platform

the

onto

and

dumping

Cuba

in

unloading

capacity

the

to

and

time

a

with

using

The

in

time

of

are

device.

this

factories

using three devices

Dumping the

cane

general types upon

discharged

a

the

These

carrier.

factories from

the

and

cars

or

of

which

to

breakage

of

a

bundles

the

favor

in

the

cane

load, in with

a

occasions

often the

of

arrangement

less end-

drag the

provided

yoke,

cane

heavy

are

However,

of

it is carried

under

passed

are

usually

car-load

a

which

arms

employed

hoists

The

elevators

with

hoists

of

use

railway

in

tracks

milling plants. great

quickly and

with

are

of

dumping

platform,

endwise

the

from

hopper

in

of

railway

again used

generally

third

attached

is little loss

there

carriers

or

are

cane

very

a

method.

simplifies the

greatly

cart

upon

carts.

or

cables

or

hoist, and

a

half

a

are

and

intervals

at

Chains

them.

tripping loss

fitted

pulling the

cars

elevators.

by

in the

Louisiana

many

devices

drop it into

mills

chains,

for

lift

to

in

or

large piles for the

derricks

same

cars

termed

in

or

but

carrier.

Hoists

a

form,

placing it

in

used

are

in Java

extent

some

and

cane

such

used.

the

from

conveyors,

the

case^

of

often

are

cane

interruption

prevent

the

Raking

their

to

latter

up

have

run

to

derricks

endless

devices

deteriorates

cane

lift the

to

cane

factories.

the-

Louisiana,

upon

according

picking

in

at

in

as

and

^The

"

forms

Many

factory.

is cool

climate

Cane.

mechanical

especially in Cuban

use,

or

the

by

carts

modem

deposit it

service.

to

and

cars

JUICE.

THE

Unloading

"

usually arranged

are

night work,

in

the

storage,

elevators

or

Processes.

well-equipped

the

carts

OF

cane

minimum

in

devices.

which

through

a

is then a

Cuba.

of labor.

transit. In

the

tilted

swinging

door

There one,

charge dis-

They

ther, Furtwo

are

the

car

is

and

the

load

into

the

hopper 9

is

10

EXTRACTION

"

elevator.

of an

wise. and

The

when

points

when

the

in the

cane

The

due

the fields and

in

to the

the of

3-roller mills.

The

the

prepare

and

structure

the

cylinders. is required It is

position. tor

handling

delivered

to the

of the cut

mills.

to the

cane

The

sun

in

large.

and crusher

in or

used

are

expressing shredder

and

for milling case

it to tilt

causes

first used

at

industry.

crusher

in the

level

ployed em-

by

and

shredder

of the crusher,

three arc

breaking

exclusively

juice.

its

These

or

more

designed

down

the

to

hard

extra.ctinga part

of

juice.

The was

cane

a

released

is hinged

pressure

Multiple-mills

"

top

is usually

hydrauhe

a

were

exposure

cane

usually consist

to

car

devices

is very

cars

the

the

at are

platform

little water

be promptly

Machinery.

crushing

The

from

and

mechanical

should

loss of sugar

Mating

very

sorghum-sOgar

cane

hinged

aie

Hydraulic-power

is released

platform

that

probable

car

latches, which

platform.

this arrangement the

TOICB.

the weight of the load itself

that

wat"r

return

to

with

load.

the

tilting the

such

With

sides of the

the bottom

at

dumping in

or

THE

type the platform is tilted side-

In the second

stakes

fastened

OF

first successful

the

Fiske

National

and

machine

for preparing

cane-shredder, Fig. 1, invented

first used

in Louisiana.

This

for

cane

by

machine

milling Samuel coosista

tACnOH

OF

TKB

TUICI!.

A

fie"tond type

of crusher

This

differs in its cutting

from

that

of the

and

V-sbaped in

into groups, teeth.

5.

and

This

There

machine

crusher.

are

a

ing plants, a

crushes

only

pt^

are

thoroughly, of the juice. the

cane

The

The

or

a

crusher

mills have

bottom

two

is not

blunt-tooth

type

used, but

in its

top roll in the first

known

as

"excelsior

generally used in Java.

very

"cane-roll," and roll."

to

8,

rolls, especially a

PresentKlay Fig. 1.

is well

rolls,as

prevent clogging the

cost,

special corrugated

"

rolls,

pitch, vith

provided

considerable

moderate

at

Such

mill.

ue

installations, especiallyin atr^tgthening old mill'

some

Btead

of the

teeth

separating the teeth

Fig.

In

cutting

The

also grooves

are

not

in Fig. 4.

crushiog surface quite radically

or

opposite ends

from

scnqiers

but also expresses

Fulton, shown

luranged spirally,1.75 inches

are

Fig.

ia the

Krajewski

the spiralsworking fihown

13

FBOCEBSES.

MILUKG

always three rolls, ae

roll,where

that bottom

the

cane

enters, is termed

opposite the "bagasse" rolls

are

is shown

or

in the

"discharge-

usually rigidly fixed

in

pod-

'

14

arranged that it may

so

in the feed of the the bagasse-roU by

to

in the

THE

the top roll is controIIe4

tion and is

OF

EXTRACTION

top-roll cap is

"b^asse,"

in

rise and

7. one

fall or

This

is

tions varia-

applied

is shown

ram

of rolls to

trash-turner, etc., according

Fw.

A

pair

turner,

is

presatire

crushed

plate, variously termed

the mill la used.

"float"' with

The

curved

uid

hydrai'.ljcram

an

builders,

certain

from

passed

by

Hydraulic

cane.

Fig.

JTHCB.

called

now

cane,

the

in

next

by

a

turnplate, knife, dumb-

a

in which

the country

to

7.

supported by

a

steel turn-

heavy

plate-bar. The

mill-rolls

housings

mill-cheeks.

in Figs. 1 and

shown

and

or

7.

The

crown

driven

from

engine

is connected

with The

in massive

supported

are

The 2

and

wheels

the top roll

are

through

older

recent

more

by

types

which

shown

the

castings of

housings

models

in

bottom

in Fig. 1,

flexible

termed

The

couplings and

are

Figs. rolls

are

drivinggearing

the top roll of the mill.

Fuupene housing, probably

the

G

original of the inclined

in

type,is shown shown

in

which

one

housing is cane

the mill from

is inclined.

bagasse and

the object in inclining of the top roll.

the side toward

the

Since

The

6.

"flotation"

the

promote

to

enters

latter

Figs. 1, 2, and

other types in

inclined housingis

dispenses with the king-bolts projectingabove. the top-rollcaps of

This note

may

A recent Fulton

Fig.6.

Fig. 7.

16

PROCBS8ES.

MILLING

which

stress

greatest and

that

between

ing' hous-

is between

top rolls,by incliningthe housing

/resultant of this pressure

the

The

so

the

that Cane

the the and

angle of inclination,the top-roll brasses will rise and fall freelyin the housing or the roll will With the usual types of housings there is a tendency float. top rolls will follow

the

"

**

bearing brasses to "bite" into one side of the slot. This biting-inresults in friction that retards the free motion The Honolulu of the roll in accommodating itself to the work. this tendency in their have Iron Works overcome whose tion posihousings by fittingthem with an hydraulic ram be so adjusted as to promote the free rise and fall may for the

of the roll. Mill-rolls

cast of

.

the

bagasse. A

return

smooth-bottom t

an

to small

rolls is

grooves

probable

and with

even

tively compara-

the introduction

deep juice-groovesdescribed below. The feed-roll.in recent Hawaiian practicehas juice-grooves J inch wide by 1 inch to IJ inches deep, 2} inches pitch should patents). The depth of the grooves (P. Messchaert's

of the

be

1 J inches

in rolls 34 inches

less in smaller

rolls.

The

to 36

method

of

inches

in diameter

and

grooving is illustrated

Fig. 8. Special scrapers are used to keep the grooves free of bagasse. The grooves provide a very free exit for the juice eliminate slipping and the consequent mill and practically

in

^

iron mixtiure that will remain

rough acquire a "grain" with use that facilitatesthe feeding of or rolls are and bagasse. The often grooved to prothe cane mote and the breaking down the feeding of the cane of Its of various These structure. are shapes, forming grooves little used except are diamonds, zigzags,etc. Such grooves In the usual in Java. method, the rolls have peripheral V-shaped grooves, from three to six grooves per inch of roll length. The size of the grooves has been greatly increased the slipping of the roll upon to reduce in recent years, are

16

EXTEACTION

vibrftUona. be

used

The

An

OF

unlimited

without

of saturation

quantity

Blipping

JUICE.

THE

reduction

or

water

may

grinding capacity.

of

mill inlets and

ai"e, in

some

all tend

to

outlets may be very materially reduced in instAnces These conditions nearly one-half. increased

an

juice extraction

also

and

grinding

capacity. Messchaert

'

is obtained These the

extracted inch

lower

itself above

of

The

may

be

inch

1

smooth.

preferably

grooves,

of the

bagasse

discharge roll.

is the Hind-Renton

grooving.

milling plant that obtained 97

over

per

that

It is claimed of

part it

as

a

the boot

steel roll-shells may

that

of

crop

a

and

content the

grooving

deep

in

extraction

cent,

an

(sucrose

in cone). The pitch is two grooves per cent, sucrose the groove and angle is 30" instead of the usual at^le 60",

of about

the usual

moisture

in

roll

the

those

than

inch

wide, 1

invention

tried out

been tor the

average

by

bagasse roll.

or

numerous

grooves

The

reduced

Hawaiian

Another

the

inch.

per

is materially

has

these

discharge

more

always bear

must

three

This

for

and

in extraction

improTement

the

1 inch

are

Except

top loU

about

per

smaller

are

feed"rotl and

The

further

by also grooving

grooves

pitch.

that

states

pressure

hydraulic few

on

rams,

groove

in

a

the juice flows

and

that

the

with

bagasse

this

grooving.

the top roll is usually regulated except

mills in Java

L

not

have

wedges

It is also claimed

"boot-jack,"

be used

through

out

generally

in

by

meana

paratively Com-

Java,

hydraulic regulation,,most

Mauutacturing

MMbinery

for

191^

mill

slow

engineers preferringvery

of the

17-

PROCESSfiS.

MILLING

roll

speed and

rigid

a

setting.

applied on the top roll varies with the length of the roll,the strength of the mill and the quantity The pressure is also to b^ ground in a given time. of cane tandem.'' varied with the positionof the mill in the series or mills and rolls 7 feet long about 500 tons With strong modem Practice varies as and upward is often applied. pressure but this approximates 150 to 250 tons hydraulic to the loading,

hydraulicpressure

The

''

300

from

the

on

pressure

numbers

crusher,425

to 450

tons

apply

to

applied to

pressure

crushed

the other

on

tons

on

the first mill,and

mills of the train.

top rolls 7 feet long. The the

to receive

cane

500

to

crusher

These

high

very

and

first mill pr^ares the imbibition-water,or thin juice from

the last mill.

hydraulicregulationof

The

the top roll has

a

two-fold

pose, pur-

protection of the mills from serious damage in the event should a piece of metal fall into them of a or too heavy feed of cane, and the regulation of the opening viz.,the

between

the rolls to suit variations

bagasse

passing through

in the quantity of

them.

The

hydraulic

cane

or

pressure

sometimes piece may to bury itself in the shell without raisingthe roll sufficiently with powerful spiral afford protection. Toggles combined carried is so great that

now

springs instead The has

used

are

of

en

many

of metal

a

of

Mirrless,Watson

Co.'s

mills

hydraulic rams. of very

use

strong cast-steel housings

manufacturers

enabled

to

or

mill-cheeks

dispense with

king-bolts. only part way

Fig. 7, or to use very short bolts that extend through the housing (Honolulu Iron Works). This arrange* of large diameter ment permits the use of hydraulic rams with consequent increase of life in the packing leathers. mill The setting''or the adjustment of the openings '^

between

the

rolls and

the

relation

of the

tum-plate

to

the .

rolls,varies greatly in different factories and with the rate the quality of the canes and the grooving of grinding and modified when of the rolls. The setting is also somewhat hydraulic-pressureis not used on the top roll,or when it is of this chapter, applied to the bagasse-roll. For the purpose and

not

as

a

it is only necessary guide in mill-setting,

to

give

18

EXTBACnOK

OF

THE

JUICE.

in Cuba. These openings, etc.,of a small milling-plant shown in the diagram, Fig. 9. be noted that the It may are evening between the turn-plateand the top roll is gradually etilargedfrom the inlet to the outlet end. Special juiceused in mills. these This not enlargement are grooves permits the bagasse to expand after the first pressure and

the

facilitates the passage

of this material

and

the escape

of the

juice-groove6 (Messchaert) are juice. Where used, millopenings are very much smaller than in the example cited. The speed at which is usually a system of mills is driven of the periphery of the rolls. expressed in feet per minute Practice varies greatly in different countries in regard to the

speed of

the rolls.

in Java

to

as

This

high

as

from

ranges 30

over

as

low

as

12 feet

minute

feet per

or

less

in certain

SrdliiiU

Cuban

plants. The

Hawaiian

practiceis

about

an

average

of these numbers.

improvement in mill-accessories of recent years permits carrier by means of or the driving of the cane-elevator independent engines instead of from the milling machinery. This Two engines are used to avoid stopping on the centers. An

method in the

of

driving the

delivery of the

the crusher

and

each

the extraction of the

Milling-plants are many

as

conveyor cane

to

uniformity thus by giving

results in greater the Crusher

mill full work

and

at all times

it promotes

juice. now

21 rolls in addition

in

operation using from

to those of the crusher.

9

to

as

A favorite

a large factories consists of 12 rolls and of rollers engineers consider this number crusher, and many limit except where a largetonnage about the present economic be driven by one or more engines. be passed. These may must be ground, it is must When large quantity of cane a very

combination

in

20

OP

EXTRACTION

THE

JUICE.

bagasse from the firstmill and that of the last mill upon the bagasse from the second mill. Water is applied to the bagasse The the third mill. from juice from the crusher, first and second

mills enters

into

is modified

of the water

the manufacture. the needs

to meet

The

application

of other

tions combina-

For example, in the exceeding 12 in number. Mill, Maui, H. T., when grinding with their tandem of rolls

Paia

consistingof a crusher and 21 rolls,all the the bagasse from the fifth and sixth mills. on Maceration and

lower

lower

from

is

applied

applied to both the upper side of the blanket of bagasse. The application surface of the bagasse does not usually penetrate layers. It is preferable in applying the water

to the upper

the

water

to do

above

is sometimes

water

so

just as the bagasse emerges

between

from

IV

"0i"""^ To

Fio.

Defecation

10.

the rollsso that it will absorb it in it acts

as

a

that has been

sponge

^^

expanding. In

this way

compressed.

The

of saturation is obtained in the double highestefficiency and compound There is,however, always danger processes. if the plant of fermentation of the thin juicein these methods is not well arranged for it,hence many manufacturers prefer the mills. The mills water to use only, dividing it among be shut down must at frequent r^ular intervals for a thorough

cleaning where practice, due

these to

methods

high

cost

are

used.

of labor

and

The

usual

Cuban

cheapness of the

the mills grind the largest quantity of cane will pass with good efficiency. This condition prevents thoroughly saturating the bagasse with thin juice as in the since very and wet double bagasse compound processes,

product, is

to

slip and the mills refuse to receive have improved with the introduction

rolls to

the

causes

conditions

These

21

PROCESSES.

MILLING

it. of

the time to factories can juice-grooves. Few Cuban spare thoroughly wash down the mills and tanks of tener than once a

week.

by

Tests

investigatorslead

many

is practically the

the mill extraction be used

of

The

manufacture.

sugar

the

of the

matter

that

tion-water macera-

quality

some

water.

warm

whether

same

The

l^onclusion

-fuel economy usually dictates the usq Alkaline water should not be used in white-

and

of the water

cold.

Ipt or

the

to

hot

is derived

water

from

the

evaporator-coils,etc.,t"ver requirements of the steam-plant, and is therefore very water, from

of return

Those

distilled water.

of the heat

into

the

juice

units

that

pass

with

plus sur-

the pure

the

largely economized. is also a slightlyincreased There evaporation of moisture the bagasse in transit to the fires,as compared with from with cold saturation. With that obtained properly fitted rolls th"*e is Uttle danger of looseningthe shell from the shaft

saturation

water

by expansion in the The

saturation

bagasse.

Neither

use

of

warm

are

water.

completely penetrates the the physical condition of the bagasse nor water

never

element, i.e.,the duration of the contact with the water, permits complete penetration. Manifestly the nearer we approach this ideal condition,complete penetration, the the

time

better the

the extraction

of the sugar.

of the older methods

reverse

in which

and

the heaviest

were roll-pressures

the

series.

cane

The

is

now

Modem

broken

mill

practice is

the strongest mills

found

in the last mill of

thoroughly in the of the juiceas possible, up

crusher,with the expressionof as much and the heaviest roll-pressureis carried in the first mill with a view to thorough preparation of the bagasse to receive The present tendency in milling is to apply the saturation. the maximum

pressure

to

the firstmill that is consistent with

of cane, amount strength and the grinding of the necessary and thus rupture the maximum of juicepracticablenumber cells. In other words, it is clearlyrecognized that the bagasse be thoroughly prepared for saturation. these Under must

its

conditions,moderate mills.

pftessures only

are

requiredin the

sequent sub-

22

EXTRACTION

If all the or

that

JUICE.

THE

of the plant are ruptured juice-cells

crushing

when

OF

and

process

is

the water

in the shredding

the first grinding,it is evident

applied

to

the

bagasse, if the time

sufficient,it will penetrate it and dilute all of The time element, however, in practice the juiceit contains. be

element

is

so

only

cells escape the superficial portions of the juice are

short, and

so

many

of the

rupture, that diluted.

demonstrated

by laboratoryexperiment with water is required follows, that very long contact as for the dilution of all the residual juice in the bagasse: A was sample of bagasse from thoroughly crushed cane in the proportion of 5 parts of bagasse heated with water The

to near

45

author

has

parts of water, and the

boiling-pointone

maintained temperature was The and bagasse water hour.

thoroughlymixed

and

the dilute

COMPARISON

OF

MILL-JUICES.

the

juicewas strained The residual juicewas off,using moderate- pressure. expredsed with a laboratory cane-mill,using very heavy pressure, and the two samples of juice were separately analyzed. The percentage of sugar in the juiceextracted by the mill was very ing. largerthan that in the juiceobtained by strainperceptibly This repeated several times with experiment was like results. Again, in diffusion work with cane, the author ate has frequentlynoted that the thin juiceobtained by moderfrom the exhausted chips contained less sugar pressure These experiments show that than that by heavy pressure. it is not practicablein millingto dilute all of the juicein the and that a factor depending bagasse with the saturation-water, the time element and the efficiency of the mills must upon be appliedin estimates of the water actuallyutilized. The followingfiguresare from records of actual milling:

were

then

Water the second

mill.

The

layers of the bagasse

upper

saturated,but the lower

bagasse as it emerged

the

sprayed upon

was

23

PHdCBSSES.

MILLING

received

ones

much

from well

were

less water,

as

the

and comparatively little penepartly absorbed trated from the analyses to the lower layers. It is evident that the water did not uniformly dilute the juice in the

latter

was

bagasse. Influence of the Structure' of the Cane has

structure

influence

marked

a

on

MiUing.

on

the mill results.

^The

"

With

efficient

milling certain canes* yield bagasse containing 50 per cent woody fiber (marc) and 45 per cent of moisture; mills and mill-setting ground with the same others, when and apparently the same give bagasse containing efficiency, very

45

per

cent

conditions

of fiber and

have

varieties Nos. In his on

Mill

been

Work

*

in Java

These

grinding the

when

100.

study of "The "

of moisture.

cent

per

observed

and

247

60

of the Structure

Influence

Noel

Deerr

"It

says:

not

of the Cane

infrequently

happens that while the fiber remains of constant percentage, the extraction varies largely,the millingconditions remaining Such variation can the same. the be readilyunderstood on the of fiber remains assumption that while the total amount its distribution between the pith and rind varies,an same, increase in the proportion of the latter being accompanied by

decrease

a

in the extraction."

Adhering leaves and the immature tops of the stalks, remaining through careless harvesting,increase the quantity of fiber that must be passed through the mills and adversely affect the

extraction.

Increased

saturation

is necessary

to

this influence.

overcome

Efficiencyof Milling. The efficiencyof milling is most conveniently expressed in terms of the percentage of the total "

in the

juice. Numbers 92 and 95 indicate good efficiency;those above 95 between are exceptionallyhigh, and 98 is perhaps the best recorded number in mill-work and is one which rivals results by the diffusion process. The efficiencyis also indicated by the numbers obtained in the analysis of the bagasse or by sucrose

the

cane

relation between 1

Bui.

that is extracted

the fiber and

30, Hawaiian

Sugar

in the

sucrose

Planter's

in this material. Expt.

Sta., 41.

24

EXTRACTION

OF

THE

JUICB.

Straining the MiUrjuiee. ^Three types of Juioe-strainers "

viz.:

in use,

(1) Hand

strainers

in which

the

juice is passed through a perforated-brassplate surface,kept clean Such used only in very small screens are by hand work. factories. (2) Strainers consistingof perforated-brassplates surfaces are whose of flightsor slats, k^t clean by means The similar to a squeegee. less flightsare attached to an endare

They brush

link-belt.

the

particlesof bagasse from

the

plates and elevate and deliver them onto the bagasse-carrierfrom the first mill. The holes in the strainerplate are round and about 0.04 inch in diameter, or the plate of the

surface

is

perforatedwith

If the

holes

thinner

and

smaller

are are

about

round

324 the

holes

plates must

liable to break.

This

be

per

square

inch.

correspondingly

is the type of strainer

generally used in large milling-plants. (3) A recent strainer,patented by Van Raalte, a Dutch engineer of the grasshopper sugar-conveyor in Java, is a modification that

is very

(see

page

102).

In

this

modification,the

bottom

is

composed of brass plates perforated with A canal holes of approximately 0.02 inch diameter. fine bagasse, the strainer collects the juice. The conveyor

the

of

roimd under '^cush-

English factories,is discharged at the end of the strainer,in a thoroughly drained state, and is returned by an elevator to the mills for regrinding. cush''

The

of the

first type of strainer is not

to be

considered

second

or

is very

great, and

for

use

in

drag type has certain marked disadvantages as compared advantages and some very It strains large quantities of juice with with the others. and occupies very little space. The wear few interruptions factories.

modern

of the ihick

The

perforatedsheets sheets

the

be

perforations must The

otherwise

be

foul,and

undoubtedly this is

necessary.

link-belt a

in order

larger than soon

becomes

to

use

would very

of sugar losses which chemical control begins with source

consideration,since the be frequently the strained juice. The belt and flightsmust The juice-canaland tanks under cleaned and steamed. this strainer cannot usually be conveniently located,thus making in a thoroughly sanitary condition. it difiicult to keep them The elevator also fouls quickly from juice-drippings. escapes

The

third

type of strainer,the

"grasshopper,"so

far

as

DIFFUSION

writer is aware,

the

is

25

PROCESS.

outside

yet untried

as

of Java.

A

marked

with advantage of this strainer is the ease which it may be kept in a sanitary condition,thus reducing Thin sheets with very thci loss of sugar. fine perforations very

be

may

used.

There

strainingsurface for

1000

of

of

tons

is very

4.

cane

Process.

in 1889, there

the

6.

page

the

of

When

"

on

sheets.

A

feet is sufficient The

importance of its bearing on the

juice and

raw

the

on

hours.

24

per

is stated

Extraction

wear

approximately 2X16

thoroughly straining the manufacture

little

'

Juice

tlie

by

Diffusion

first edition of this book

was

written,

rapid extension of the diffusion process in the cane-sugar industry. Even at that had very largelysuperseded presses in the date this process the only process used in beet-sugar industry. It is now extracting the sugar from the beet. The advent of diffusion forced mill-builders greatly to improve their machinery, and, of multiple-millsrivals at the present writing, the work the best diffusion results in extraction. The ever, mills, howdo their work

and

the

excellent the

expense

has

diffusion.

of

regards the

been

mills, has In

devoting

doned. entirelyaban-

so

the

also

view

of these

much

space

industry,is

cane

almost

milling, with

of

by modem

writer hesitates in as

fuel economy. It is largely for fuel,the large water requirements

diffusion

results

decline

a

marked

convenience

The

expect

in disposing of the residual ''chips" difficulty

bagasse, that

or

with

to the increased

due

to

reason

was

contributed conditions

to

almost

attendant

a

process

only

to

the

that,

of historical

interest. In

the diffusion process

the

cane

is cut

into small

chips

oralices, which are packed into cylindricaliron vessels termed Each diffuser is provided "diffusers,"or "cells." with and page

strainers

at

with suitable 27.

The

with from

as

with

indicated

a

in

juice-heater the diagram,

diffusers are a

arranged in a series and the combination "diffusion battery." The cane-chips

systematicallyextracted

diffusers.

bottom,

pipe connections

is called are

the top and

The

chips that

water

enters

with

warm

water

the first cell in the

in

these

filled series,

and of sugar, nearly exhausted passes cell to cell,each containing cane-chips richer than its are

26

'JUICE.

THE

OF

EXTRACTION

predecessor,UDtil it finallyfillsthat containing fresh canecuttings. A measured quantityof juiceis now drawn oflFfrom is pumped defecation-tanks. to the the last diffuser and first diffuser

The the

is

chips it contains

exhausted

diffusion process

which

passing through classes

Certain

readily

and

The

colloids.

of

pass

include process

or

not

chips

with

the

that property

upon

in

solution,of

contiguous solution. through a membrane

a

all.

at

The

former

stances, sub-

crystalloidsand the latter, "dialysis,"or, taking into through the crystalloidmoves

sugar, are is termed the

"exosmosis."

or

into slices little more

ideal

The

highest efficiencyof this

for the

The

juice.

dense

possesses,

substances

"osmosis"

membrane,

is based

into

the' direction

accoimt

theory

slowly

with

sugar

membrane

a

others

which

discharged. always in contact

class of substances

certain

a

in

series and

the

are

containingthe least sugar are weakest juiceand the richest in The

from

disconnected

now

tion condi-

is that

process

the

ness plant-rellin thickrupturing few cells,thus permitting the process to be low conducted at a temperature, extracting the greater leaving a considerable part of part of the sugar by dialysis, be cut

cane

than

a

impuritiesin the exhausted residue. This condition can not be even approximated in actual practiceand the process of maceration rather than diffuaon. one usually becomes the

Diffusion Process. Manipulations. The first duties of the head that all joints are to see batteryman are in place, and that are ti?;ht,that the various signal-bells The

"

all mechanical

details essential to

good work

received

have

attention. One

of the

several

methods

of

arranging the valves

battery is shown, in the diagram, page For

convenience

of reference

the first to be filled with when

the water

to

supply

about of hot

Fill cell No. 4 with heater No.

No.

3 and

4 at the

203** F. water

will suppose

the water

heaters; fillNo.

two

cell No. 1 with

into No.

3 in the

same

first round

4 is

water;

2, passing it

heating

manner,

(95" C.).^This

for the

a

27.

chips. Fill cell No.

this cell is filled turn

through

we

of

assures

an

of the

dant abun-

battery.

cane-chips; pass the hot water up through down through heater No. 4 and into ceU

bottom, drivingthe air

out

of this cell

through

28

EXTRACTION

with

chips. It is For

time

now

same

top, is

the

with

the

drawn

to

measuring-tank

and

requisiteamount

the

tank-valve,

that

open

previouslyreceived

from the

No.

precedingones,

having No.

connecting heater

its

the

Having

charge.

a

juice and

12

Having

II.

being already established connecting the juice-main draw

of

fiU cell No.

juice-main and is

valve

of diffusion-juice.

the first draw

as

pressure

the

open

JUICE.

draw

us

manner

manipulation, the

next

THE

make

to

example, let

filled this cell in the

at

OF

closed

the

with

the

12

usual, this cell having

as

cell No.

charge of chips. When

12

Continue charge of juice as before. in this manner, drawing a charge of juice from each cell of cell No. 14 is reached, discharge the fresh chips. When from Nos. 1, 2, and 3 through the waste-valves, the water valve connecting No. 1 with the water-main having been draw filled,

closed

also that

and

of cell No.

connecting heater

Connect

5.

cell No.

Cell No. 4 is now

main. of the in

another

5

directlywith

of the circuit, and

out

battery is completed.

If compressed

forcingthe circulation, as

each

is usual

(except the first round

of the

will have

little water

The

to open

air;

or

the air-vent

left in it.

the

the

top

water-

the firstround

air were

juice is drawn very

4 with

No.

employed

time

a

cell of

battery),No. 4 next operation is

No. 4 for the escape of the compressed if water-pressure is used, to admit the air to the cell on

through the waste-valve.' The door at the bottom of the cell must be opened and now the exhausted chips discharged into a suitable car or carrier. The workman on duty below, before latchingthe door, should rapidly pass his hand, protected by a cloth, about that part and

of

permit the

the

jointto The the

bottom

water

which

escape

first "round"

of the

with

in contact

comes

adhering chips,which

remove

regularroutine

remain

to

might

cause

battery having been Three

commences.

and filling

hydraulic

the a

leak.

completed,

cells should

always

being prepared for fresh chips. Every time a cell is filled with fresh chips and juice be drawn and a cell of exhausted a charge must chips rejected. work In regular it is usual to designate the cell first in the open

"

series, i.e., the the

one

one

which

one

receives

the

water

direct

from

supply-tank, No. 1, and that from which the juice is drawn. No. 10 or 11, according to the number of cells com-

29

PROCESS.

DIFFUSION

posing the battery. In the above descriptionof the battery said in regard to the temperature to routine nothing was which the

juiceshould

the

at

temperature

experiments

Fahr.

.

.'.140*

.

followingtable

United

the

tion. Magnolia Planta-

at

8 203"

168"-176"

shows

Government

States

in the work

(234667)

1

OeUnumber

Temp.,

which

conducted

were

The

be heated.

0

10

11

12

203"

203"

186"

160"

subsequent work, using the Hyatt cane-reducer, much dilution of the lower were required. The temperatures In

juice was but

0.07 pep

of sugar

cent,

high temperature

The

necessitated

by the

lower

millingand

of the

temperatures

diffusers

of the

the

saturation,

left in the exhausted

was

coarseness

which

experiments, in much

with

greater than

no

was

chips. In the earlier

maintained

were

chips.

in this work

sliced, not

was

cane

and

shredded,

with

factory satis-

a

extraction. ,

juice is heated into the circulating pipes. This method batteries the

In many

the

of

and manipulations slightly, sugar through leaky heaters.

Prinsen-Geerligs* advises

by injectingsteam of heating modifies

eliminates

risk of loss

the

^

following procedure: "The most advantageous way of heating is by steaming the diffuser of 75" C, and not filled with fresh chips to a temperature this temperature the others. At the cells die warming and the sucrose diffuses,whilst the albumen coagulates. is drawn After the diffusion-juice off,its place is taken by the

in contact with has been previously heated juice which chips and hence has a lower temperature, and this goes on until the exhausted with chips leave the diffusion-battery the

temperature

same

in the In

chips no

heat

order to obtain

chips and

coarse

at

they had

becomes a

entering it, so

that

lost."

maximum the

when

extraction time

same

a

with

juice of

moderately a

maximum

of cells 9, 10, that the temperature density, it is necessary 11 be kept as high as is practicable. The hotter the and water entering the cell containing the fresh chips,the better "

""..

1

Cane

J-

"

Susar

and

the

Process

of its Manufacture

"

in Java, p. 26.

30

EXTRACTION

the

extraction

for the It is

in this

well

a

heavier

of

dilution, and

if we

91, and

about

average

draw

the

do

we

analyses of the juices contained to

the work

commence

estimating

on

an

Extraction

If the

juice,and is

density safe

to

chemical

economical

chips

the

and

of

about

With

thin

reduced

to

density

less than until

18

when

of

cane.

sion-juice diffu-

the

90

per

bum

coal to

more

but

there

two

which

or

might

three have

evaporate tenths

per

it is not

is

careful

a

additional of

cent

obtained

been

cent

satisfactory regular work

cent,

per

cent,

per

a

and

chips

except

23

juice in the

of

be decreased

following table, designed

The

based

dilution

by

poor

it is

water, sucrose a

little

dilution.

hieher

the

should

the

It is safe

promptly detect and remedy a the best multiple effect evaporation

leave

than

rather in

to

sucrose.

contains

and

though the normal

of

the

cane

lower

be

to

With

extraction.

a

this limit

control

is

ordinary plant-cane will

cents

per

satisfactorybut

be

below

go

variation In

cane.

even

vary,

cent

obtained. may

This

will

per

the draw

dilution

the

in the

sucrose

juice in

dilution

of 90

average

low, the

too of

same

with

is

normal

(ratt^oons)89; consequently, of juice when diffusingplant^cane

juices wilt

two

the

in stubble

stubble, the

with

in

cent

per

cent

per

amount

same

quality of

perfectly regular extraction,

a

the

ever, had, how-

the

sucrose

juice-content of the

(in Louisiana)

seasons

be

upon

considerably.

vary

variable

the

to

of

consequently the

diffusion-juice,will due

and

the

maximum.

a

percentage draw,

chips 'and

should

effect of high t^nperatures

uniform

juice, a

in

sion rapidly the diffu-

more

consideration

Due

constant

a

the

this cell.

difference

greater the

the

in them

place.

less work

enter

juice bathing the

juice in de";idingupon

With

as

that

thin

the

juice contained

for the

the

JUICE.

consequently the

cell,and

fact

known

will take

the

THE

subsequent portions of thin juice which

densities

the

OF

dilution an

on

of

an

for

different

assumed average

specificgravity).

for

preliminary work, gives

quantities

of

juice-content in the

density of

16"

Brix

juice drawn. cane

of 90

(9" Baiun^,

It per

or

is

cent, 1.0656

BT-PROBUCT

5.

OF

of

By-Product

derived

moisture

supplies

a

is

bagasse

fiber of the

woody

and or

in many

The

product by-

nies), (EInglishcolo-

megasse

the residual

the saturation-water.

from

large part and

very

Diffusion."

with

cane

31

DIFFUSION.

AND

Milling

milling cane

of the

MILLING

juice and

This

instances

material

all the fuel

required by the factory. The exhausted chips from diffusion dried in Egypt by flue-gasesand supply a considerable are part of the fuel. has

It

utilized

but

to the commercial

Havik East

*

Indies

islands per

paper.

to

with cent

a

stated Havik's

these or

operated only

utilization

by

view

to

paper

mills short

a

of exhausted

of the diffusion

success

materials

three

be wee

time,

chips would process.

the Government

investigate the fibers of Java

of the

The

Two

were

commissioned

was

that

urged

manufacture.

paper

hoped that such

was

lead

32

in

for this purpose,

built it

frequently been

of the Dutch and

manufacture.

He

the

other

obtained

weight of dry bagasse in dry unbleached

bagasse yield of

52

Cheribon

from

was

per

cent

of paper

experiments. *

Int.

Sugar

Journ.,

14, 52.

cane.

is

The

quently fre-

disproved by

STEAM

Steam

6,

in

Boilers

a

the

and

the

is necessary of

boiler

requirements boiler

boiler

horse-power large Cuban

factory, having

utilizing the

or

1

per

of the

reduce

these

with

15

cent

per

Both

is often on

meet

the

The residue

bagasse

very

the

of

boiler

horse-power feet

utilization

boiler of

the

materially white-sugar

may

steam

to

have

large

of

the

for evaporating

requirements

applying

advantage

of

of the

heavy

cane-

The over

fire-tube the

other

fits it to

the

factory for steam. factory is the woody Many instances

in many

requirements.

saturation

in

water-tube

capacity, which

water

cane-sugar

their only fuel, and excess

an

used

select

safety.

itself, bagasse.

cane

are

factories

irregular demands

from

in

the

evaporating

of

boilers

greater

their

of

of its

fuel

produced

the

of

or

square

the

increase

including

pans

steam-consumption

Cuban

considered

usual

as

15

to

and

water-tube

Many

account

type

other

or

manufacture

in

etc., may

account

on

12.5

The

and

factories.

boilers

to

more.

fire-tube

sugar

boiler

or

industry,

using pre-evaporators

first

mill-work

increase

wash-waters,

the

customary

equipment,

multiple-effect in juice-heating

its attendant

of

factory in nominal

a

nominal

1.50

to

numbers.

If the

beet

is

It

juice-heating

about

or

Good

heating-surface.

in

1.25

capacity-ton,

vapors

in the

not

the

multiple-effect evaporator sirup, requires from

facture manu-

juice, in juice-heating

good

but

from

vapors

the

capacity-ton.

cane

quadruple-effect evaporator,

a

the

capacity required by per

for

capacity

application

lessened.

are

boiler

for raw-sugar.

is customary

fis

of saturation-

and

cane,

quired re-

manufacturing

More

multiple

evaporating

purposes,

the

is

rich

includes in

state

A

produced. for

the

capacity

quantity

plantation white-sugar than

for other

its

with

the

cane,

sugar

than

poor

generated

vapors

and

grade of

boiler

-The

factory varies

equipment

factory

Fuel."

quality of the

for

FUEL

AND

and

cane-sugar

equipment, water

PLANT

in

The

factories

use

this material modern

milling has

dency ten-

increJtsed' 32

8TEAM

the

demand

oil must

BOILERS

for steam, with

often

the result that

also be burned.

cost, labor and fuel

dear

very

33

FUEL.

AND

Where

or

is of moderate

cane

and

the sugar sells for a very sometimes bring in larger net

price, the factory may returns by grinding a large quantity of low

coal,wood

less

efficiently than it could a small quantity. This large grinding produces fuel in the and surfaces to more proportion radiating it is usually necessarilyaccompanied by the use of a reas duced nated. quantity of saturation-water,extra fuel is often elimiThis condition frequently exists in Cuba, hence few factories have adopted pre-heaters or use a part of the cane

the

multiple-effect evaporator in heating juices in evaporation sirup in vacuum-pans. or There three general t3rpe3 of furnaces used in burning are first bagasse for the generation of steam. (1) The green of these was patented by Samuel Fiske, the inventor of the from

vapors

cane-shredder. Cuba

It

first used

was

and

in Louisiana

then

in

at ''Soledad"

Cienfuegos. This furnace consists of an fitted with horizontal grate-barsupon which the bagasse oven is burned. A singlefurnace was often connected of by means flues with several boilers,thou^ preferably in entirelynew installations was

under

with the

but

front

end

the

In

two.

of the

used

in the

after

using it in Louisiana.

latter

boilers.

the

case

furnace

Forced-draft

was

since the bagasse often left early installations, the mills with as high as 60 per cent moisture. (2) Almost Cook introduced his simultaneously with Fiske, Frederick at bagasse-burner into Cuba "Hormiguero,'' also green

bagasse is burned two

water-tube

Fiske

and

hearth

a

boilers.

through

bagasse the

on

Air

tuyeres.

Cook

In

bumiers

this

in

an

all

to

furnace

the

placed between

oven

is forced

Prior

of

type

into

the

bagasse

the

burning

introduction sun-dried

was

of in

burning it. The inventions of Fiske and Cook had a profound influence upon sugar-manufacture in Cuba through enabling,and, in fact,forcing the factories to operate day and night instead of but fourteen hours, and in sending Cuba

before

of people to the fields who large numbers in drying and firingbagasse. furnace

is the third and

is usually a

fiunace

most

in front

recent

of each

type.

were

formerly

(3) The

ployed em-

step-grate

In this type there

boiler. The

grates

axe

r

34

STEAM

and

inclined

resemble

FUEL.

AND

PLANT

and in fact step-ladder,

a

often

are

"step-ladder" grates. These grates are very long and narrow. The bagasse falls upon the top steps of the ladder and gradually works its way to the small flat grate termed

at the bottom.

installations of all three types of furnaces

Modem

efficient. The

draft is in

and

very

usually used

Forced

in

very

the

Hawaiian

and

Islands

littleused, since with the vast

now

milling,the

often

very

The generallyused in Cuba. efficient with very dry bagasse and are

is most flat-grate

step-gratesare those

are

much

usually contains

bagasse

less moisture

Java.

ments improve-

50

givesgood

and

cent

per

results

with natural draft.

of Bagasse and Other Uesidues. ^There is great of heat units (B.T.U.) of peruniformity in the number fectly Fuel

Value

"

dry bagasse,as has been shown calorimeter world.

consideringthe

In

it is burned that

a

tests made

combustion

upon

actual

by the results of in various

fuel value

the grates, it must

certain number

of heat units

are

be taken

many

parts of the of

bagasse

as

into account

absorbed

heating the resultant vapor peratiu^ of the chimney. Further, a part of the fuel is consumed of air that is drawn in heating the excess through its moisture

and

in ing evaporatto the tem-

with this and an is carried away also with the products of combustion.

the grates and

additional

quantity

Dr.

Norris

^

publishedthe followingfiguresfor

of various

Hawaiian

R.

S.

bagasse

degreesof moisture: Fuel Value per Pound of Bagasse, B.T.U.

Moisture Per Cent in the Bagasse.

42

3129

43

3057

44

2982

45

2909

46

2835

47

.2762

48

2687

49

2614

60

2540 2468

51 "

' "

"

Bui. 40, Hawaiian

Sugar

Planters*

Expt. Sta.

outline

an

of

customary

the

manup;acturing

Introductory.

with

them United

the

States

of

Outline

Juice,

by is neutralized to

the

In

Louisiana

by milk

practice the

juice after heatinij and continued

tanks

juice"

mud

retained

in

with

the

"clarified"

the

clear

"sciun"

the

of

tories fac-

juice in specisd

the

juice.

fied "clari-

or

(Cuba="

"slops"

filtrate The

"filter-press cake,"

press,

F.

ing by boil-

liquid

or

clarified

the

off

number

greater

the

raised 200**

is then

filter-pressed and

is

is mixed

"press-juice"

decant

"mud,"

the

from The

cachaza).

and

little below

settle

juice

is then

"brushed"

process

plished accom-

acidity of the

is often

The

brushing.

heating,

after

latter

the

defecation

using the

The

a

esses proc-

book.

juice is

of the

usually

scum

The

in

Purification of the

"

heat.

or

than

of the

part

lime, its temperature

of

point,

"cracking"

and

and

ing illustrat-

elsewhere

subsequent

a

imize min-

especially to

parenthesis.

clarification

or

of lime

means

in

is to

time

same

used

Manufacture.

defecation

^The

"

the

the

at

Terms

in full in

outline

descriptions and

included

are

this

of

terms,

examples.

described

are

7.

technical

of the

many

cane-sugar.

purpose

repetitions in future

the define

raw

The

"

op

method

or

tates precipiused

are

in

fertilizingthe fields. Evaporation, to

vacuo

^The

"

(Cuba,"

"sirup"

a

mdadura

"

single-effect

sirup

is

point

crystals pan

or

with

evaporates,

upon

the

and

the

grain present Should

sugar

without

Pronounce

it contains

At

sugar.

in

sirup from

additional ^

separate

the

time is

the. formation

boihng to

time,

this mass.

as

the

largely deposited of

additional

crystals, "false-grain," **

in The

pressure.

with

=

of water.

accomplished

reduced

saturated

"grains"

"charged"

water

crystals.

imtil

evaporated

is

under

vacuum-pans

partial

industry

cent

per

crystallization is

Crystallization, ^The

in

beet

^;

juice), containing approximately 45

thick

The

juice is evaporated

clarified

May-lah-ddw-rah.'!

36

form

OP

OUTLINE

through carelessness mterference

THE

or

37

MANUFACTURE.

otherwise

they must

be remelted

to

subsequent stage of manufacture. Finally whesi the crystals are of sufficient size or the pan has been of crystals and filled,the mixture sirup is concentrated prevent

to

dense

a

fill-mass)and

at

the

^^

a

"massecuite/^ (beet industry

mass,

=

strike'^ is then

latter is often termed

This

dischargedfrom

the pan.

^'strike'' pan.

a

The massePurging; R^xnUng Molasses, Centrifttgaling; cuite is conveyed into a mixer and from this is drawn into have centrifugal-machines,"centrifugals.''These machines "baskets/' lined with wirecylindricalperforated metal cloth or at perforated bronze-sheets and are high spun "

are sugar-crystals

velocity. The washed

be

may

upon

it with

retained

by the liningand

if desired.

water

The

mother

of liquor, "molasses," passes through the liningby reason The machine is stopped after the centrifugalforce exerted. of the molasses

removal

the

and

the

leaving the centrifugalready for another and

is reboiled

molasses

The

the

yielding

"second

massecuite"

"second

sugar"

is also reboiled

molasses

molasses," "black The

than

increases

thus modern and

or

is here

"pan-boiling" molasses sirup or is said

of

strap"

the

to be

down,"

charge of massecuite. second

a

is

and

and

followed

processes

complicated the

obtain

to

is "cut

sugar

of

crop

centrifugaled as

"second

crystals before,

molasses."

This

yields"third sugars" and

"final

"third molasses."

in the

modem

indicated. is

factory

At

a

certain

injected into the

"boiled-in^'

or

more

stage of instead

"boiled-back"

output of high-grcidesugar.

factory usually produces but

pan

are

one

In

and

it

fact ths

grade of

sugar

final molasses.

Factory Design and

Construction.

^A

large Cuban

factory of recent construction,designed and erected by B. Glathe, Chief Engineer of The Cuban-American Sugar Company, in the Frontispiece. This factory has two tandems is shown trains of mills. It is so arranged that its capacity may or further increased or even by adding a readily be doubled extending the boiling-houseat the right. The present annual capacity of the factory is approximately The of of tons buildings are steel, 80,000 sugar. is operated. largelyelectrically and the machinery mill-house

at the left and

"

"

PURIFICATION

Pariflcation

ttons. beeu

OF

of the

THG

JUICE.

Juice.

General

Considera-

juice is first thoroughly strained

The

"

The next step is ]"age 24. Lime the class of sugar that is to be made.

described

upon

t

PROCESSES.

MANUFACTURING

8*

"

on

has

as

dependent and

heat

facture. manuexclusivelyin raw-sugar methods of making plantationwhite In the simiiJer and high-grade yellow sugars, sulphurous acid is used in Conjunction with a small quantity of lime. In these processes the lime is added to neutralize or partly neutralize the acids of the juice and that of the added acids if any,

the agents used

are

and heat is then

almost

appliedto

temperature

a

a

littlebelow

94"

C.

and thick heavy precipitateis thrown down rises to the surface of the juice. The albuminoid and coagulated largelyrise to the surface,and are

(201" F.). A scum

matters

with

the acids combine salts. in the and in

The

scum.

soluble and

included part of the gums are juice b separated by subsidence

is termed

the defecation

localities the ''clarification''of the

modification

of the

ble insolu-

and

wax

clean This

decantation.

some

A

fat and

The

the lime to form

carbonation

process,

or

juice.

process

of

the

beet-

industry as regards temperature and limingconditions in combination with is frequently used sulphitation in of plantation white sugar, notably in Java. the manufacture sugar

An

identical

carbonation

process

was

worked

out

about

by the U. S. Department of Agriculture^ in experiments and sugar-cane with sorghum in Kansas at Magnolia Plantation, the Louisiana. Possibly originatedin Spain. process A sulphitation process devised by Bach, in Java, dififers 1886

from

the usual

one

in the addition

viz.: to the juice and "

See

the

report of the

of the lime at two

stages, sirup (concentrated juice),each Bureau

of

Cbemiatry. 38

CLARIFICATION

be filtered sirup may by decantation.

and

the

or

precipitatesmay

be

rated sepa-

of them processes and slightmodifications almost exclusivelyin the cane-industry.

used

those

prpcess for white sugar, by Wijnberg, all others in Risinga decolorizing carbon of great

differs from

bleaching

''Norit."

called

power

slightlyacid

defecated carbon

boiling with

cent

5 per

a

carbon

is added

is then

to

boiled and

(press-cake) is revivified

solution

it in

by rebuming

The

juice,which

filter-pressed.The

with

are

patented

recent

the

39

TANKS.

above

The

A

OPEN

Both juice being followed by sulphitation.

of lime

addition

WITH

a

soda

of caustic

kiln.

The

and

by

sionally occa-

sirup is filter-pressed

kieselguhr. differingradically from process,

the

others, has been an patented by Batelle and worked experimental upon scale. The glucose of the juice is destroyed by the action This enables the use of lime at boiling temperature. of A

the

Steffen

the

sugar

saccharate-of-lime the

from

in the

process

The

molasses.

of

recovery

is used

saccharate

as

in

ing heatin liming the juice. After beet-sugar manufacture and the glucose the juice is carbonated to decompose sulphited as in the carbonation factories of Java. have been used by many of substances A very largenumber and in purifying beetcane-juices. Von exp^menters list of

Lippman's is given on In

600

entries,

532.

page

hence

spores,

than

more

of the processes for the maintained temperature

none

high

the

these, comprising

purificationof the juice is long enough to destroy to avoid decomposition at

is necessary

care

later stages of the manufacture. DeTecatton

9. "

^ThiB is the process

improvement The

As

until recent

vessels

bottomed of the

of the

juice is pumped

raw

termed

years. from

as

the

bottom

juice,milk

of lime

and

is turned

steam

is added Into

the

and

the

the

to

has been

practbed little

.

mill-tanks

''defecators.'*

of

Tanks.

Open

industry,with

cane-sugar

defecator, is of copper

soon

and

in general use

early days

the

since

with

Clariflcatioii

and

the

The outer

defecator it to

space

to

inner

bottom

shell of

is covered

neutralize between

double-

the

the

iron. with acids

bottoms.

40

PROCESSES.

MANUFACTURING

The

regulates the

workman

time

that

of! and

'*

surface

the

covers

pressure juice the

boiling-point.The

its

nearly reached scum

is filled with

defecator

the

steam-

have

the

thick is shut

steam

of

subsidence

for the

juice is left undisturbed

the

the

cracks"

will

latter

moment

the

by

that

so

impurities. will

as

rise to. the and

the

properly gauged,

part of the

inapurities ''blanket,"

forming the

sciun,

of the defecator.

coagulates the

heat

and

albiuninoids

acids

the

salts with

soluble

and

insoluble

forms

lune

the

a

on,

the bottona

to

of the

action

The

with

surface

part settle

a

farther

described

be

required has been

lime

quantity of

If the

the heavy precipitatein settling and juice. The the impurities separated them with in rising carry scum the at in the defecation, leaving a thick deposit of mud of

the

defecator,

of the

bottom

of

blanket

a

the

at

sciun

surface

liquid,with .bright,clear juice below it. of the juice rises in the defecator the temperature When

of the

breaks, in the efforts of the air and

the blanket

and

escape,

defecators

time

the

filter-presses,the

charge-tanks to

the

series

a

and

cient Allowing suffiregular order. is ''cracking" for settling,the mud

the

after

off from

drawn

usually arranged in

are

juice in

filled with

are

"crack."

it is said to

Several

to

gases

or

of the

bottom

juice is

clear

into

defecator

and

sent

into

the

evaporator

run

finallythe

and clarifiers,

scum

to

the

is sent

presses.

skill. liming of the juice requires considerable is used, the impurities settle slowly, the If too little lime clarified juice lacks brilliancy,and the subsequent boiUng of the sirup and purging of the sugar are impeded. litmus also to A juice limed to neutrality usually settles settles rapidly,with slight overslowly. The precipitate or In the a juice. bright manufacture leaving under-liming, of The

raw

proper

sugar

the

lime

precipitate,but dark-colored

no

should more

sugars,

be

added

should

however,

long

so

be used. more

lime

In

as

making is used

required for the clarification of the juice. This prejudicialto the yield of sugars. In

the

manufacture

of

white

or

it produces

a

certain than

is undoubtedly

yellow clarified sugar

is

CLARIFICATION

WITH

41

TANKS.

OPEN

ft

using sulphurous acid, the to neutralityto litmus

The

be

limed

nearly

paper.

of the juice and the blanket appearance of the suspended matter in a observed as

motion tube

juice should

and

the

glas^test-

usuallysufficient guides for an experienced defecator The should move particlesof suspended matter

are

man.

surface

liquid at the sides of the tube, and descend promptly at the center, forming a compact These be tests cone. supplemented, in- daylight, may of very sensitive litmus paper. to advantage by the use rapidly toward

the

of the

be quantity of lime required in the defecation may ascertained by a titration of the juice with a standardized The

solution

saccharate

calcium

methods

other

or

acidimetric

methods.

work usually employed in raw-sugar only in and then control. a laboratory occasionally of the factory,the sugar-maker In conducting the work such quantity of lime to the juice as his experience adds Such

indicates tors

are

approximately correct;

be

to

been

have

may

it, by the

from

filled before

only,

eye

of litmus

he

or

heat

can

the

gauge

two

lime

three

defeca-

first and

the

for the

others.

in

daylight,he can test the juice and from this in the first defecator, immediately it is filled, test modify the alkalinityof subsequent portions of juice, until the liming is properly adjusted. As the changes of be well observed not litmus paper can except by daylight, be slightly acidulated phenolphthalein solution may a in testing a few used drops of juice in a white saucer. color reaction is plainlyvisible by artificial light. The in raw-sugar In liming juiceto alkalinity, work, samples of By

means

juice,filtered through

defecated time

paper,

with

time

to

a

solution

paper,

of

should

saccharate

be tested of

from

lime, in

a

precipitate is produced by the saccharate, lime should be used in the defecation,and, vice versa, If

test-tube. more

is

if there

It is the

the lime should be reduced. precipitate, usual practicein Louisiana to use the same tank,

no

coils and

fitted with and

darifier. that

is then

a

the

boiled

off the

The

steam-jacket, as both defecation is accomplished as not

blanket

a

is

immediately removed

briskly,the workman scum

that

rises.

This

at the

same

defecator

a

above

and time

the

cept ex-

juice

ing'^ "brush-

latter part of the process

42

liANUFACTURIMO

is

properly termed is

this word

the

applied to

PROCESSES.

''clarification/' though in Louisiana entire process.

the

In addition to the defecation clarifiers

darifier is clear

The

eliminators

or a

tank

it is boiled and

where

already described,

as

The

frequentlyused.

are

steam-coils

fitted with

juiceis drawn

process

from

ordinary a mud-gutter. into the clarifier,

and

the defecators

skimmed

and

is then

into

run

settling-

tanks.

English eliminators differ from the ordinary darifier in having a steamnnanifold, with the steam-inlet and waterThe

is thrown side of to one arradged that the scum handinto a trough, and the juice requires no the tank method avoids in skinmiing it. This labor boiling th*e with the juice while from the defecation mud clarifying. minute In the elimination a total boilingduring one process outlet

so

usually sufficient.

is

It sometimes

impurities separated in the settle promptly in the settling-tanks, that

occurs

clarification will not This

be due to the condition of the cane, may of sirup tank-bottoms usuallyarises from the admixture

subsiders.

or

but

juice in the clarifiers. Thorough agitation of the wise, layers of juice with a long-handled paddle or other-

the

with upper

or

more

spraying of the surface with cold water, will Cold water the impurities to promptly settle.

liberal

usually cause is

the

effective than to the surface

scum

modification

A

is

stirringof the juice. The

probably due

of the defecation

rise of the

the presence of gases. process consists in boiling to

to the juice and scirnis, instead of only heating them cracking-point, and running them into settling-tanks. All of the of the separated impuritiessettle to the bottom scum remaining on the surface of the juice. tank, no

the

In

oonneetion

is sometimes

the

diffusion process

accomplishedin

quantity of lime the

with

battery, and

is added

the

to the

the

diffusers.

The

at

requisite

their way

cane-chips on

the diffusion is conducted

defecation

a

to

high enough

The coagulate the albuminoids. caneall the of act as a filter, retaining impuritiesseparated chips hence neither in the defecation, defecators nor filter-presses are required. is used in liouisiana in raw-sugar Sulphurous ftcid-gas

temperature

to

44

PB0CBS8B8.

UANUFACTUBING

juic" entering the toward about

gallons should the

the outlet.

inchcfl

4

in

25

Bquare

of

actual

feet

writer

of

the

heating surface

below.

in

now

and

These

tanks

have

use

tank

While

a

it has

the advantage

In

tar

so

veyed The nde

deep

as

from

provide per

the

tank.

of

the

tank

bottom

and

of copper

in

rectangular

a

imately approx-

1000

U.

Hie to

coils

facilitate

the draw-down

requires of

a

described

arrangen^ent

be of very

may

tank, with

drfecating

large capacity. in

rather

excess

long

of 6000 time

for

yielding a small proportion

Many gallons.

settling, of mud.

possible, it is preferable that the juice be the

draw-down

outlet'^lbow.

8,

11.

woriiing capacity

a

be

ward for-

mud.

prefers

comers

should

and

the mud

to cany

coila should

The

Fid.

rounded

t^nds

juice capacity

of the

removal

rear

diamel^

well above

be

The

at the

tank

ddecators

arrangem"it with

a

through is shown

pq)e-4iius rather in Fig. 11.

cot^

than

AtAiaa,

ventilating pipe,F, lekdiugabove

the

CLOSED

HEATEBS

top of the tank.

CLOSED

AND

45

SETTLERS.

drawing down, the juice flows through the nipple,the elbow, A, and the cross valve,B, into the small collecting-boxand thence to the trunk line,D7~ The angleIn

before drawing down the valve, C, is opened for a moment that may have settled in the juice,for the removal of mud the outlet-nipple. The valves, pipe-lineor that may be near

B, C,

are

G is used

controlled in

from

the

The

working-platform H,

washing the mud

into the main

line to the

valve scum

It will be noted that the pipe is ventilated to tanks, E. prevent sjrphoning and that the juice therefore stops flowing its level reaches

when

pipe and

insure that advisable each

mud

no

that

be drawn

can

down.

juice shall be drawn

to

locate

about

of the draw-down

of the bottom

three

The below

from

four

or

elbow the

centers.

The

inches

above

the bottom

should

be about

nipple It is

scum.

draw-down

defecator,with difference of level of about between

and

pipes in inches,measured

4

pipe should be about 12 of the tank. The draw-down pipe

3.5 inches

lowest

in internal diameter

in

defecator

a

gallons working capacity. If the juice has been properly limed and heated, there is no probabilityof drawing down mud, provided a sufficient settlingtime is allowed. Ample tank capacity and proper supervisionof the liming are essential. Eight 5000-gallon tanks are sufficient for a grinding capacity of about 1400-1500 tons of cane per day. Defecation Closed Heaters and 11. Using Closed Settlers. 's Process. This vented inwas Doming process by M. A. Scovell in a sorghum-sugar factory. The purchased by Deming, who developed the procpatents were ess of

4000

"

and is

made

it available

in

adaptable to The juice is limed

in the

cold

in

Deming's

Milk tank. of single constant-flow juice'at the heater-pump intake and it in the pump juice is heated to

with

and

an

lime is

it parts with the

method

in

process,

flows

into

a

the

thoroughly mixed

in transit to the heaters.

approximately 235"

eliminator,where concentrated, and warms

into

This

practicalwork. factories of all capacities.

F. and the cold

The

limed

passed is slightly

is then

gases,

incoming juice on its way eliminator is a cylindricalclosed-ironThe to the heater. and is provided with a large vessel with a conical bottom tubes. Cold juice circulates heating-eurface in copper

46

FROCBSSBS.

BfANUFACtURING

through the tubes and condenses the hot

juice enters 'Is

vacuum

and

other

produced by

withdrawn

are

gases

the

air

juice. The

hot

with

tial par-

the

the

or

pump

a

system.

vacuiun

The

juice should be reduced here it is pumped From

of the

temperature

F. in the eliminator.

210"

from

is connected

part of the eliminator

upper

and

this condensation

the

A

of the eliminator.

section

the lower

set free when

steam

ii

settler

I

A

I

^

into the

A, of the closed

compartment,

outer

to about

pressure-separator, shown

or

Fig. 12. The oflfcontinuously from

diagrammatically in

^

mud

is drawn

the conical

bottom

and

the clear

the

central

of the

tank

at

C

juiceis discharged from cone,

B,

In

tories fac-

many

using Deming's heaters and the juice is heated to only settlers, 212"

to 218"

In

.

^

j_.

^^ W

.

.

his first

these

experience with

tanks, the earUest Cuba, the writer

of their noted

type that

in the

//

mud

^/

cating operating had an offensive odor, indiately decomposition. He immediinstalled very slowly moving

drawn

scrapers

mud

Fig.

F.

ofiF after several

in the tanks

from

to

prevent the

settling on

bottom

of

the

nearly

eliminated

hours'

separator

the and

conical thus

decomposition.

12.

Certain

resist the

perature high temof the heater and the decomposition. In cause Cuban to liquidateand clean practiceit is found necessary be practicable. (See 35.) the tanks as often as may 11a. Cleaning the Heatlng-siirfiices of Defecators. The heating-smfaces of juice-heatersand defecators usually incrusted with scale,impairing their efficiency. become soon

The

of copper-surfaces

the

spores

ordinary double-bottom

defecators

usually kept clean by washing with water and scrubbing after each use. Long-handled brushes, made of maize them husks, are used in Cuba in this.work. It may occur in scHoe are

SULPHITATION

localities that the laborers with

brushes.

In

with

.covered

OF

PROCESS

unwillingto clean the defecators

are

this ev"nt, the

water

muriatic acid

for use usually'sufficient

are

in

gallon defecator. "The heating-surfacesof coiMefecators juice-heaters foul

with

defecation

whole

but

little.

is

process

muriatic

acid

lightchain

and

the

dilute

circulate hot

to

follow

muriatic

which

the

require frequent in

defecator.

Juice-heaters usually foul very tubes

in

be

cleaning,as

When

the

cleaned

in

coils

by drawing

the surface.

over

cleaning is

1000-

in combination

Those

is used

may

cleaninga

used

conducted

cleaning. Dilute the ordinary double-bottom much scaled, these are very

of

should be

bottom

copper

strongly acidulated with hydrochloricacid the solution boiled. Five to six pounds of the commercial

and

a

47

LOUISIANA.

quickly. The

caustic-soda

this first with water The

acid.

soda

usual

solution and

then

may

be

solution

method

through with

hot

returned

storage-tank for repeated use, decantingit from the mud and adding caustic soda from time to time to maintain a strength of about 1 pound of soda to 7 gallons pf solution. to

a

Occasionally the scale in the tubes is of a very resistant and must then be removed nature by scraping the surfaces. is properly adjusted to the volume of the If the tube area juice, so as to force a very rapid current, the scalingis much reduced.

12.

of the

Sulphitation

PROCESSES.

of Loulsiana.-^This

Process

is

one

and when fully skillsimplest of the sulphitation processes conducted good, though irregular, produces a very

qualityof The

WHITE-SUGAR

IN

DEFECATION

cold

"near-white"

or

"off-white"

sugar.

through a sulphur-tower or and through a current of sulphurous

raw-juice is pumped

box, in opposite direction acid

gas.

The

to

juice should

absorb

as

much

of the

is followed by liming to possible. This sulphitation slightacidity to sensitive litmus paper and the juice is very tion th"i heated, settled and decanted, as is usual in the defecaThe juice is usually reheated to boiling and process. then brushed before settling. Evaporation to sirup follows. This brushing factories boil and brush the sirup also. Many gas

as

is

48

PROCESSES.

MANUFACTURING

since

it entails

large consumption of loss of sucrose. fuel and Heating to the boiling"pointis concentrated suU sufficient. The juice is also sometimes

is

a

wasteful

process,

phited. is

This

a

old process,

very

English or French colonies. has always been the custom

and It

possibly originatedin the is interestingto note that it

to work

the

coloration

sensitive

litmus

condition

corresponds to the essential

acid

the

of one

This

sugar.

of the recent

Java

thin-juiceprocess.

Reserve is very

box

prevent

to

juicefaintlyacid* to

(Louisiana) White-Sugar with

strongly impregnated cast-iron sulphuring-box

is

3 feet cylindrical,

of

Process.

"

The

juice

raw

sulphurous acid in cascade

the

in diameter

by

26

feet

a

type.

tical ver-

The

high. This

has sufficient

capacity for 2000 tons of cane per 24 hours. The sulphured juiceflows from the box into the liming-tanks, to it in sufficient quantity to milk of lime is added where reduce the acidity to the equivalent of 1.2 cc. of N/10 soda 10 cc. of juice,using phenolphthalein as an indicator. per box

juice is

The

next

heated

in

a

tubular

heater

to

212**

F. and

settling-tanks. through Deming's continuous have hot juice should The an acidity to phenolphthalein equivalent to .85 to .9 cc. of N/10 soda per 10 cc. of juice, and is then strictlyneutral to htmus. Phosphate of soda the to the juice flowing into the settling-tanksat is added 1000 rate of 1 pound per gallonsof juice. This phosphate and has the of soda is especiallyprepared for the purpose same aciiity as that of the juice. No lime is added to the it then

mild

flows

filtrate from the filter-pressing.The the juice flowing from the settlingto is added presses is passed through bag-filters.The and the whole tanks acidity of the juice remains equivalent to from .86 to .9 cc. N/10 soda per 10 cc. of juice. This is not sufficient for a high-grade sugar, hence the juice is again sulphited and the

preparatory

acidityis raised

to

to

1.2

cc.

juice is evaporated to a sirup of 54.3" Brix. The sirup is perfectlybright and itiscolor is a dark yellow. furthe* precipitationif heated to the boilingThere ?s no point. The sirup is boiled to massecuite, as is customary The

in

clarified

white-sugar manufacture.

SULPHITATION

AFTER

high acidityof the juice as

The

is

work

Harloff*s

compared with that

quite noticeable.

this is usual in Louisiana

49

LIMING.

in

previously stated,

As

practice.

This differs Liming. process from the preceding in adding the lime, in large excess over that required to neutralize the juice,before sulphitation. Approximate

Sulphitation

13.

after

"

gallons of milk of lime of 26.5** Brix is used, thus producing a very heavy precipitatewith the sulphurous which be readily removed acid and by setthng and may decantation. If a largerquantity of lime is used, e. g,, 10 to 12 be removed by filter-pressing. gallons,the precipitatemay 8

sulphitationis continued

neutralityto phenolphthalein. The decanted or filter-pressed juice,after concentration and to sirup, is usually cooled sulphited to slightacidity The

to

acidity equivalent to that required in

An

neutralize

25

to

30

cc.

of 100th

normal

10

of

cc.

alkali is

sirup

to

suitable

a

amount.

Bachused

in

Lime

Sulphitation Process.

8

Java,

is added

under and

"

the patents

This

process

of its

inventor,A.

is

extensively H.

Bach.

is

precipitated by sulphurous acid at and decantation two or stages, each followed by subsidence lime is used than in Very littleif any more by filter-pressing. the process described in the preceding paragraph. 5 to 7 gallons of milk of lime of 26.5" Brix is added From 1000 each phited to gallons of cold raw juice. This is then sulto neutrality to phenolphthalein and finallyheated in the to full boiling,settled and the clear juice decanted as The clear juice is evaporated to the ordinary defecation. density,approximately 55" Brix. customary sirup obtained

The

and

cooler

per

above

its temperature

factory's water lime

as

described

is reduced

supply. From 1000 gallons are now

16 to

added

is

to

17 to

passed through

about

that

of the

gallonsof the toilk it and

a

it is then

of

sul-

neutralityto phenolphthalein, or the full quantity be added to the sirup of sulphurous acid in solution may Since the volume of the sirup is about 30 prior to the lime. of milk per cent of that of the originaljuice,the total volume of lime used per 1000 gallonsof juiceis from 10 to 12 gallons. the foam phitation. Steam during the suljets are used to beat down The sulphited sirup is heated to about 194" F.

phit^

to

50

MANUFACTURING

(90**C.) and

PROCESSES.

The press-cakeis washed filter-pressed.

is

with

in the press and a large part of the sugar it contains is recovered. The filtration is rapid and the cakes are firm and water

well formed. The

filtered

therefore

sirup contains

heated

to about

**

195

bi-sulphites. The

heated

tanks, and liquoris decanted

and

some

bisulphiteof lime and

F. to

decompose

this and

is

other

sirup is usually run into settlingafter the deposition of the precipitatesthe clear cooled

and previously,

as

phited to distinct acid reaction then ready for the vacuum-pan. Bach's

is sometimes

process

is

modified slightly

by separating mixing and filter-

precipitatesby decantation and pressingthem together. This process requiresapproximately 0.055 the

sul-

phenolphthalein and

to

all of the

on

is then

weight of the

The

cane.

sugars

phur of sul-

cent

per

of

are

good

quality. PROCESSES.

CARBONATION

with which caneThe ease Preliminary Bemarl^s. and sulphitation juices yield to the ordinary defecation 14.

"

processes

retarded

has

it

Java, where

in

even

of the carbonation

extension

an

has

its

ess, proc-

largest application.

extensive Department of Agriculture conducted manufacturing scale with carbonation a experiments on and of sorghum-juices in Kansas cane-juice in Louisiana, writer was The active in this nearly thirty years ago. experimental work with Dr. H. W. Wiley, then Chief of the As the Government Bureau of Chemistry. reports, show, these experiments were satisfactoryfrom a manufacturing, but not financial point of view. They brought out the necessity

The

U.

S.

of carbonation

well below

60"

C, as is practiced in Java, though this possibly originated with now the French in the early Spanish installations. There

are

and twice lime

the

by

a

lime

In and

second

the

is saturated

double

removed carbonation

viz.:

processes,

carbonation,in which

gas.

is carbonated

followed

carbonation

all the added

the double

with

temperatures

distinct

two

single,in which

at

the

process,

in

one

tion, opera-

juiceis treated a

part

by filtration and in which

the

the

of

this

the is

remaining

52

MANtlFACTURING

forming the

carbonate

PROCESSES.

and

lime

and

that

foaming begins and

renders

then

viscous.

juice very

the

sucrocarbonates

forms

It is at

with

it increases

the

of

this stage increase

of

is

always danger of forming darkcolored decomposition products with the glucose when steam sucrocarbonates.

is used

There

down

beat

to

this

Further

foam.

there

be

shown

to

excessive

rise of temperature,

which

be

very

objectionable. The

carbonic

gas

of by the bubbles in the juiceand the violence of the frothingare indications with

lime.

the

sound

of the progress

the attendant

to

The

will later be

may

acid

bines 4;raduallycom-

made

of the carbonation.

of gradually rises during the progress the carbonation. During the early stage the temperature should approximate 46** C. and should nearly reach 55" C. is not used when all the lime is precipitated. When steam The

temperature

frothing,the rise is not sufficient for the final stage of the process. neutrality of the juice to Therefore, when is nearly reached, sensitive phenolphthalein paper very into the heating-coilsand the temperature is turned steam to reduce

is

gradually raised

lein paper heated order

to 65" C.

(Dupont

to 70"

to raise the temperature in It is necessary and the sucrocarbonates to facilitate up

C.

break

to

filtration of the

Finally when the phenolphtba^ paper) indicates neutrality the juice is

juice. The

attendant

may

note

approac"ing

of the neutralityby the "spoon test," i.e.,the appearance The precipitatesseparate sharply juice held in a spoon. the latter has an from the juice when alkaUnity equivalent to

approximately 0.04

per

cent

calcium

oxide

or

often

as

lime per litre. The expression "equivalent" stated 0.4 gram is used here because the alkalinityis partly due to potassium

hydroxides, formed by the action of the lime upon and potassium salts of the juice. The spoon*test the sodium be followed by frequent tests with the phenolphthalein must (Dupont paper) until neutralityto this paper is reached. paper The bonated juice is then heated to nearly 70" C. and is over-carand

sodium

during

a

few

very

lime

alkalinityarising from carbonic

the on

acid.

In

beet-juicesallowance

than

due

to

lime,

to

seconds that

to

has

not

practicingthe must

avoid

be

made

neutralize been

slight

attacked

carbonation for

the

by

process

alkalinityother over-carbonating. This is not

SINGLE

in

usuallynecessary occasional

work, but it is advisable

cane

to make

potash alkalinityto be prepared

for

tests

53

CABBONATION.

to

rect cor-

for it. The

is the

stage of the process

next

dressed are filter-presses defecation

with

cotton-cloths

heavy

cotton-cloths

Thin

process.

The filter-pressing.

are

in the

as

usually placed

Three suits of heavy cloth to protect it from wear. heavy cloth are usually consumed per five suits of the thin. the

over

is turned

Steam

into

off until it escapes of this

steaming

the

before

press

the

freely from

and

use

is not

juice-cocks. The

shut

object

is to

of destroy bacteria,which, on account the low temperature of the material to be filtered, would otherwise be very active in destroying sugar. carbonated The juice is pumped into the presses at pressures about

to

up

juice should

The

lbs. and

45

flow

should

filter very

rapidly.

freely from the cocks and the and tions, granular. Contrary condi-

very

press-cake should be firm sluggish filtration and a pasty press-cake indicate the of too little lime or an imperfect carbonation. The work use is the best indication

of the filter presses

the press

to

low

a

filter press-cake is

The

manipulations.

of correctness

usually washed

(See under

content.

sucrose

of the in

filter presses,

67.)

page

The

filtered

juice is sulphited,concentrated, etc., as in the

sulphitationprocess. De

Haan's

Single Carbonation

modification

Haan,

of the

carbonation

process

Klaten, Java, and. is in

his technical This

Process.

"

important

is due

in several

use

This to

J. S. de

factories under

direction.

fies consumption of lime and simplithe equipment without the quality of the sugar sacrificing product. The alkalinityof the juice is kept within very limits during the carbonation. moderate The raw juice is heated to 45"-50** C, and then a small stream

process

reduces

the

of milk

of lime

and

turned

into

carefully regulated so very closelyto has 35.7"

been Brix

added. is from

The 4 to

the

it. as

0.25

The

carbonic-acid flow

usual 5 per

cent

total cent

lime

are

and

taneously simulgas

is

alkalinityapproximating until all the lime required

to maintain per

of the

gas

an

quantity of milk of lime of of the volume

of the

juice.

54

MANUFACTURING

PROCESSES.

*

Approximately used

are

1000

p6r

carbonic-acid

of lime-stone and

20 tons

The

gas.

neutralityto Dupont The injectionof the is reached.

of

tons

and

The

into

carbonate

the

discoloringit. The juice is

from

is

gas-coke

continued

now

juice is heated

the

is continued

to

to 70" C.

rainute after

trality neu-

object of this over-carbonation

is

prevent particlesof lime

to

of

producing the lime and

carbonation

paper gas

in

cane

1.8 tons

that

one

have

been

not

converted

r^idering the juice alkaline

and

in the preceding process. filter-pressed as is approximately 1.7 square The required filter-cloth area feet in a frame-press per 1 millingcapacity-ton of cane per now

day. to sirup and, after cooling, juice is concentrated is sulphited to an acidity equivalent to 25 to 30 cc. of alkali per 10 cc. of sirup. lOOth-normal

The

filtered

16.

Double

methods

are

Carbonatioii based

upon

the

in

treating beet-juices. The

in

cane

factories

Process.

^All carbonation

"

original French double

differs from

the

process

process

modem

as

beet

used

applied method

only in the temperature of the operation and in carbonating to neutrality to phenolphthalein paper (Dupont paper). From 7 to 10 per cent by volume of milk of lime of 35.7" Brix is added is warmed to the juice,which 113** F. to about is then conducted The first carbonation (45" C). precisely method in the single carbonation as (15) up to the point when the spoon test shows a sharp separation of the precipitate chemical from the juice or a test shows about 0.04 per cent alkalinity. Shortly before this alkalinityis reached the juice is warmed to a temperature of nearly 55** C. and is then filter-pressed.Nothing would be gained by continuing the gassing to a lower alkalinitythan 0.04 per cent. With this alkalinitythere is no danger of redissolvingparts of the precipitates,the juice filters very freely and sufldcient lime is left for the second Lime the

may

or

may

first carbonation

juice usually contains error, the

carbonation not

or

be added

preliminary

saturation. to

the filtered

to

the

sufficient lime

gassing has been

pushed

too

saturation.

except far.

juice from This

when, through The

second

car-

harlopf's

acid

55

process.

thin-juice

.

bonatipn

proceeds

very

rapidly, without

foaming, and

is

The pushed to neutrality as in the preceding processes. juice is finallyheated to 158** F. (70^ tD.) preparatory to and before discharging from the tank should be filtration, gassed for a few seconds to prevent deleterious action of have been occluded in the particlesof caustic lime that may precipitates. The saturated of the condition of the juice,on account is precipitates,

shallow

filters or purpose

The

with

a

filter press

means

The

filtered under

frame-presses

pressure

with

low

very

of but

are

4

gravity pressure

filtering. object in conducting the

to

Gravity

pressure.

usually used for this 5 pounds. (See 24.) is the

more

economical

of

process

in two

stages and

the stronglyalkaline juicefrom the firstis the removal filtering that are tion. of substances or soluble; slightlyso in neutral soluAmong these substances are magnesia, usually largely derived

lime-stone,the oxalates and possibly other organic salts and substances, such as coloring matters, that held mechanically by the precipitates. are the second filtration are The precipitatesfrom usually and are mixed with the juice going to the first filter-presses from

the

subjected to washing with the press-cake. Sulphitation of the filtered juice from the second carbonaand as recomtion is practiced as in the previous processes mended by Harloff in the following paragraph, and it is concentrated then to sirup. The sirup, after cooling, is usually sulphited to an acidityequivalent to from 15 to 30 cc. of N/100 alkali per 10 cc. of sirup. thus

17.

Harloff's

Acid

Thin-Juice

Process."

Harloff's

experience in Java led him to a study of the influence upon the juice,sirup,and consequently the sugar, of various salts, and the especiallythe potassium sulphites and carbonates corresponding salts of lime and iron. These studies led to a juice or the general practice of sulphitingthe raw very carbonated juice to acidity to phenolphthalein in the Java factories.

The

writer

visited many

factories in Java

in the

and, with very few exceptions all sulphited to sulphitesirupto to acidity. It had long been the custom acidity,but not the juice. summer

of 1913,

56

PROCESSES.

MANUFACTURING

importance, Harloff ^ found that sulphitesdo not clarified juice containing glucose on heating and that

Of most darken

do.

carbonates in

far

BO

as

may

This

led

be

all the

the

to

natural

salts should

conclusion

that

converted

into

be

them. He sulphites,since it is impracticable to remove accomplishes this by sulphitingto neutralityto litmus,which corresponds to slightacidity to phenolphthalein. Further,

salts,if present in the

iron

in

carbonated

or

reduced

are

juicesby the sulphurous acid and in acid

so

salts

These

the ferric state.

raw

with

the sugar

Litmus

The

solution.

state

remain

crystallizeout

hands

the the

night

at

of

laborer.

a

of the Vivien

use

The

tube

is filled to

the

strument in-

Harloff

tube. Fig. 13, in beet-sugar

employed largelyin France

is

when

or

uncertain

therefore,is an

and

poor,

recommends

work.

salts do not

ferrous

in

which

colorless and

conveniently used

be

lightis

the

to the ferrous

in

acid solution.

from

cannot

are

juice,are

mark

zero

with

phthalein, potassium hydroxide containing phenoland sulphited juice is added until the red color is discharged. If, for example, the requisitequantity of juice to discharge the color N/100

25

is 10 of the scale 20

the Vivien

on

tube and

a

smaller

"

obtained, the juice is too acid and the be reduced. injection of sulphurous acid must should with Check tests occasionally be made juiceneutralized to litmus in daylight. Obviously control could be used, but this is not burette a quite so easy a manipulation as with the Vivien number

15=

10

"

5 =

is

tube, 0==^

recommends

Harloff

precipitatesbe

the

than Fig.

13.

above

the custom

with

work "W.

Norman

study

H.

an

Harloff'8

Th.

Rodger, of carbon

acid

London,

ation

and

the

juicemixed

heated

to

a

higher

C. (194" F.) in closed

90"

with perature tem-

heaters

ing foulingthe heating-surfaces.Heat-

this temperature

It has been to

of

account

on

not

that

should

for

a

be in open

great

many

juicesimply because "Plantation should

be

White consulted

sulphitation in the

cane

tanks.

years

in Louisiana

with

this condition

Sugar

Manufacture,"

for

a

very

industry.

thorough

WIJNBERG^S

and the color of the sugar is better,

apparentlywith

definite

no

Harloff's investigationsshow why this is true. clearlywhy the sugar is better.

idea

to

as

very

calls attention

HarloiT

evaporators, to

57

PROCESS.

NORIT

litmus.

the

on

that

also states

He

and

boiler-feed

The

side, when

vapor

this condition

under

the. corrosion

to

of the tubes

the

the

juice is left acid

return

waters

damage the tubes of the should

water

be

of the

are

ers. boil-

steam

rendered

acid

slightly

sulphitationis practiced. * Norit Process. The juiceis defecated

alkaline with soda when

Wljnberg's

18.

"

ordinary raw-sugar except that lime is process, added to slightlyshort of neutrality. Ten per cent or more the apparent solids in the juice,is of "norit," figuredon added to the decanted juice. The reaction of the juice to litmus must remain acid,and, if not so, phosphoric acid should The be added. juice is heated to boiling-pointand filterthe

in

as

is sweetened

pressed. The

cake

boiled

5 per

with

a

cent

caustic

washed, and is finallywashed norit is then ready for The is rebumed

norit

in

a

kiln.

manufactured

color,but 19.

a

Factories

of very

by a secret large part of the

Remarks

upon

After

several

uses,

the

sugar.

high decolorizingpower It not only process.

and

is

removes

gums.

White

Sugar

producing plantation white "near"

is then

sirup from juice treated the addition of kieselguhr and is

ready for boilingto white carbon

and

The

then

a

is usual

soda

re-use.

norit is filtered with

is

as

solution,filtered and with diluted hydrochloric acid.

with

Norit

off

"off"

Processes.

sugar,

with

few

"

ceptions, ex-

white

product as compared standard American refiner's with the granulated sugar. In occasional "runs," however, in well-equippedfactories, from refined the product is almost or quite indistinguishable make

a

or

sugar.

quaUty of produce a perfectly uniform in the factory owing largely to the variable purity of sugar with many material. the raw Judging from conversations by the carbonation producers of white sugar, that made uniform quality than by the exclusively processes is of more It is difficult to

Unt. .

relative

Sugar to

Journ., 1912, 720;

patents.

1913, 248

and

404;

1914, 488, all

r

58

MANUFACTURING

PROCESSES.

latter are

The

sulphitation processes.

usuallythe cheapei

processes.

is

There

a

rise in the coefficient of

marked

purity of the

This rise often exceeds juice in the carbonation prqcess. two degrees. It is a true rise and is reflected in an increased The rise of purityby sulphitation is not so yield of sugar. Haan carbonation and de claims that the latter great as. by than 2 per cent increases the yield of sugar more process than justifies the increased sulphitationprocesses and more over cost.

is considerable 'difference of

opinion as regards the of making as white a product from the very darkpossibility colored canes from the lightyellow and so-called white as The effect of the dark color is reduced by increase canes. There

in the

of lime

defecation

It is very produced from the

processes. are

attention

Great sugar

manufacture.

as

in the

carbonation

probable that the canes. light-colored

and

best white

Bach sugars

to detail is essential to successful white-

A

Uttle carelessness in the carbonation

sulphitationand filtration will result in a poor product. Double reduces purging of the sugars in the centrifugals the risk of stainingthe sugar through the necessarily imperfect removal of the molasses. Thorough cleanliness from start to finish is very essential;not only from the point of view of color, but also of yieldof sugar. or

SPECIAL

APPARATUS

USED

IN

THE

SULPHITATION

AND

ATION CARBON-

PROCESSES.

20.

These

Sulphur

Stoves

or

Ovens

and

Sulphitors. "

of two

general types: (1) Those employing induced draft and usually used in connection v/ith sulphur-towe or boxes; (2) closed stoves, Fig. 14, into which compressed air is forced and which deliver the sulphurouastoves

acid gas

are

under

pressure.

These

are

used

with

all types

of

sulphitors. In the first type the draft is

usuallyinduced by a steamejectorplaced on the sulphur-box. Air is drawn into the the burning sulphur and the sulphurous acid stove over is drawn produced by the combustion through the juice fallingfrom shelf to shelf in the box. The surplusair and k

60

MANUFACTURING

The with

Louisiana

usual

induced-draft

the

PROCESSES.

sulphitoris described

Sulphitation tanks

stove.

forms, but the usual provided with a cover

in connection

is

of

are

moderately deep ironand chimney to the outer air, tank suitable test-cocks,valves, and a tributing perforated pipe for disthe sulphurous-acid gas: The pipes and tanks should be arranged to facilitate cleaningat frequent intervals. is preferablyconical. Perforated pipes for steamThe bottom foam should be provided in sirup suljets to break down many

one

a

phitors. Where the tank is used to saturate large quantities of lime, as in Bach's process, intermittent work is advisable, and at least three tanks should be installed, otherwise a single tanks Two continuous be sulphitationshould be used. may used in this method, though one deep one with more very The careful manipulation will answer. juiceenters the first and is sulphited to approximately -the tank at the bottom desired

and

the bottom the

second

filtersto 21.

and

overflows

test.. It

the

enters

second

tank

at

ifesulphited to the required acidity. From the

juice flows through juice-heatersand the charge-tanks of the evaporator. tank

Carbonation-tanks.

iron and

should

be

"

than

The

carbonation-tanks

are

of

feet in

depth for the first otherwise should be provided with perforated carbonation or to break down foam. pipes f6r steam, carbonic acid or air-jets The tanks should have sufficient steam-coil capacity to heat and the juice quickly. The carbonic-acid juice-connections for should be large to provide A first carborapid work. nation should

more

requireabout

three to five minutes

ten

20

minutes

and

a

second

about

for the

gassing. led into the juicethrough perforated Formerly the gas was tions pipes. Such pipes always give trouble through incrustarecent In more of lime. practicethe gas enters through largepipe in the conical bottom of the tank and is deflected other device, so arranged as at intervals by baffle-plates or acid. There to insure thorough distribution of the carbonic methods of arranging the pipes to reduce the scaling are many and facilitate cleaningthem. a

carbonation

Continuous of the process.

email

and

with

The a

is advisable

quantity of lime suitable device

for

the

second

to be saturated

the

stage is very

outflowingjuice is

61

LIME-KILNS.

readilycarbonated continuous

point.

to the demred

carbonators

Descriptions of them

the market

on

There

several

are

d"signed for beet work"

will be found

in many

works

beet-

on

sugar.

If intermittent

Ume-kllns.

22.

kiln, as

machinery

all other

the

identical

The

kiln proper of

cone

is 25

from

specialcontinuous

a

carbonation devices

top through

to 30

sulphHation

and

that

are

kiln.

used

in beet-

and

of

kiln at

the

is fed

coke

into

the

conical

door. Three distinct self-closing in the kiln,viz. : (1) at the top, the fresh

a

maintained

and

unignited coke; (2)

and

dissociation

that in which

high and is the frustum end the small upward.

feet

angle with

narrow

of lime-stone

mixture

are

in

is obtained

manufacture.

sugar

a

acid

carbonic

^The

also

are

practiced,the tanks there is littlefoaming.

as

calcined by coke-fires

lime-stone This

"

is

carbonation

comparatively shallow,

be

may

second

at

the

middle

(3) below

zone;

the resultant

is the

A

zones

stone

combustion

combustion-zone

the

lime is cooled and

drawn

is

off.

'

usually built of the Belgian type in which the body is supported upon four short columns, leavingthe bottom stand and free for the discharge of lime. The columns open Kilns

are

Stone platform upon which the lime rests. this platform to support the kindling and mix'is piled upon and coke, when the kiln is put into commission. of stone ture the firingprogresses and the lime is produced this stone As is removed from time to time and finallyits place is tak^i concrete

a

upon

openings, by quick-lime. The kiln is provided with numerous having tight-fitting plates or doors, for use in watching the "scaffolds." of the firingand for breaking down progress draft is induced which The by the carbonic-acid pump, -

is located

A pipe the carbonation tanks. conveniently near leads the gas through a washer and scrubber and thence to

the

pump

The

gas

The the

which

discharges it into the carbonation-tanks. is thoroughly washed with water.

kiln must

lime

is

have

but

inlet for air,and

one

discharged. The

that

quantity of air drawn

in,"and,

therefore,the combustion, is regulatedby the speed carbonic-acid

pump.

It is evident

kept in thorough order and

must

that

work

this pump

with

where

of the

must

be

great regularity.

62

MANUPACTUBING

since the

of the

sucoeas

of dissociation

zone

PROCESSES.

carbonation

be maintained

must

essential conditions

The

above

depends

the

are

in its proper

deUvery of rich

of carbonic

acid and

30 pet

cent

gas

should

be

The

qualityof the coke and

it.

upon

The

place. ing contain-

gas

properly burned

lime.. The 276*

frequentlytested

described

as ^

stone

be controlled.

must

of kiln conditions following brief summary in the interpretationof analyses:

The

(1) The

oontainB

gas

oxide, and is indicated

at

a

point

a

If the combustion fast

too

low

between

the

is white

zone

of

will assist

little

oxygen,

of carbonic

percentage

the coke is too

or

large excess

a

in 275,

bonic car-

acid:

Leakage

and

the kiln.

gas-pump

hot the gas-pump is running The draw of lime should be

coarse.

increased.

(2) The carbonic

contains, too

gas

oxide

of lime

of stone

is excessive:

oxygen

nor

should

little carbonic add

be drawn and

coke

and

Smaller

pump

be

may

(4) The

contains

gas

quantity of incomplete and

normal, the coke is

fluctuating: irregularly.

and

The

combustion

acid

is converted

deficiencyof

of

account

on

acid is

of carbonic

excess

oxygen:

carbonic

slowly

too

an

too

coarse

contains

both

quantities

The mixture longer intervals. be investigated, the proporas tion

should

running

neither

at

of the latter may be too large. (3) The richness of the gas in carbonic The

and

of

and

the

into

other

oxygeu;

oxide

mal nor-

coke

is

monoxide

conditions

and

the pump

oxygen

and

being is running too

fast.

(5) The

gas

The

excess:

drawing The

circulation

American

forced

coke

and

the

in their kilns.

Java

Spencer,

"

Hand p.

qualities.

211, Also

The

in

sampler is

The

the

residuum

by the weight.

use

high-grade

cost of such

high

factories to substitute

oil-still residuum.

of 1 to 9.6-11 See

the

beet-sugar factories usually

ratio of 1 to 12 of stone

^

and

oxide

air.

some

metallurgicalcoke has

of the gas is slow

carbonic

cheaper

is used

Coke

coke

is used

gas-

in the in ratio

of stone. Book for

for

Chemists

o"

Beet

lime-stones

analyses of analysis of lime-stone,

this

Sugar and

a

work,

p.

Houses,'* discussion

386.

G.

L.

of their

PROCESSES

FILTRATION

AND

MACHINERY

"

Filtratiop.

23.

but

that

only

all

the

of

juice The

contains

fine

flocculent

addition

juice preparatory both

process,

juice and

the

the

In

varying

Sand

success.

filters but

sugars,

these

sulphitation

filtering medium

a

as

been

used

making

displaced by

with

results.

give good in

using

types,

many

have

used

been

have

none

filter-pressed. The

apparently

formerly

were

Bach

of

filters

filters

clarified

processes.

filtering media

other

or

Bone-black white

mechanical

years,

cloth,

sand,

be

carbonation

in the

carbonate

recent

the

may

the

upon

the

to

the

devised, but

been

sulphite supplies

precipitated calcium does

depending

In

sirup

process

obstructs

soon

processes,

practically successful.

been

has

ordinary

defecation

which

filtration,have

to

process

through

lignite,charcoal, etc.,

sawdust,

of

tates precipi-

carbonation

the

by

and

scums

the

matter

Several

cloth.

the

of

the

cane-sugar

filter-pressed,

not

readily filtered

clarified

juice

presses.

pores

be

may

in

With

defecation.

the

from

juice is

contained

portion

of

processes

clarified

entire

the

manufacture

usual

the

In

"

plantation ous-acid sulphur-

the

processes.

The

It is advisable

pressed. juice

and

thin

juice.

alkaline, 24.

kinds,

The

viz.

inside

:

(1)

of

filters, in which inside

of

the

Cloth

the

bag the

Filters.

"

filters,in which

Bag

water

outward;

filtration

be

usually

should

gain

to

Cloth the

the

residual

readily to are

the

outside

when

it. of two is from

filtration

(2) mechanical

is from

There

decanting

filters

in

both

the

added

in

clean

the

treatment.

filter-presses more

lime

Mechanical

a

settling it, and

and

mud

therefore

is

this

by

material

decant

There

by adding

of sugar

heating

again

mud

the

gain

additional

an

filtration

facility of

and

sugar

easily filter-

this

heat and

mud,

filtration.

to

preparatory

the

be

may

thoroughly

to

settle

"blowups,"

steam

is

juice tank-bottoms

and

scums

gravity

or

toward

bag. 63

the

64

PRQCESSES

FILTRATION

used

filters are

Bag

largelyby

and

outer

inner

an

and

in the

per

cent

mud

but

consists

little of

collects inside the

juice. Unless

bag it is evident that there is

the

refineries and

sugar-factory work of

more

or

The

bag.

of

case

MACHINERY.

filteringelement

Each sugar-factories.

in

AND

a

contains

this mud

an

bag,

about

80

is washed

large loss of

in with

sugar

these filters. filters

Mechanical

not

are

tion satisfactoryin the filtra-

very

The expense juicepurifiedby the defecation process. labor is very for cloth and large and the capacity of the filteris small. Bag-filters give better results for this purpose. filter may be used for filtering The mechanical juice from the of

carbonation, but

second

under

low

frames

ing work-

economical.

more

filter consists

mechanical

The

are

pressure

using shallow

presses

of

a

large niunber

of rectangular

Each bag or bags suspended in a closed iron box. independent discharge-pipe communicating pocket has an A

of it.

inside

the

with

metal

distender

collapsing. The clarified juice flows by gravity,under a low head, fillsthe box,

into

from

the

The

bags. time

from

mud

to

collects

mud

falls off.

time

the

on

The

is

pressure

to

sent

Filters, in

juiceand sirup are also be

may

The

used.

the

it contains

the

the

medium filtering is displaced with

filter will is

the

the

cloths

the

sand

mud

is

filters

for

Pulverized be

must

and

coke

of

grains

dog.

soon

clogged with

water

that

of the filter implies,

name

material filtering

size,otherwise

of uniform

When

As

use.

of

types

is fine, sharp sand.

filteringmedium

the

Several

"

filter

bags and

low

so

When the cloth. impacted upon foul, the flow of juice is shut off and the filter-presses.

Sand

25.

the

of the

outside

bags

filters into

and

is not

become

the

prevents

mud

the

the

juice

is then

sand

with hot water under or thoroughly washed pump-pressure otherwise, according to the type of the filter. After washing filter is

the

filters have

These the

again ready for service.

cane-industry. Many

have

been

26.

converted

Excelsior

Filters. "

The

used

been

with

of those

into the

moderate

installed

a

few

years

excelsior filtersdescribed

Filters, Bagasse excelsior filter was

Filters, etc. devised

in

success

ago

below. "

sior Excel-

in the Hawaiian

EXCELSIOR

filteringclaxified juice. A small tank, about dimensions for manipulatto 3 feet deep and of convenient ing about the filtering medium, is fitted with a false bottom

Islands 2.5

65

ETC.

FILTERS,

BAGASSE

FILTERS,

fcr

its bottom.

above

2 inches

A

jiice to the filter is connected and

tank's bottom

it at the

with

this inlet is placed

over

the force of the current

to break

pipe-linefor bringing clarified of the

center

small

baffle-plate and distribute the juice. An the upper edge of the tank to a

overflow-pipeis connected near lead the filtered juiceto the charge-tanks of the evaporators. filter is prepared for work The by packing it with the ordinary excelsior that is used in shipping merchandise. is placed on A wire screen top of the excelsior to prevent it from floating and to retain particlesof the material that might be carried along with the juice. A filter capacity of

approximately 1000

of

tons

cubic

150

feet of excelsior

is necessary

per

cane.

filters will

materially improve cloudy juice If the juice caused by defective Uming and defecation. has been properly limed and heated, but carries suspended These

cane-fiber,the filterswill greatlyimprove it.

and

matter

fenrentation

excelsior

the

of

advantage

An

not

serious

or

be washed

excelsior may

and

used

Fillers.

over

filter is its freedom

from

clogging with

precipitates. The in the filter or in an ordinary washing-machine and over again.

These

filters are

constructed

in

precisely the excelsior filters except that fine bagasse as the same way medium. When the filtration becomes is the filtering sluggish Bagaase

"

from bagasse is removed carrier for regrinding.

the filterand

the

material

This

contaminate it is

much

a

pulp

in have

a

and

defecation treatment gums.

ferment

to

juices during filtration. less desirable filtering medium way

found

Various

"

similar to a

small

with

little

process

by

some

fibers

excelsior.

are

For than used

Thin

and this

thus reason

excelsior. to

sheets

a

limited

of paper-

Granulated applicationin sirup-filters.

and

cork, asbestos used

great tendency

a

the

Filters y etc.

Fiber extent

has

the mill-

put upon

many

success.

cannot process

other

materials

have

been

Cane-juiceand

sirup by the be readily filtered, except after that

will

largely remove

the

66

FILTRATION

PROCESSES

old French

In ft very

AND

process, alcohol

sorghum-juice. Filtration

in

The

U.

MACHINERY.

used

was

followed

a

as

tant precipi-

without

S.

culty. diffi-

modified of Agriculture Department in adding an equal volume of strong alcohol to this process sorghum-sirup of about 55" Brix. A very heavy precipitate thrown down and was was consistingpartly of gums very The alcohol was recovered by filter-pressing. easilyremoved as is customary. by distillation and the sugar was crystallized forms of Centrifugal Separators. Several centrifugal separators have been brought out by inventors from time to differs from the ordinary centrifIn these the machine time. ugal in having no perforationsin the basket. The defecated of the mud juice without previous removal juice or even ^

"

(cachaza) is the

mud

The

basket.

into

run

the

is thrown

centrifugalforce and

The

of the

cost

machine

heat, oil,etc., are

the

to

the clean and

plant possiblythe

the

near

wall

bottom

of the

juiceflows

of

the

basket

by

the rim.

over

the expense

for power, loss of for the small extension

reasons

is good and the separaIf the defecation of this process. tion of the precipitatestherefore sharp, the centrifugalswill clean clarified

juice. 27. Filter-presses. Filter-presses are so generally used in the sugar industry that full descriptionof them is unnecessary. consists of number of iron Briefly,a filter-press a deliver very

"

plates and

frames

recessed

which plates over filtering cloths are placed. The frames and plates are supported oji and are' clamped together by a powerful a heavy framework the joints between the jack-screw. The cloth itself makes frames and plates. There two are general types of presses, the center-feed and

side-feed

The

hole

frame

or

center-feed

plates,with in

clamped There

cloth the

to

is

no

presses. up

opening in each

to

form

in the

of

and

heavy a

inlet channel.

the

plate at each

hole

made

are

presses

round

a

the

or

of these

cloth

in the

recessed

corresponding The

cloth

is

openings. frame-press. A

lug

projectsfrom each frame and plate and in each there is an Rubber opening to form the mud-channel. rings or cloth form between the the lugs. ''stockings" joints 1

See

the

reporto

of the

Bureau

of

Chemistry.

68

FILTRATION

of

capacity

PROCESSES

gallons

400

AND

cachaia

of

MACHINERY.

per

pr"es

hour

per

is

claimed.

KeUy

FUtcr-presa. filters

These

in 24,

filters,described

to the inside

outaidc

TTie Kelly, used

in

over

frames

with

a

netted mud the

Fig. 16,

the

latter into

the

discharge to

the

low

The press

at very

Sweetland takes

its

press, name

from

the

to

and to

time

and

mud

the

canal.

in

end

The door

of the rack

press-cake

or

the

is ad-

The

pressure.

juice flows

the

are

communicates

bag

the

and

be

placed

are

juice (cachaza)

for the removal

The

to

type

pipe-rack

eonaiderable

content

sucrose

require changing

Each

Muddy

cloths

time

mud.

"

of

type

filtration is from

Filter-bags

cylinder.

the

is opened

cylindrical body

mechanical

first filter of this

pipes leading

from

stopped

the

hs

suitable

upon

cylinder under itself to

of

far

the

manufacture.

filtered juice-canal.

attaches

washed

so

the

was

inclined

an

of

FUter.

bag.

a

suspended

in

to

is

in

of

cane-sugar

enclosed

Sdf-dvmping

development

a

are

SweetUmd

"

press.

The

through tion opera-

of and

the the be

may

cloths

infrequent intervals. Fig. 16, its two

or

"clam-shell"

parts

opening

type and

of

closiiig

69

FILTER-PBBS8ES.

the

after The

of

manner

with

hinged together,

cybnder

when

crimped-wire the

and

these

place in the filter body

connection

with

Variable

the

epacii^

is

for

provided

conditions.

filtration

closing of the

lai^e ^le be

may

The and

This

press

of presses

operated

at

and

the

the

wash-water

juice

in the

has

The

and

suit different

to

them

the

valve.

displaces the air

to

is then water

the

upon

the

filter-cakes

The

and

presses

hydraulic collects

adjacent

a

opening Several

It

mud

opened.

delivery,

accomplished,

one

filter.

cachaza-valve

removes

The

power.

through

until

is

in

filter.

the

separate

etc.

from

The

passes

valve cake

the

leaves.

continues

alightly separated. the

into

outlet-nipplea

the

quickly

time

same

clamped

be

may

leaves

using hydraulic

hiiuid

the

process

leaf

is easily and

the

screens

IQ.

Each

Uquid is forced submerges

cloths

the

nipple

these

over

with

glass delivery-tube,

cock,

outlet

an

they

of

composed

fittings outside

delivery

Fia.

ahut-off

that

water-tight

a

are

is fastened

arranged

so

form

to

with

provided

Filter-cloth

bucket.

Bemi-cyUndricsil membera

2

filter leaves

each

are.

Bteam-ehovel

gasketa,

The

screens,

latter

in

euitable

closed.

filtrate.

tightly

clam-shetl

of the filter compriaes

body

for

the

outlets. but

are

closed

and

displaces

large part of the

sugar.

^ 70

FILTRATION

PROCESSES

AND

MACHINERY.

washing, Uie cakes are partiallydried by compressed air,if so desired,and the lower half of the body is swung open and they are discharged. Steam or compressed air may be After

used inside the leaves to loosen the cakes from

coating of of the

cakes.

is

A

the cloths facilitates the

kieselguhron This

the cloths.

applied

discharge suspension before

in water

filtration begins. in Dlffnsion-worb:. Disposal of the Skimmings ^The skimmings from di"Fusion*juices sometimes cult diffiare to filter-press. A simple meth6d of their disposalconsists in returningthem to the diffusion-battery. A measured volume, approximately 10 gallons of skinunings per ton of cane, should be added to each cellof cane-chips.In drawing the juice from cells containingskimmings, allowance must be If their volume. the not made for skimmings are ton must 10 gallons per than settled,considerably more is practised be added to each cell of chips. If this method in diffusion-work. be dispensed with settling-tanksmay The The sooner the skinunings are disposed of the better. if rendered slightly skinmiingscan easily be filter-pressed alkaline and heated to the boiling-point. Many chemists and sugar-makers question the advisability The of returning the skimmings to the diffusion-battery. objection urged is that under the influence of the longof the impurities may continued some high temperature in the defecation. be redissolved and may be reprecipitated not culty with cane, diffiIn the early days of diffusion-work the sometimes was experienced in filter-pressing houses of the skimmings; this led to the adoption in some is a plan of returning them to the battery. This method with the costly filtervery attractive one, as it does away and a heavy expense-item for cloths and labor. presses Moreover, the loss of li to 2 lbs. of sugar per ton of cane avoided. contained in the press-cakemay be almost entirely To what extent the advantages of this process are offset by 28.

"

the

possibleand

juicehas 29.

not

been

probable return

even

of

impuritiesto

the

estimated.

Reclarification the

of

Filter-press Juice.

filtrate from

sugar-makers return and defecators;others clarify

the

presses

"

Many to

the

resettle this filtrate separately

RECLARIFICATION

mix

then

and the

filtrate

This

last

the to

juice the

greatly

it

with

directly is

an

may

mud increase

FILTER-PRESS

OF

the the

to

clarified

appear

(cachaza) the

to

be,

scaling

of

practice, if to

of

the

the

lime

has

filtering.

tubes

others

of

the

pump

evaporators how

matter

no

especially

preparatory

still

juice;

charge-tanks

objectionable

71

JUICE.

clean

been Such

added filtrates

evaporator.

REAGENTS

CHEMICAL

JUICE.

Lime.

30.

There in

use

several

are

with

ground

water

to

liming

(2) Dry

slaked

juice preparatory is

to

from

prepared

circulating. This the

both slaked

in

heavy

paste.

The

preparation

The

in the

the

reducing large

so

lime

retain

15"

Baum6

the

to

of

tors defeca-

kept

constantly generally throughout (4) The settle

to

linae

and

is drawn

water

is of great

is

form

off.

a

The

too

are

much

the

full time be

water

conditions

be not

allowed

added,

slaking-tanks

The heat

importance, especially Essential

sugar.

that

temperature.

to

as

the

When

season.

density

A

factories slake

to

custom

the

been

the

lime

that

form

of the

reaction

for thus

should

and

be

promote

slaking.

the

1

and

allowed

of white

manufacture

reaction

is

TvitK

in the defecators.

use

of the

properly slaking

in

very

supernatant

paste is weighed for

it

of

lime

industries.

then

and

This

pumped

which

beet-sugar

large tanks

is

is used

method

and

cane

in

is mixed

powder

of

is_used sprinkling

by

defecation.

the

and

quicklime

pipe-lines,

through

sifted

slaked

be

method

prepared

(3) A milk

in Cuba.

is also used

is

for

lime (1) Quick-

must

juice. This

The in

juice

follows:

as

which

powder lime

use

cost

is lime.

preparing this substance

the

heaps of lime.

on

lime

fine

a

moderate

of the

cane-juice

before

water

Cuba.

in

of

of

agent

treatment

of

methods

defecation

the

is

for the

i

1

effective

most

found

been

has

that

^The

"

THE

PURIFYING

IN

USED

The

milk

with

water

list of

proposed

several for

use

of Louisiana the

was

and

hundred in sugar

lime

in

were

advance

reduced, then

very

after

passed

substances

manufacture,

and

of

small the

slaking, through

on

page

was

grinding to

fine

combinations

is given

it

a

low

screens

that 532

72

h

73

LIME.

into

second

a

filled.

and

tank

so

allowing

After

few

a

settle out, the supernatant

to

portions of the strained milk The

tank.

the

in

repeated until further

slaking even

filled.

been

alternate

two

added

to

filled with

three weeks

or

were

already

settling were the heavy lime-

frequently noted

indications

after the tanks

description is given

This

the paste

drainage and

were

has

author

The

containers

days for the hydrated lime drawn off and fresh liquidwas

were

all the tanks

paste.

until all the

on

to

of

had

emphasize

the

importance of the time element. The lime used in t^Jie purificationof the juice should be The magnesia and soluble silicates of the lime pure. very in the defecation

used

is made

mention

However,

form

processes

farther

on

scale in the evaj- orators. of the satisfactory use

containinglargequantitiesof magnesia.

of lime

quality of the lime-stone used in the carbonation process rich in silica tend is of great importance. Certain stones others have "scaffold" in the kiln,and hydraulic properties,

The

to

resulting in

an

almost and

of lime-stones

comments

factories.

Hawaiian this

coral beach-sand

from

shows

source

cent;

lime 91.7

made

for the

these

92.5 and

The

Cuban

of two

of

content

sands

calcium

burned

in

coral sands

6.6

would

oxide, 6.0

and

4.5

(dry) gave The

cent.

per

a

produce lime

containing per-cent magnesium oxide

cent

factory, Island

Paia

the

in the

extent

some ^

etc. silica, following information

1.6 per

of Beet-

following analysis of lime from Silica 0.18 per high magnesia content: cent; magnesia 4.15 per cent. Analyses

Cuban

cent

per

to

The

author

carbonate

magnesia first of

per

for Chemists

is used

amples Ex-

their characteristics

on

"Handbook

given in the author's Houses," p. 211. sugar are

Lime

impervious filter-cake.

rotary kilns

relative

of

Maui, H.

with

coral

to

T. *:

temperature

sand

is from

"Coral

sand

control.

is

Danp

preferred,since the temperature at which dissociation dioxide takes place is slightlylessened in the presof carbon ence of steam generated from the moisture." sand

is

"Coral "

Spec. Report,

"Planters'

contains

sand

considerable

July, 1913, Expt.

Monthly

(Hawaiian),

Sta.

Haw.

magnesia Sugar

Nov., 1909, 444.

Planters*

which Ass'n.

is

74

objectionablein the defecation owing the heating-surfaces. Further, a

to be

usually presumed its

depositing,upon portion of the magnesia to

increase

The

large elimination defecation was good, the yield of

the

output

5.45

per

and

saw

showed

a

molasses

of of

cent

in

in the double

magnesia Sulphurous

30a.

the

from

the

inates

use

Acid.

white-sugar chapter,

the used

in

raw

Aside

carbonation

process.

The

process

elim-

"

This

58.

page

except in Louisiana.

heavy

clarification.

the lime salts and

thus

It also the

reduces

"

freely in the

massecuites

than

vacuum-pan

up

duces prochanically me-

of

some

viscosityof the sirup and

Sulphured sirups and

massecuites.

breaks

in

is little

reagent

bleaching effects the sulphurous acid precipitatewith the lime which assists

in the

more

defecation

in 1913

its

from

a

contained

lime

juice. ^The production is described

manufacture

sugar

The

writer visited Paia

The

filtration in the

sucrose.

satisfactoryand

sugar

small.

was

magnesia." lime

coral

alkaline "

consequent loss of

Agricultural Co., Paia factory, of the magnesia in the press-cake.

Maui

of the

would

remaining in the molasses

output with

the molasses

experience

The

USED.

REAGENTS

CHEMICAL

those

boil

made

much

without

this reagent. Carbonate

31.

begun

have

rather that

Caustic better

are

with

the

lime, objectionable. The

very

as

neutralizing molasses.

in a

ferment

to

than are

of Soda,

beneficial effect when

Soda.

neutralized

latter

The

with

soda,

produces soluble

soda

salts

carbonate

are

salts

also

useful

apparently

into the pan

taken

^Juices which

"

in

has

boiling string-

sugars.

Carbonate

of soda

its salts in sugar

from

de

Grobert

to

a

^

found

52

equivalentsmore part

wa,s

states

incomplete precipitant of

an

solutions.

that

the

of soda

of the soda

neutralized that

per

cent

In

a

addition

sirup in the proportion about

A

is

of

precipitated81

remained

in

a

series of experiments of

carbonate

its equivalent

of the lime.

The per

free state

"

Eighth

of soda

Cong.

App.

is used

in

Chem., 8,

of

of

lime

addition cent

and

by the organic non-sugar.

if carbonate

lime

of

cipitated pre-

of two

the lune.

the remainder M. de Grobert

juices,sirups 21.

soda

etc.

76

REAGENTS

CHEMICAL

acid

phurous zinc

with'

these

Among

facture.

calcium,

(made tin

or

clay,

tin

salt,

or

alumina,

muriate

of

this

material

is

hydrosulphites

is tin.

of for used to

of of

hyposulacid

sulphurous sodium

and

of

etc.

acid

Kieselguhr

barytes,

are

reduction

the

dust),

washes

centrifugal

substances

by

Hyposulphurous

USED.

yellow as

juice

a

or

used

in

The

bleaching

last

named

molasses, is

also

also used

sugars.

filtering sirup

medium.

greatly

The

facilitates

addition filtration.

in

EVAPORATION

OF

Multiple-effect

34.

sirup and kettles

the

over

sirup fire

a

in

or

these

high,

or

the

steam

to

the

being

in so-called

from

of

form

the

according

the

to

standard

of

fitted

calandria the

tubes. The

This

large

tube

second

is

pan

H.

pan,

calandria

the

^

of

means

See P.

of

pp.

350

a

and

381,

"

film

but

to

in

film,

thin

a

which

pans

by

it boils

the

calandria,

vapor-space

The

and

The

the up

of

center

juice back the

through

"down-take."

the

is

vapor-space,

with of the

the

Juice

the

nected con-

steam-space

second of

vapor-space

large pipe with

Evaporatin*?

the

steam.

the

or

steam-

a

which

through

carries

as

'*pans" with

In

large vapor-pipe

a

tors evapora-

consists triple-effect,

provided

tubes,

is called

the

answer

deep layer,

a

and

"calandria."

third.

the

by

connected

the

the

above

in

surrounded

are

large tube of

is

each brass

the

part

by of the

which

a

inches

evaporator,

or

termed is

will

evaporator.

of

part

lower

space

in shallow

the

generally used.

most

cylindrical vessels, termed

and

is

steam-drum

a

of the

copper

juice circulates

the

ducted con-

which

of

apparatus,

few

is

evaporation

liquor is boiled

of the

lower

with

factory,

description of which

the

from

more

or

The

depth, whereas

vertical

three

pennit.

two

vacuum

a

book,

type

''effects"; the drum

of

type

molasses

or

sugar

of

few

times, according

duty

triple-effectis

varies

was

by but

and

price of

conditions

open

boiled

nearly disappeared

factories

the

liquor

a

do

forms

in

depth

have

evaporator.

of this

to

modem

to

the

esses proc-

multiple effect in the

evaporator,

4 feet

3 to

The

made

various

purposes

to

local

"standard''

this

the

where

of

type

small

where

is in

the

processes

very

old

evaporated

was

in which

pans

places

evaporation

The

the

in

except

is very

In

in

juice

the

In

"

point of crystallization, in

These

only used

are

the

the

to

by live steam-coils. and

Evaporation.

sugar-manufacture,

of

JUICE.*

THE

with

pan

the

third

condenser

Heating,"

and Prof.

by

Creighton.

77

W.

78

EVAPORATION

The

vacuum-pump. exhaust steam

juicein

from

the

of condensation

water

OF

JUICE.

is boiled

first pan

the

various

flows

THE

and

pumps

through

a

trap

by

the its

engines and

to the boiler-feed

water-tank. The

generatedin

vapor

in the second, and

sirup in the third circulates

that

the first pan is used to boil the juice generated in the second to boil the

juiceis fed into the firstpan and reaches the third,the and finally, fast as the' evaporation of the as

The

pan.

from

pan to pan juice being admitted

thin

the removal

and

water

of finished

sirup permits. A

vacuum

is*producedin in the

the third pan by the pump and condenser and first and second of the by the condensation pans

vapors

in the calandrias in each

of the

second

third pans.

and

The

the working upon of mercury 5 to 7 inches conditions, but is usually about in the first,14 to 17 in the second, and 26 to 28 in the third vacuum

pan. travels

By

reason

from

depends somewhat

pan

differences in the

of the to

pan

and

pan

evaporation in the first pan in the the

second, and

third

is either

pan.

drawn

directly pumped

produced

hot

enough

to

second

the the

to

of the

water

calandria

of the

boiler-feed

in

boil the

boil the

third

tanks, and

juice the

liquor

sirup in

second pan,

that

pan or

of

is

the

is also removed

third pan These

vapors

condensation

into to

the

in the

those

The

are

the

vacuum,

by a pump. usually termed

*'

pumps.*' sirup continuously by pan of a pump, the workman regulating its density by means the steam-pressure and the quantity of juice in the first pan, the liquor from the third pan. the rate of pumping and Valves are provided on the pipes connecting the pans to pumps

are

is removed

The

from

the

sweet-water

third

regulate the flow of the liquor. is sometimes The somewhat fied modiprocedure described These pipes by the use of Chapman's circulating-pipes. are

like inverted

are

of such

cient

to

syphons connecting the liquor-spacesand

length that the

empty

them.

vacuum

They

are

in the pans

arranged

to

is not

sufl[i-

maintain

a

constant liquor in the pans without the use of other than those for the juice and steam in the regulating-valves

level of

first pan.

These

pipes

rapidlythrough the tubes

cause

the

liquor

of the calandria.

to

In

circulate

very

operatingthe

MULTIPLE-EFFECT

the workman

apparatus

that

state

uniform

requisiteto satisfactorywork

of

in the third pan

vacuum

with

inflow

less It is perhaps need-

the first pan.

on

very

a

only to regulatethe

needs

juice and steam-pressure to

79

EVAPORATION.

is

circulators.

these

rapidityof the evaporationin multiple-effects of juice with the vapors. less entrainment there is more or This juice is recovered by leadingthe vapors against baffleplates,usuallyin a greatlyenlarged section of the vapor-pipe. The enlargement of the pipe reduces the rate of the travel and of the vapors permits the deposition of the entrained to the

Owing

juice. This device is called a "save-all." of two Multiple-effectevaporators are constructed four three pans called a double-effect, a triple-effect, a

The

etc. quadruple-effect,

this

apparatus in

outlined

of descriprtion

the

higher combinations

With

is worked and

is the

based

are

under

of

the

triple-effect. the first pan triple-effect,

the

the

within

is that

standard

it,instead

of

a

vacuum,

"pressure-pan."

calandrias

for the removal

pressure

a

is called the

The

than

for all and

same

pans

all types of

which

principle upon

pans

of

multiple effects

of the

incondensible

removal

of these

provided with pipes

are

A

gases.

gases

because

careful supervision

only the heating-surfaces,

is necessary,

not

they reduce the efficiencyof The gases contain but, further,they frequentlydestroythem derived largely from the decomposition of the amida ammonia .

juice,and partlyfrom

of the The

should

anunonia

ends of the copper It

vapor

tubes

practice in

is the

largelyin

be

the

other

nitrogenous constituents.

removed, since- it attacks in the steam-space

the upper and ruins them.

beetnsugar industry and

the

cane-factories of Java

to

utilize

a

very

part of the

generated in the firstvessel of the multiple-effect and,

also a part of that from the second quadruple-effects, vessel in juice-heating.Vapor is also sometimes supplied in and in convertinga tripleboilinga calandria vacuum-pan with

effect

into

"robbed,"

a or

quadruple effect. "extra

steam"

When

is taken

the from

first vessel

is

it,largerheating

provided in its calandria than in those of the vessels. other Frequently a pre-evaporator, to increase for juice heating, evaporative capacity and supply vapor

surface

is

etc.,is used in connection

with

the

multiple-effect.

80

EVAPORATION

OP

JUICE.

THE

of the first effect heating-surface

The

is sometimes

double

the

requirements of the evaporator so as to supply the extra The of heating are juice heaters in this method vapor. usually of the closed return-tube type. This use of the vapors extends double^ffect heating to the juices and, in some instances,even

to

Preheaters

part of the massecuites.

a

(Pauly-Greiner) their

cane-industry, though extensive.

This

in

to the

made

^

Deerr

the

at

sugar

a

and

complex

very

of salts of both

amounts

alkali. may

a

Hence

a

juicesshould with

suffer

detectable

no

ing destroy-

with

factories

half hour's

a

be safe with

another.

one

at

120"

It would

be

cane-

of free

juice

conditions

(Hawaiian

heating

loss of sugar.

With

he

variable

very

acids,and

weak

that may

local

conclusions

obtaining in

system

strong and

inversion

usually prevailing in

other

consisting of

one,

temperature

serious

cause

to fear of

or

is

of exhaust-

large amount

among

arrived at the following: (1) "The

juices is

the

that is necessary. Noel high temperature study of the effect of high temperatures in solution

cane-sugar

upon

in

beet-sugar factories

usually available in cane-factories

steam

little used

VCTy

use

be due

may

are

Islands),

C. (248" F.) conservative

adopt this temperature as the highest to which cane-juice should be subjected during evaporation, though under a to

careful 125"

of control

system

C.

(257" F.),

or

and

even

observation C.

130"

a

temperature

(266" F.) for shorter

permissible." (2) "The products is possiblesince it occurs be

periods, might cane-sugar

at

evaporation and

C." the

(3) "The

use

preheater system

After

a

rational

the

taneously instan-

high-temperature

of

evaporation and products is possible

control."

concentration

of the

multiple-effectevaporators, settling- and

almost

of

of

house

also the sterilization of all cane-sugar under

sterilization

"

125"

of

it

storage-tanks. A

juice

is

to

a

pumped

considerable

sirup in the to combined

quantity

of'

soluble in the thin juice are insoluble in plentiesthat were the sirup. A part of these impurities deposit th^nselves the heating-surfacesof the evaporator, forming a hard upon scale. Those which renaain in suspension are removed by im

*

Bui.

36, Expt.

Sta.

Hawaiian

Sugar

Planters'

Ass'n.

MXTLTIPLE-EFFBCT

the

This material

be

cannot

usually pumped

is very

above.

rich in sugar. it is

therefore readily filter-pressed,

the defecators

to

mentioned

tanks

that collects in these tanks

sediment

The

in

decantation

settling and

81

EVAPORATION.

to be diluted clarifiers,

or

by decaatation. precipitateremoved of pumping the sirup directlyto the settlings Instead tanks, it is often first boiled and skimmed, i.e.,clarified. juice and

with

the

of white sugar, probably beneficial in the manufacture of sucrose, but at the expense through inversion. The glucoseratio of the sirup rapidly increases during the clarification, is

This

and

the

and

scum

the

the

sirup to its be

must

removed

would

of the

that

faster than contains other

cane

The in

Its

composition

in

and

The

third

The

and

most

tubes

pan

a

very

poor

somewhat

with much

very

always

which

with

those

of the

contains triple-effect

of lime

2d Pan, Per Cent.

3d

Pan,

Per

Cent.

56.98

2.02 3.25

Silicate of lime

7.86

the

oxide

Combustible

matter

tubes and

may

be

scraping

tedious

method,

15.02

7.49

0.54

1.65

4.68

19.55

9.93

0.71

7.02

11.32

11.27

13.31

1.53

2.31

2.58

7.79

7.43

39.26

54.34

20.37

13.41

11.04

5.08

by moistening the scale with This

surfaces.

therefore

the

is

a

Prinsen-Geerligs, Kobua

very

laborious

followingis usually used,

applies also in cleaning the coils of the "

Cent.

2.03

cleaned

the

4thPan, Per

1.92

of lime

Silica

and

a

scale.

57.85

of lime

Carbonate

and

varies

of the first pan,

of

obstinate

of lime

Phoflphate

water

evaporators

it is

as

following analyses of the scales indicate their tion composithe different pans of a quadruple effect: ^

Sulphate

The

of the

localities forms

some

IstPan, Cent.

Iron

3rieldof

the

as

by rapidly heating

tubes

Per

Oxalate

far

juice, scale little compared

pans.

thickest

the

on

frequent intervals

at

in others.

thin

the

as

realized

be

forms

of heat.

conductor

approximately sirup from

boiling-point.

which

scale

purity

results, so

better

that

is concerned,

The

of

have

derived.

are

It is probable sugar

rise to the surface

that

coefficient

same

they

which

foam

vacuum-pans.

Ar chief, 1900, 694.

*

r 82

EVAPORATION

The caustic of

into with is

soda

boiled

per

iron

and

water

afterwards

enough

be

The

soda

alkali from

solution

cleaning

is

to

always

evaporators

then

about

a

week

it

acid

is

usually

be

used

the

will

be

necessary

strong if

treatment

usually the

which

acid,

should

This

pans

washed

are

pans

At

condition.

solution

from

muriatic

a

pounds

soda

run

taste.

with

two

to

This

The the

tubes

keep

the

of

the

give

the

end to

scraping.

solution time

one

dilute

with

to

good

Reason

thorough

from

the

The

sewer.

of

in

manufacturing a

the

intervals

at

of

is

and

boiled

acid

very

level

store-tank.

into

heating-surfaces

tubes

hours

JUICE.

solution.

of

foot

then

run

to

repeated

cubic

lead-lined

or

the

containing

several

during

an

above

to

solution

soda

the

is

filled

are

pans

THE

OF

may

time

as

it

boiled and

becomes

under

pans.

repeatedly, weakened.

atmospheric

caustic

adding The pressure

soda in

84

The

formaldehyde. should the

fill

mixed

be

ing's

closed

juice

always

tends

added

through

the

in

the

to

the

of

be

also

and

tank

are

the

to to

organisms

not

killed

due

The tinae.

short

a

which

from

eliminator

Dem-

mixing is

formaldehyde

The

juice!

in

thoroughly

in

difficulty

the

and

standing

after

to

held

satisfactory.

entirely

not

pump-tank,

heaters

may

walls

due

with

decomposition

it

pumped

is

The

separators.

lodge

that

by

upon

heat.

the

{See

11.) The

writer's

juice,

the

of

saving breakage juice,

due

labor

with

would

usually is

juice

indicated in

the

In and

the

in

above.

evaporation.

to

It

This

the

were

large of

event

of

the

insignificant.

barrels

practically

the

deterioration

is

employ

there

very

in

sugar

of

tion deteriora-

as

of

view

slight

formaldehyde,

advisable

deterioration

slight

sucrose,

of

often

formaldehyde be

of

inversion

machinery,

the

of

cost

fuel,

and

preserved

The

to

a

formaldehyde.

fermentation.

of

of

of

presence

probably

indications

no

indicated

experiments in

even

was

the

starting

on

juices

preserving

decompose

be

possibly

usually

than

is

to

formaldehyde

also

immediately

juice

in

separators

may

the

the

formaldehyde

of

use

the

with

preservative

the

of

quantity

defecator.

The

This

measured

SIRUP.

AND

JUICE

OF

PRESERVATION

is

it

in

all

so

small

larger

that

it

quantities

disappears

from

CRYSTALLIZATION

The

36.

Vacuum-pan. of

concentration of

more

This

largely reduced of

a

vacuum-pan

strike-valve The

roof

and

condenser

the

to

of the

by

of

type

or

been

have

facilitate the

to

in

bottom and

The

pump.

velocityof

large, that

the

slow, thus

reducing the

is fitted with

and

has

large door or discharge of the sugar.

for the

a

is connected

pan

cylindrical

vertical

a

large vapOT-pipe vapor-pipe or by a

a

directlyby the

pump

conical

a

bottom,

the

dome

or

usually

steam-coils

copper

at

cent

per

could

water

the

evaporation is conducted

is

iron^,with

of

number

a

45

in

single-effect.

The

cast

eirup obtained

of

further

sugar

in

vessel, of

SUGAR.

but multiple-effect,

vacuum-pan,

modem

The

"

content

in the

the

THE

juice still contains

the

water.

graining

OF

with with

and

small

save-all

a

vacuiun-

a

pipe,according

vapor-pipe is usually made the

be

may

vapors

entrainment

of

very

comparatively

sirup. Hhe

is

pan

to provided vsrith eye-glasses or lunettes through which of the boiling liquor, and a proof-stick observe the progress

also

removal

the

for

the

that

arranged

of

is

which

produced by the

is said to be of the ''wet and

water

condensed

of the

pump

and

separate The

pan

thence

pipe as

vacuum-pans

in

a

a

from

and

torricilian the

removed

described are

are

and

flow

tube

by the

condensing-

with

when the

air is led

using

condens-

"leg-pipe"

or

to

a

hot

off in

as

pump..

usual

These

pump

passed through it. The

factory. The

is of the

used.

all of the

special condenser,

''dry system,"

ing-water through well

vapors

of

vacuum

The

condenser.

when

so

temperature

decreasing the

and "

is

apparatus

the

vary

pump

system

ctmdensed

the

are

vapors

of

can

panman

boiling liquor by increasing or

the

a

The

samples.

test

form.

vary

Various

in the

extent

85

types and

,

86

CRYSTALLIZATION

of

arrangement

of the pan,

Sugar

Grain.

to

of

absence

or

use

boilingmass.

of the order

In

"

of the

relation

the

in the

and

the circulation

to promote

Boiling

37.

SUGAR.

heating Hurfaces,in

the

height to the diameter

specialdevices

THE

OF

facilitate

to

and to familiarize the chemist descriptionof pan-boiling, with factory terms, a few expressions used by sugar-boilers the

will be

first

the cane, those

in expressionsdiffer somewhat refiningbranches of the industry. Only These

given.

beet, and

will be

in cane-work

given: The concentrated juice is called "sMp'* or "meladura," is used the latter word is Spanish and by foreigners in The and other Cuba trated concenparts of Spanish-America. form of crystalsand molasses the ''massecuite," mass when boiled partly with sirup and partly with molasses, or customary

"mixed

massecuite," and

When

portion of

a

remainder

from

"strike."

a

the pan

and

the

footing or nucleus upon which to boil another There "cut." a strike,the portion so left is termed is some confusion of the word in regard to the use "cut," as this Word for the massecuite removed use sugar-^boilers many from

the

Where

is left

strike is removed

a

called

boilingis

each

two

suitable

more

or

with

These

another

one

called

are

modem

the

a

stage, diluted molasses it is said to

side

by side they by large pipes, with from

massecuite

to

one

"cut-over

practice, when

sirup and

"cutting."

worked

are

pans

valves, for drawing

certain of

pirocess is termed

connected

another. In

The

pan.

often

are

a

as

pipes." grained strike

is drawn

be

into the

"boiled

in,"

reaches

instead

pan

"boiled

or

a

in

on

grain-sugar." When

the

liquor in the certain density and is more to haVe

fs said or "weak"

reached

is still further

connection

with

the

closed, shows

valve td

cover

a

the

concentrated

less saturated The

modified,

with

proof may or

less

will

as

be

is started, and

pump

and

coils.

to

it

sugar, ' '

"

strong

density.

be

a

This

explained

in

of

of 15 to

is opened

been

boiling molasses-sugars. boiling sugar is as follows: The

vacuum

vacuum

has

of greater

the of

process

"

proof.

expression The

or

liquid is

the

as

"

pan

20

inches

sufficient Steam

of

when

mercury,

sirup is drawn

is turned

into the

the tlie

is

pan

gauge

charge-

into the coils ahd

pan

tlie

SUGAR

BOILING

proof. The quantityof sinip the boiler wishes "to grain" high whether In making fine-grained sugar he will grain

sirup is rapidlyconcentrated used

depends

or

upon

in the pan.

low

needs

he

high,

as

room

for their

crystals and

many

At

are

this

The

stage there

concentration

sample into

with

is

condenser

procedure:

(1)

ciently liquor is suffi-

the

is indicated

as

sugar,

increased

now

coils reduced, thus

the

until

is continued

by the proof-stick. The

drawn

the

of

methods

two

are

supersaturated

on

comparatively little

and more successivelyclosed, anii as it becomes concentrated, the portions projected against the eyeglasses flow more and more and increases the slowly panman of decreases the quantity water denser injected into the conuntil the liquor boils at the desired teftiperature.

coils

or

to

grained growth; on the contrary, in making coarsehe will grain low, and form few crystals. sugar of the upper the liquor boils down, the steam-valves

As

more

87

GRAIN.

TO

and

of

watet

the

by a injection

steam-pressure

coolingth^

boilingmass, increasing degree of saturation,and forcing minute crystalsof These to form. ing accordmanipulations vary somewhat

the sugar

the

to

but

in

of

sugar

itself and

vacuum-pan

quality of

the

(2) The

described.

the

sirup,

method general are as of graining is that usually employed in the United States. of the liquor is continued The concentration until crystals

there the a

separate, sufficient

are

of

sugar

crystalsrequired are

the

After

the

formed

to

time

at

the

of

produces since

all ol

once.

formed, sirup is drawn as

that

temperature

sirup. The first method grain than the second,

crystals are

time

from

pan

consider^

panman raises the

crystalshe

uniform

more

the

when

injectsmore

and

pan

and

second

water

into

evaporates.

the. This

to charging of the pan with sirup, and Judging just when skill and charge, requires much practice on the part of the

boiler

in

order

to

the sirup when surrounding the will

be

termed

formed -'false

mass

secure

the

is too

must

grain," and

results.

If

concentrated, with

crystals too and

best

be

rich

in

sugar,

remelted.

where

formed

injects the liquor

fresh

crystals crystals are

Th^se at

he

a

late

stage

through carelessness of the sugar-boilerand are not removed, they impede or even prevent the curing of the sugar in

r 88

the the

OF

CRYSTALLIZATION

THE

SUGAR.

False grain may be formed by charging centrifugals. massecuite with the too or sirup, by cooling freely pan

sirupsurrounding the crystalsis rich in sugar and of such densitythat it is supersaturatedat a lower temperature. of have been not if sufficient number crystals Also, a formed when grainingthe strike,there is great risk of the formation of false grain, after the crystals to have grown largesize. If the false grain is formed and not removed at this stage of the boiling, the sugar be purged of cannot False grain is gotten rid of by raisingthe temmolasses. perature of the pan and drawing in additional sirup to melt the fme crystals. is evaporated, sirup is As already stated, as the water while the

drawn

into

the

The

pan

time

from

time until the

strike is

kept very free,t.e., of c""nparativelylow density,until the crystalsare large or the pan is about two-thirds filled. At this stage it is gradually boiled the end of the operation,thus dryer ioid dryer until near impoverishing the molasses surrounding the crystals,and finallythe massecuite is evaporated to an apparent degree Brix of about 93, and is then discharged from the pan. should be as cold as possibleat this stage. The massecuite of estimatingthe proper moment There are various methods the massecuite, i.e., for striking dischargingit from the pan. This is usually determined by withdrawing a sample with the and forming it into a conical heap upon the proof-stick with the finger. The consistencyof this massecuite, thumb rate of flattening, etc. are noted as shown by its appearance, in this way and a practiced man can by the sugar-boiler, limits when to drop the strike. judge within narrow must be observed after each During the boiling,care the mass to force sufficiently charge of sirup to concentrate the crystalsalready present the sugar to deposititself upon finished.

massecuite

to

is

,

and causes

not a

to

form

new

of time

waste

concentration Unnecessfiry

ones,

and

with

sirup,employed with but not applicablewith all,is by means vacuum-pans, many After the formation of the grainthe charge* of a "set feed." valve is opened and so adjusted that the flow of sirup into the pan justcompensates for the evaporation. The opening A

method

of

charging a

steam. pan

BOILING

of the

valve

is

adjusted

varies, with

density of the a

the

minute

many

has

been

from

the massecuite. massecuite

boiling a

from

sugar

should be formed

so

of very

charging, with uniform quality

low

a

yield of

obtain

to

An

false

crystals,from

as

tration concen-

massecuite.

the

it, the full number

the

grain sugar

maximum

of

crystalsrequired the crystalsshould be of

graining,and

at

the

as

steam-pres""ure, the

method

melted, results in

that

yield of

in

This

time

graining,produce a good yield from very

irregulargrain, with

In

to

of

and

not

time

variations

sirup, etc.

the first method of sugar,

from

89

GRAIN.

TO

SUGAR

false grain at regular size. Of course, The formation be avoided. stage of the operation must any of too few crystalsresults in rich molasses, since there is not moderate

and

sufficient

crystal-surfaceto take

increases

the

very

risk of the

boiling a strike a

on

a

the

up

formation small

very

of

nucleus

cut, there is also risk of false

small

exhausted The

false

soft,white

or

grain or in

maintained

be

to

of

noted

will be

are

sugars

with

or

on

partially

a

the

of

in the boiled

in the

customary

chapter

whether,

sugar,

practice also differs to

respect

temperatures.

on

sugar-refining, 119, page refineries,

F. in the American

at 180"

Similar

inversion.

no

in

Java

massecuite

superintendentprefersrelativelylow temperatures.

Java

hard

American

raw.

or

that

from

somewhat

As

grain. When

of massecuite

during boilingvaries with the desired grade of

The

besides

molasses.

temperature

hard

and

sugar,

but

lower

white-sugar factories

temperatures

are

of Louisiana.

stated,are boiled at high temperatures, but also be produced at moderate they may temperatures from should be sirups of low densities. High-test raw sugars Hard

as

sugars,

grained

at

temperatures

approximating

should be continued high temperature well developed. The temperature may latter part of the

strike to promote

160"

until

F., and

grain is

the

lowered

be

reduction

the

of the

in the

purity

that surrounding the crystals. Massecuites be further crystallizedeither in motion (crystallizer

of the molasses to

are

in tanks

massecuite)

or

at

temperature

as

possible.

In

making

a

rest

very

soft sugar,

should

after

be

boiled

at

as

low

the temperagraining,

90

CRYSTALLIZATION

OP

THE

SUGAR.

low boilingmassecuite should be maintained as possible. Low-pressure pans, having large as i.e., pans of below 10 lbs. pressure, steam heating-surfaceand utilizing usually preferredfor soft-sugars. are of Sugar-boiling. Methods Pan-room 38. tions. Definiof the

ture

"

Raw

"

designate their

and by the letters "A," "B" "C," number them, to distinguishthe grade

vacuum-pans or

and

often

manufacturers

sugar

not

themselves.

the pans

employed in boiling the of fts proximity account

grade

same

to

is

pan

a

in

a

of

fineries, re-

cuite masse-

usuallyalways

in

of sugar

certain mixer

usuallytrue

but this is not

A

in

as

and

refinery on

a

set of centrifugals,

factory.

into pan complications introduced practice by boiling-inmolasses, it is simpler to designate massecuites With

by

the

rather

n"Un"3

boiled' with

was

and

molasses all the

pahs

thfere is

the may

"third."

and

pure

third

confusion

some

massecuites

are

boiled

strikes

The

with

first strike of

second in

the

in

with

first

present

molasses, hence

nomenclature. of

cuite masse-

with

At

molasses.

part with

return

only

numbered

were

cane-sirup,the second

boiled

be

when

Formerly

boiled, the

"straight-sugars"were "first,""second"

numbers.

than

When

three

molasses, the writer

prefers the following designation for each: containing only sirup or sirup and massecuite

(1) First a

very

cuite, masse-

little first

high coefficient of purity. (2) Mixed massecuite, containing a footing of and a large proportion of first massecuite from first pan a This is of medium molasses. purity, approximately 75** to massecuites will produce the same 80**. The first and mixed (3) Second or crystallizer massecuite. grade of raw sugar. is of low purity,usually of 60" and upward. This massecuite This

molasses.

factories but

In many case

is therefore

that

of

The

the

two

second

a

massecuites

of

are

boiling is termed

first massecuite

boiled,in "mixed"

in this method

or

which

ond." ''sec-

is reduced

to

purity with first molasses. of pan-boiling Utilizingthese definitions,the methods applicablewith rich tropicalcane in raw-sugar worl^ will be methods described. These are rapidly extending in Cuba about

75"

and possibly elsewhere. The

boiling-backof

molasses

"has been

practiced ih Louisi*

92

CRYSTALLIZATION

OF

SUGAR.

THE

diately after leavingthe vaeuum-pan^ the

grade of

same

and

and

should

produce

widely different is purged crystallizermassecuite

sugar

molasses

of

purities. The second or after remaining three or four days in the crystallizers.This massecuite be sold as seconds, or yields a sugar that may be converted grain" sugar it may preferably,since it is a into sugar equal to the firsts by double purging. noted that in boihng-in molasses this should It should.be be accomplidied after no more sirup is required by the strike. be free of sugar-crystalsand should be The molasses must '*

than

warmer

to

a

the massecuite

density of about Boiled

MassecuUes

largelyin the upon

a

54"

sirup. Grain

which

In

"

and

formed

of

method

a

practiced

the strike is started

Java

string-sugarmingled with

build

to

be reduced

It should

temperature.

pan

""Seed."

Islands

magma

upon

called ^^seed."

Brix, at

with

Hawaiian

footing of

in the pan.

is

in this way

popularly

be made good grain and test may in this way, and without remelting of string-sugarthe factory produce a singlegrade of product. may The writer has recently introduced a slightly different

method

of

A

of

sugar

boilingwith seed

in Cuba.

The

difference

is

only

grain-sugarobtained from the second or crystallizer strikes is mingled with first molasses to is used preferablyas a footing in This magma form a magma. startingmixed strikes which are finished with first molasses, in the

source

but

it may stored in without

pan

used

also be

The

in first massecuites.

with motion, and crystallizer,

another

from

is

magma

is

following is is boiled

a

without

pan.

convenient

molasses, except when second (mixed) massecuite is boiled

massecuite.

from

molasses

The

method:

pan

purity is very high. A third (crystallizer) A strike The

The

always available loss of time and in this respect is preferableto cutting a

massecuite The

of the seed.

on

this

a

The the

sirup

is boiled.

footing

massecuite

first

of

is

first final.

crystallizer sugar,

unwashed, is mingled with first molasses and in the as a mixed serves footing pan upon which to boil first molasses. Working with cane of very be necessary high purity, it may to mingle the crystallizer sugar

with

second

molasses.

grade of product of

very

This

method

strong grain and

produces any

a

single

desired test.

METHODS

'

OP

BoUing MolasaeS'Sugara. In

many

"

for the process

93

SUGAR-BOILING.

of crystallizationin

not equipped factories, motion, after two crystallizations

in the vacuum-pan, the molasses is boiled to what " is variously termed string-proof,""smooth," " blank," etc. The

is first heated

molasses

in

a

blow-up tank, i.e., a tank

perforated steam-pipes instead of coils. This of melting such crystals of sugar heating is for the purpose have as passed through the sieves of the centrifugal may often for further machines, and purifying the molasses. with

fitted

sugar-makers add lime to the molasses at this stage neutralize its acidity;others use caustic, and still others

Many to

The

of soda.

carbonate

acidity and

if added

salts,at least

lime

to

into

the

and

pan

determination

Carbonate

with

experience, with

to

matter

is

soda

and

ently, appar-

The

advantage.

boiled

of this

string-proof,it is simply drawn

to

down

to

the

tests

finger and

a

required proof varies with

density.

proper

density,by the usual

the "string" between judgment requiring much

drawn

the

up

of

the molasses

the

lime.

boiling molasses

In

quantity breaks

extent.

some

author's

the

is.preferable to

soda

sufficient

into the pan

frequentlydrawn in

in

neutralizes

of soda

carbonate

and

of

The

sample

a

is

thumb,

a

The

experience.

the

purity of the molasses and kind of containers in crystallizingthe used the sugar. from In this crystallizationat rest, as the distinguished of crystallizationin motion, the crystals modem process

slowly settle to the bottom becoming gaining slowly in size,never formed

in

range

polarizationfrom

quality pan-boiUng.

the

89"

The

to

of

"

not

the

boiled

molasses

the

A suitable

to

and

densityfor

90*, apparent

car

or

tank,

large. Such sugars 90", varying in test with

the

skill

displayedin

the massecuite

is

the

mately approxi-

Brix.

mixed

from

strikes,boiled on footings of grained in the pan, though boiled with molasses,

sugars

massecuite are

of

80"

of the

"

in the

sugars

Molasses

term. to

"

molasses

stringtest

"

sugar

and

commercial

is obtained

crystallizedat

from rest.

acceptance' massecuites Such

sugar

crystaland is permeated with molasses. The mixed strikes are grain sugars, and when well boiled are equal has

a

soft

"

to

first sugars

"

except in color.

94

CRYSTALLIZATION

OP

Crystallizaiton in Motion.

39.

used

in the

SUGAR.

THE

^This process

"

first

was

turers beet-industry. Cane-sugar manufacslow in abandoning string-sugarmethods, and were when the strikes were first introduced crystallizerswere into them. boiled blank and run As the name implies, this consists essentiallyin keeping the crystals of a process massecuite in motion while completing the crystallisation. The best results are therefore obtained in pushing the cr3^8tallization

European

and oompracticablein the vacuum-pan pleting it in the crystallizer. * that A theory of the process with the writer's conforms is as follows: If the crystals of experience with cane-sugar so

massecuite

far

is

as

be

kept constantly in motion

and

be

brought intimately in contact with the sugar still in solution, this will deposit upon the crystalsalready present rather sugar reduction than form new sudden of ones, provided there is no a

temperature

to increase

the

supersaturation.

Manifestly it

each impossible to produce a stirringdevice that will move crystal independently, in the heavy, viscous massecuite, to be brought into entirely new environment, so that it may in supersaturated with fresh portions of the sugar contact solution. of motion Further, there is little possiblefreedom for a crystalin a dense massecuite,since the film of molasses is

separating it from

its neighbors is but

a

few

thousandths

of

crystal gradually takes on the in its own immediate neighborhood, reducing the density sugar and viscosityof the molasses surrounding it,and in its increase of size it approaches nearer fresh source of sugar. a Great long exist, since inequality of density cannot the inch

an

in thickness.

stronger solutions

near

by diffusion.

The

by

The

must

motion

mix

with

of the stirrers of the

by rocking the crystals,promotes uniform

fall of temperature

of the

crystalsis

crystallizationcontinues. the

"

crystal size

'"

ceases

Crystallizationof

Int. Sug. J., 14, 284.

sugar

to

A

of the

tion solu-

lizer, crystal-

this diffusion and

in the massecuite.

of temperature, the saturation the growth

the weakened

solution

With

the

a

fall

resultingfrom

changed to supersaturation and point is finallyreached when

increase.

This

in aftei-product

is due

massecuites,"

to

H.

the

vis-

Classen

CRYSTALLIZATION

cosity of the medium

IN

and

95

MOTION.

lack

of

supersaturated this point is reached, the massesolution of sugar. When if preferred with dilute cuite should be diluted with water or Diffusion is again possibleand the crystallization molasses. dilution must be repeated from time The again progresses. is preferableto molasses Water to time for the best results. as

a

diluent

the above

From should into

since

be

to

has

massecuite

should

while

solids to the

massecuite.

that the massecuite

discharging it

be diluted

not

with

molasses

should

increased

begin the moment the viscosityso much With

longer progresses.

readilybe

may

a

high density before

Dilution

no crystallization

condition

add

not

very

vacuum-pan.

fall of temperature the

to

remarks, it is evident

and crystallizer

the

in the

boiled

it does

not

the that

practice this

determined in

in motion

of the by observation the crystallizer.It is able prefer-

by dilution of the massecuite rath r than by boilingto low density. method of boiling massecuites for crystallization in The and preferredby the writer is described in the motion three to

diffusion

promote

**

There three other methods are methods," page 91. of operating,but they have not been entirelysatisfactc ry he has in the author's experience,except the second, which

massecuite

used A

to

limited

a

gKainstrike

a

and

account

on

is usual and

as

hot molasses is mixed

of

with

of about

a

a

local condition:

(1)

part of it is discharged 90"

Brix

is drawn

into

the massecuite

ing. remaining by boilWhen the mixing is completed the strike is discharged is discharged crystallizer.(2) A strike of mixed massecuite

the pan

into

is boiled

the pan;

from

extent

into

and crystallizer

mixed

with

of string-strike density that is flowing from higher temperature and moderate of molasses and string-sugar (3) A magma an adjacent pan. into the pan and heavy molasses is mixed with it is drawn as

a

a

in the first method.

of forming always great danger in these methods writer has used the second method in a false grain. The factory deficient in pan capacity with a fair degree of success. is difficulty in mixing the molasses with the massecuite Thwe Thare

or

is

magma

Among the

older

in these processes. the

advantages

methods,

are

a

of crystallizationin motion

saving of

labor

and

over

floor space,

96

CRYSTALLIZATION

OF

THE

SUGAR.

the production of grain-sugars and the ability cleanliness, turing promptly to liquidatethe factory at the close of the manufacNo

season.

the next

massecuite

need

be

carried forward

to

thus

avoiding loss by fermentation. ^The apLaboratory Control of Crystallizationin Motion. parent Brix and the purity coefficient of the massecuite should be determined to control the density of the massecuite and of molasses. the admixture A sample of the massecuite should be purged in the laboratory apparatus immediately after leaving the pan. The molasses this should be from tested for purity. The immediate molasses from a sample have of 60" purity in the Tropics should of masscuite a purity below 40**. A fall of at least 20" from massecuite to molasses further fall in purity to be expected. The may final molasses depends upon the condition of the cane, and will be less in the Tropics than in Louisiana. The Louisiana and therefore the initial purity of matures cane never the juice is never as high as in the Tropics. The total fall in purity in the Tropics is from 55" to 60" and in Louisiana A final apparent purity number of 25" may from 50" to 55". while the cane be expected early in the tropicalseason is season,

"

immature.

Crystallizers.The "

are crystallizers

of three

types, works: (1)

littleused in cane-sugar This is a horizontal cylindrical vessel crystallizers.

the third of which Closed

usual

is now

trol powerful spiralstirrer. A water-jacket for conwith the Bock of temperature was provided original httle used in cane-sugar These jacketsare now crystallizers. These are simply open tanks factories. (2) Open crystallizers. of half-cylinder cross-section,fitted with stirrers as in the These closed closed type. (3) Vacuum are crystallizers. vacuum-connections and a crystallizersprovided with This is in fact crystallizer steam-jacket at the bottom. with forced circulation of the a slow-boiUng vacuum-pan

fitted with

a

massecuite. The

large extension of present-day factories has led

discharge of the massecuite

through in the pans

to the

the pans into the crystallizers air-pressureis applied pipe-lines.Moderate from

to force the massecuite

pipe-linesshould

have

an

through the pipes. The

internal diameter

of not

less than

_i

SOLIDIFIED

97

MOLASSES.

if the erystallizera are IncheB,especially

14

located far from

the pans.

used

CrystallizerBare firstand

mixed

to

massecuites

for the

extent

some

pending

storage of

opportunity to purge them. the point of view of the crystallization, From it is to use at this stage to further excrystallizers haust unnecessary an

the molasses.

Solidified

40.

this to

The

Molasses."

far

the

as

product is produced only in Java

British India

for arrack

Molasses

apparatus. and

is first

formed, writer is inand

for

ment ship-

manufacture.

of soUdified

manufacture

skimmed

So

molasses

**

requires no "

blown-up

with

special and

steam

is then

simply evaporated to dryness in an operating with a very high vacuum. ordinary vacuum-pan The proof-sticksamples Serious frothing is Uable to occur. tested by cooling in water. The cooled sample should are the characteristics

have a

molten

mass,

hot

very

The

into

run

solidifies

and

covered

are

is

described

below.

The

vacuum-pump

molasses, while

it is

tops of the baskets

burlap for shipment. should be operated for

with

dried

baskets

closelywoven

cooling.

on

The

a

short time after

the pan from to partiallycool the shutting off the steam molasses. Cooling by the circulation of water through the coils is also practiced. Gases are produced by decomposition, therefore the

to break

The

should

be

not

commercial

for this product specifications

solid molasses

(1) The

shall break

fracture; (2) it shall sink in water; indent

to

with

the

whether

^

the

the

results to

a

as

upon

follows:

(2) The

dry substance.

dependent

hard

too

the

before

and

to

extent

the

be

(1) There

temperature.

1

during the

of

a

after

ash

mine deter-

to

occurs

basis

originalmaterial, assuming it were

clean

a

(3) it shall be

solidified molasses

dry substance analyzed the molasses

calculated

conclusions of

examined

loss of

He

with

are

fingernail.

J. J. Hazewinkel

and

stopped until ready

vacuum.

usual

follows:

as

the pump

facture. manu-

drying,

content

constant.

is considerable

of His loss

decomposition is (3) The reducing sugars of the

Archief. 1912, 20, 181.

98

CRYSTALLIZATION

in part pass that

to

reducingHBugar and

of both

SUGAR.

(4) It is possible is due

dry substance

loss of

extent

some

THE

organichoh-sugar.

to

over

OF

organic

position decom-

to

(5)

non-sugar.

equal parts of dextrose and levulose are decomposed. and levulose it is* view of the proportions of dextrose

About In

probable that' polymeiization of dextrose

levulose

to

takes

place during the long heating. **

41.. Froth boiled

Fermentation/'

the sides of the containers. or "

termed

only in the

of

that

hours

some

recent

the

of

cause

"

froth

have

we

are

run

over

ately begin immedi-

may

pheanomenon

fermentation.''

is

It

is

fairlydefinite knowledge

a

It is not

foam.

bacterial

is, to

foaming

or

and

foam

striking. This

"

that

years

The

after

fermentation

massecuites

they often

high temperatures

at

^Wh^

"

activity, but

to

due

fermentation, decomposition of to

the

certain salts. Herzf eld Lafar's

acids, the

^

results

of the

recently shown

suddenly when

Kraisy explains the

C.

65"

until

crystals catalyzes its liberation.

of sugar

massecuite

the

(149** F.) is

by the

phenomenon

remaining in supersaturated solution of

dioxide, is

(sugar-beet) foam

of about

temperature

a

results

that

invert-sugar with amino

Massecuites

foaming.

of

cause

dioxide

the reaction

on

has

Kraisy

glutamic acid, splitting off carbonic

e.g.,

reached.

that

states

in

carbon the

mation for-

The

cosity vis-

Herzf eld

foam.

also

states, always referringto the beet industry, that foaming since the introduction

rare

in

The

This gas.

is to pour

reduces

observed

the

of

water

not

in

foaming

will stop the

the

upon

surface

have

usually fpam.

The

md^ssecuites.

cane

of

in

the

not

a

cane-sii^ar

of the massecuite.

facilitates the been

escape

of

heated

above

conditions

same

beet-sugar manufacture

in

foaming.

stopping foaming

that

provision for

be uncovered

phenolphthalein for rosalic acid

viscosity and

massecuites

Cane

156*^ F. do

have

method

usual

factory

of

Lime

alkalinitytests.

of

is

should crystallizer

A

those

as

probably the

are

the

cause

always

preferably should except while discharging by air-pressure. escape

gases

or

.

^Zeit.

Ver.

ZuckeriDd.,

64, 543.

100

PURGING

is directed

AND

CURING

into the second

SUGAR.

THE

is returned

gutter and

to the pan-

is not reboilingwith rich sirup. This arrangement of the account of the lagging behind satisfactory on very off, which in part mixes with heavy molasses first thrown The 'classificaticm is better wash. the accomplished by for

room

purging as described farther on. Each sugar-drieror purger usually manipulates two centrifugals. to place a man at each It is necessary large machine these to their full capacity in drying very free purgto work ing 24-inch A 40-inch driven centrifugal, by by sugars. belts and working with one operative to two machines, should double

from

purge

4000

4800

to

lbs. of 96" with

the

polarization sugar

the

per

skill of the

quantity varying hour, operative, massecuite and the with the which the quality of the facility centrifugalmay be started and stopped. This capacity may of mechanical be increased by the use dischargers,or selfdischargingbaskets. that is lowered into The discharger is a plow arrangement the

basket

directed

and

basket

wall

against the

of

slowlyagainstthe plow, which

is revolved

The

sugar.

down

cuts

the

valve. by the bottom pushes it out of the machine basket has a steep conical section at The S3lf-discharging have not and the bottom a or discharge-valve. may may The the discharge-valve has a deflector on type without and

sugar

spinele the

or

shaft

basket.

direct the massecuite

to

the

In

other

type,

the

toward

valve

the

wall of

be

raised

may

sugar

with a deflector centrifugalis running. The machine while running. When is charged with massecuite the has been purged and the centrifugalis stopped the

sugar

usually falls

while

the

it without

to lift the it is necessary machines is stopped. These

other

with

of

out

form

freelypurging

sugar

of strong

of white

manufacture

assistance. valve

before

should

be

In the

used

the trifugal cen-

only

grain.

sugar

demands

wash

water

in special care in the centrifugalwith large purging. The sugar is washed quantities of water, upward of six gallons being required A small quantity of ultramarine per charge in a 40-inch machine. The

is often

tinge

of the

added

sugar.

the best results in

to

The

the

method

of

to kill the

double

washing plantation white

yellow purging gives

sugars

CENTRIFUGAL

sets of

Two The

is

sugar

are centrifugals

device

and

for double

necessary

purged in the first set without

little water.

very

101

WORK.

It is then

formed

into

a

**

down

cut

with

magma

"

smip

purging.

washing or with into a mingling the second

from

is elevated to the second mixer and purging. The magma b purged in the second set of centrifugalswith thorough washing. Double two-fold It separates purging serves a purpose: the the dark, low-purity molasses of the first purging from This sirup is of the rich, light-coloredsirup of the second. suitable color and richness to permit reboiling with canemixes the The mingling process sirup to make white sugar. crystalsthoroughly with the light-colored sirup. The friction of

of the

removal

the

crystal against crystal promotes

hering ad-

film of molasses. introduced into Cuba purging was by the writer in the pro* facilitate the handling of crystallizer-sugar

Double to

The grade of sugar and final molasses. is purged without washing and the molasses crystallizer-sugar is discharged into a mingling it is final. The from sugar The and transferred to the mingler proper. screw-conveyor duction

of

one

is lubricated

conveyor-screw

78**

about to

purging

in

or

"seed" Raw

this molasses

to

in

a

is also used

simply

in the a

mixer used

to be storage crystallizer

are

without

dried

mingler The

mixer.

for immediate as

footing

a

usually packed in bags for shipment, and further drying than they receive in the

centrifugals.Their moisture may be reduced by superheated steam in the centrifugal. Raw sugars granulators or driers such refineries (see page 120) provided they be

to

boilingmassecuites.

sugars

Cuba,

diluted

first molasses

the magma. The mingler is is pumped to the first machine's

form

magma

or

Brix, and

with

in

as are

high

use

of also

may

used

are

of

the

in test

the and

of drying is very liable to result crystal. This method cake in the packages. in a product that will harden or The usual Cuban bag holds from 325 to 330 lbs. of sugar 29 inches by 48 inches and centrifugalsugar and measures clean

its tare White

with

is

approximately 2.5 lbs.

sugars

may

superheated

be steam

dried in

in the the

granulator

or

centrifugal.The

dryer or crystal^

102

PXJRGING

lose

SUGAR.

THE

part of their glossin the granuiatorthrough friction

a

with

CXJKING

AND

another.

one

The

American

is accustomed

market

to

possibly prefers it. The gloss is preserved in drying with superheated steam and it is such sugars that such

made

are

and

sugar

The

in Java

for the

should

be heated

steam

home to

and

East

about

200"

Indies C; in

markets.

separate

a

boiler. Various

types of

used

are

conveyors

in

transfixing

sugar

centrifugalsto the packing4"ins. Sugar should not fail directlyfrom the centrifugal into the package, since under this condition it cannot be of uniform quality,and besides harden. Three in general use: are types of conveyors may the

from

(1) Ribbonribbon it.

that

The

revolves

cross-section

(2) Endless attached the

in

to

belt.

chain.

a

is

objectionable feature This

conveyor.

of is

used

very

very

quickly,leaving the

a

leakage of

parabola.

a

hopper (3) Grass-

sugar.

that

is

design. As is is something of the conveyor implied by the name, the motion like that of a grasshopper. A trough is arranged to move slowly forward, carrying the sugar, and then pull backward

sugar

generally in factories

slats

device,but has

efficient conveyor

very

with

sugar

curved-steel

of

efficient

very

a

be

spiral

or

screw

carries the

is often

belt

This

a

trough should

the

of

The

and

trou^

a

is

This

screw-conveyor.

or

Each

sugar.

stroke

advances

All parts of the conveyor

certain distance.

a

Scotch

of

are

the

easily

accessible for.cleaning. be cooled to atmospheric temperature Sugars should before packing them, oth^^isc they usually cake in the package. 43" Classification of Raw ^The basis of the Sugars. American is usually a centrifugalsugar polarizing96*^. market "

This

* *

sugar

based

molasses

is of

test and

sugar

in Java

''

and

be

sugar

95" or

and

tedt

of

96".

seconds.

Muscovado

market

the

instead

crystallizedat rest, but included.

higher

in the American

conditions

market may

vacuum-pan.

be

muscovado,

certain

grained in the

must

This now

sugar

upon

The

' *

The

is there called

Javas.

which next

responding cor-

''

Under

the

price is grade is 89""

formerly always a sugar low-testing grain-sugars are is that made by open-air evaporation was

in coolers crystallization

at

rest.

The

molaases

SUGARS

LOW-GRADE

INTO

by simple drainage. The

b removed

103

GRADES.

HIGH

bulk

of the

sugar

raw

product of the Tropics is of the 96** grade. States Raw entering the United were sugars classified according to the Dutch color standard.

formerly Certain

The countries, notably Japan, still retain this standard. Dutch Standard is a series of sugars ranging in color from a

brown, numbered

dark

very

numbered

These

25.

They

Holland.

bottles

square

of the

given

No. of

Classification

44.

Plantation order

122.

White

grade above

n:ust 45.

market No.

Conversion

Grades.

The

"

White

Tropical 96**

size.

Sugars."

The

cation classifi-

of

method

in

sugars

Indies

Standard.

Low-grade of

white

Java

of the East specifications

25 Dutch

remelting the low

without

in small

trade

sugar

16 of this standard.

Granulated.

or

the

meet

to

sugar, annually in

refineries is produced by the American The plantation product is usually called

sugars

page

on

the

glass and

uniform

of the

white

pure

prepared

are

supplied to

are

almost

an

samples

usually fallsbelow

sugar

7, to

into

Sugars

making

single grade of

a

is described

sugars

High sugar

elsewhere

in

chapter. Low-testing grain-sugarsand string-sugarare ing frequentlyremelted and reboiled to higher grades. Remeltwith is unnecessary be grain-sugars,since they may and be repurged to sugar of high mingled with molasses this

be

polarization. String-sugar must be

or

remelted

in

juice or

part of the

water

used

for

to

"

seed

"

a

pan

reboiling. Remelting

being reboiled several times The remelting with the accompanying decomposition losses. introduce bacterial organisms into the of string-sugarmay

results

in

a

products that 46.

cause

may

sugar

serious deterioration of

Deterioration

Sugars.

in storage. of

Warehousing

of losses

through

with avoidance storage of raw sugar fall in its polarizationhas been a subject

of much

study.^

Jhe

Sugar.

Raw

"

^The

size and

cleanliness of the factory and the

moisture

and

See R.

also

"

The

S. Norris, Bui.

of

character

Sugars

24, Ezpt. Sta. Haw.

crystals,the

packing conditions, the composition of the

of the sugar or the crystaland the

Deterioration

of the

the

process,

content

residual sirup on

1

hardness

on

of the

Storage,"

Piantera'

Ass'n.

ware-

No6l

Deerr !

104

PURGING

house

CURING

AND

THE

SUGAR.

all influence the keeping qualities.It itself,

is also

without possiblethat washing the sugars in the centrifugals, following this with thorough drying in the machines, has an adverse film

effect in storage

of molasses

dilution

of the

account

on

observed that crystal..Claassen the film of molasses when surrounding the crystalsis supersaturated the microorganisms cannot and that the develop has good keeping qualities. Deterioration is generally sugs^ beUeved by investigatorsto be usually due to bacteria and on

the

of the

^

yeasts. for composed of large crystalspresents less area moisture absorption than one made up of small crystals. A hard crystalwill have Uttle molasses adhering to it or penetrating diluted with it. Molasses is hygroscopic and when affords an excellent medium for the activityof bacteria water A

and

sugar

thus be seen that the combination It may of a hard crystalis favorable to good storage qualities.

yeasts.

large and

Cleanliness

of the

eliminate factory and utensils cannot reduce their activity. Further, there are bacteria,but can fewer bacteria and yeasts in a'clean than in an untidy factory. CleanUness is very essential. in the centrifugalwork The wash-water should be pure and the utensils for handling it should be kept in good sanitary condition. have influence upon the an packing conditions may keeping quaUties. If a sugar is packed while too hot, it will condition necessary in the package and the moisture sweat to bacterial activityis thus supplied. The writer has noted a fall of several degrees in the polarizationof standard lated granuwhile that hbt. quite was undoubtedly packed sugar in very It is not usually a simple matter large raw-sugar factories to provide coohng arrangements. The

That

the moisture

influence

the

upon

in

dry

very

sugar

long storage.

conditions. well

keeping

observers.

of many that

content

The

It

will must

of the sugar has a very qualitiesis the consensus

It is

usually hold also

Sugar

be

permissibleupper

but it has been established,

^Beet

quite

now

Manufacture

and

very

a

its

stored

marked of

well-known

ion opinfact

polarization' even under

sanitary

limit of moisture

generallyobserved

Refining, L. S. Ware,

II, 343.

is not that

WAREHOUSING

polarizing

sugars

of

cent

per

damp

less

through

Australia, may

Per In in

the

be

less

should

offset

has

by

of the

be

with

believes

tightly

provided

its

the

that when

it

per

little

in

gain

ization polar-

is

than

in

of

of

that

the

sealed

warehouse of

reduced

non-polarization

Such thus

rise

the

warehouse

sugar

is

should

a

as

whether

to

undoubtedly

deposition

or

it should for

open

be

close

the

on

The the

free

closed

of moisture

temperature. to

difficult

large and

be

should

plan

be

may

of test.

storage

safer

a

Decomposition

test.

during

night

this

that

loss

giving

warehouse

the

that

indication

sucrose.

opinion

of

deterioration

sugars.

an

suitable

a

sugar

"0.333.

indicates

Cuban

original

small

a

the

for

always

the

cause

account

its

to

moisture,

of

pany, Coma

=

suffer

not

may

not

whether

polarization)

moisture

loss

a

judging

Sugar

polarization:

smaller

one

is

1

exposure

Colonial

Experience

somewhat

on

writer

warehouse

practicable. 6

cubic

325-lb.

bag

Approximately

Bpace.

0.333.

The

days

damp

si^ar

than

hermetically

almost

ventilation. on

of

is difference

There

than

very

without even

the

in

sugar

ratio

It is certain

make.

dry.

a

specification

full

place,

(100"

-4-

sugar

that

might

levulose

The

in

higher

polarization

less

suffer

may

of

its

conserve

greater

a

containing

sugars

value

great

suffered

not

dry

a

formula

polarization

of

Gain sugar

be

and

moisture.

the

to

words,

other

storage,

ratio

to

of

moisture

cent

should

of

is of

expected

in

105

SUGAR.

warehoused

air, such

loss

application

be

when

of

RAW

97^

stored

If

currents

The

than

moisture

deterioration. to

OF

feet of

warehouse

sugar

and

capacity 6.5

square

should feet

of

be floor-

'

^

47.

"

REFINING

SUGAR

The

Introductory. "

simple

refiningis

of

process in actual

practice. The working theory,but very complex up of the lower-grade materials,the handling of the sweetmous waters and the control of the char filtration involve an enor-

in

of which

much detail, in this chapter. of

amount

The

and

raw

"margin"

narrow

refined

tended

to

sidered fully con-

the

difference between

or

has

sugars

be

cannot

the

cause

prices of

concentrar

of

shipping industryinto largeunits. The matter of fancy grades of refined the increasingnumber sugar have also helped in bringing about this concentration. Practicallyall of the refined sugar used in the United States is now cipal produced in a few largerefineries situated in the printion of the

faciHties and

seaports. 48.

Definitions.

producing only modifications

Refineries

"

the

and

white

pure

which

those

the soft white

are

of two

classes:

granulated

manufacture

sugar

both

Those and

its

granulated

of lower

purity. chapter as ''hardsugar" and "soft-sugar"refineries respectively. It must be in mind, however, that the soft-sugarrefinery also borne The two types of refineries use produces hard sugars. however, the same essentially process, the soft-sugarrefineries, employing all expedients which will give fine color to their lower-grade liquors. The term "liquor" is used in refiningto refer lo a sugar solution from which no sugar has been removed by crystallization. solution which from has "Sirup" refers to a sugar been is A "sweet-water" a already crystallized. wash-water and

sugar

and

These

refineries will be referred to in this

1

By

Cuba. as

George The

P.

Meade,

methods

it is conducted

Superintendent

described

in the

yellow sugars

American

here

of

the

Cardenas

apply especially

to

Refinery,

sugar

refineries.

106

refining

*

l08

SUQAR

The

Jute-bags

packages. received

are

American

arrive at the

sugars

raw

RBFININa.

the

from

refineryin various

containing

300

Indies.

West

lbs.

330

to*

Hawaiian

kinds

and

of each

Central

packed in smaller jute-bags. Java are packed in palm-leaf ba^ets. Occasionally barrels sugars and used and for musoovadoes concretehogsheads are Each is weighed and package of sugar sampled sugars. before it is dumped. The

are

sugars

into bucket-elevators and is dumped carried to the minglers. Some of the larger refineries have These recently installed storage-bins for raw are sugars. the minglers. The packages of sugar are hoisted p laced above directlyfrom the ship and after weighing and sampling are raw

is

sugar

emptied into the bins. Sufficient sugar is dumped durirg the day to supply the refinery for the twenty-four hours period. The sugar is fed continuously by SCToll-oonveyors the bins to the minglers. This method from of storage materially reduces the cost of handling the raw sugars. with hot water The for the jute-bags are washed empty of the adhering sugar, dried and sold. The wash or recovery is mixed

"sweet-water"

evaporated

to

with

sirup and

a

other thus

palm-baskets are steamed boilers in specially constructed The

barrels

are

steamed

and the

Washing

50.

solutions

the

enters

and

then

and

is

manufacture.

burned

furnaces.

under

the

Hogsheads

and

sold. Raw

The Crystals. enters sugar simply strong scroll-conveyors pro"

minglers, which are with mixing-flights, where vMed

the

similar

it is

intimately mixed

with

"mash." sirup of 65-70" Brix to form a cold magma or is immediately purged in centa'ifugal This magma machines a

of the

type used is washed

in raw-sugar

manufacture.

The

in the

resulting

centrifugalsby graying a The measured quantity of water. purging and washing free and yield a the crystalsof the coating of adhering molasses light-cbloredsugar of from 98.5 to 99 coefficient of purity. sugar

This a

process

sugar

kinds

separates the

it with

raw

material

into two

parts,

one

high purity and the other a sirup of comparatively low purity. This separation facilitates the manufacture and of permits the simultaneous refining Several of very

of

raw

sugar,

e.gr., cane-

and

beet-sugar.

10^

DEFECATION.

''washed

The

weight of

sugar" is dissolved in about in

one-half its

mixing-arms and called a "melter.'' In certain refineries, of the higher some used in melting, but the better grades of sweetr-waters are The melted practice is to use clean hot water. sugar-liquor is pumped to the defecators. water

tank

a

provided with

The

''raw-sugar washings/' purged from the mash, have coefficient of purity of approximately 80" and constitute

a

melted. The weight of raws amount of raw-sugar washings will be greater as the test of the melt is lower, and for sugars having a small or soft grain. A part of the undiluted washings is used to make the with mash and is diluted the remainder succeeding raws

from

14

with

water

or

order

In

hand

18

to

per

dark

cent

and

sweet-waters

reduce

to

of the

sugar

is sent

to the defecators.

through material

losses

being

on

long, it is usual to start the mash with fresh water in twenty-four hours, all the washings on hand at that once time being pumped to the defecators. too

When

small, soft-grainedlow-grade

very

muscovadoes

and

sugars,

such

as

to handled, it is customary them melt directly without resulting lowwashing. The the as grade Uquor is defecated and treated exactly the same washings.

concretes,

Defecation.

are

The

defecators

into

the

''blow-ups'* consist of iron tanks, usually of 3000 gallons capacity, fitted with perforated coils through which exhaust or low-pressure 51.

steam

be

may

blow-up

is

"

blown

or

liquor. The

usuallysUghtly conical

to

of the

bottom

facilitate

drainage and

cleaning. A

great number

of defecants

have

been

experimented with

Blood blood albumen was or formerly refinery work. but its use has been entirely used as a coagulant and clarifier, The defecatingmaterials commonly discontinued. employed for

phosphoric acid. The phosphoric acid be in the form of monocalcic phosphate, phosphoric-acid may paste or a clear phosphoric acid. The monocalcic in the refinery by the phosphate is made bone-dust. action of commercial hydrochloric acid upon

are

milk

of lime

and

This

is called "black

sent

of available

paste," and contains

from

phosphoric acid (PsO^)*

The

10

to

black

12 per

paste

110

REFINING.

SUGAR

chlorides and

co"taind hence acid

increase

these

absorbed

not

are

by the char,

quantity of residual sirup. Phosphoric be made in the refineryby treating bonesulphuric acid. Pastes of this type may be

the

paste may

black

dust with

found

in the market

various

commercial

They

names.

sulphates which will be phate increasing the sullargelyretained by the char in the filters, of the char. The clear phosphoric acid is content made dust with sulphuric acid and by treating bone-black the solids in wooden-frame then filtering out filter-presses. The soluble sulphates are reduced to a minimum by diluting the phosphoric-acid solution to 15** Brix. The clear phosphoric troublesome than the to make acid,while a Uttle more to

apt

are

other

have

under

of

content

preparations named, is the

two

the three and The

high

a

lime

introduces

less soluble salts into the

is introduced

phosphoric acid

as

milk

a

is first added

of about

and

the

a

reaction

faint

acid

formation

to litmus.

reaction

of dark-colored

lime-salts.

Brix.

20"

The

immediately give a faintly

to

If soft sugars be maintained

may

liquors.

lime

afterward, usually in sufficient quantity alkaline

satisfactoryof

most

to be

are

to

made,

prevent

th^

phosphoric acid used is determined by the class of sugar melted, defecating material. low-grade liquors requiring in general more A about

use

available of

refineryhandling

raw

1000

phosphoric acid melted.

sugar

is turned

of 95"

sugars

lbs. of lime

and

(P2O6)

The

from for

average

test

to

600

million

each of

coils and

into the

of

500

the addition

After

amount

the

will

lbs. of

pounds

defecants,

the

blow-up temperature of the time liquor is brought to 180" F.* At the same is added to the liquor. The water washed-sugar liquor is diluted to 54" Brix and the raw washings to 60" Brix, the

steam

densities

being hydrometer.

as

determined

in

the

hot

liquor with

a

organic acids present in the raw and the excess combines with the phosphoric acid sugar tricalcic phosphate. form The to heating and defecants the precipitation of the greater part of the gums, cause neutralizes

The

lime

^ The

Fahrenheit

Used

throughoat

scale

the

is used

in all American

this chapter.

refineries

and

is therefore

albumins

and

pectins. The entrains

precipitatewhich derived defecated

The

liquor

distributed

washed

the

over

whole with

raw

forms

it the

finelysuspended

terials ma-

and

low-grade sugar or they may separate bag-filters

to

filters which

the

heavy, flocculent

a

jute, etc. bagasse-fiber,

sugar,

washings

or

either be sent

liquorsmay be

from

Ill

FILTRATION.

BAG

allowing sugar-liquors,

have

been

used

for

draining period after the

a

high-grade liquorhas been shut off. Filtration. ^The American 5!3. Bag refineries use the Taylor type of filter. This filterconsists of a cast-iron casing box, the top of which is perforated at intervals with holes, or "

each

nipple fitted into it from which is suspended Each element. bag is made up of an a filter-bag or sheath of looselywoven cord, about 6J feet long and

having

outside

diameter, and

in

6 inches

short

a

is 6 feet

which

inside

an

long and 24 inches

bag of cotton-twill fabric

being loosely crumpled in the sheath fluted filter of the laboratories. be screwed

A

The

across.

inside

bag

gives the effect of the

bronze

connection, which

nipples in the holes in the top of the is tied into the mouth of each bag. filter, The defecated Uquor is run which to the top of the filter, on is surrounded by a shallow* curbing, and flows down through the bags, the precipitatebeing retained. The filtered washedmay

Uquor is of a Ught-brown color,quite free of suspended filtered raw-washings are also clear or turbidity. The

sugar matter

darker

of much

but

to the

hours'

the

use

slow.

color.

bags fillwith

liquorgoing on

The

After mud

from

and

fifteen

to

twenty

filtration becomes

to the filter is

very

shut off and

now

the

liquor remaining in the bags is sucked out by a vacuum-pipe, The filter-bags is allowed flushed once to drain out. or are or

twice

with

presses and hang in the each

thin

the mud

alkaline

from

sweet-water

washed

is further

in the

the

bags,

as

they

jetof hot water

into

filter-casing, by introducinga successively.This "sticking" is repeated from

five times

washed

in

after which a

the

bags

series of tubs

are

to

taken remove

filter-

out

three to

of the filter and

all the

mud.

The

sent to the evaporator for conare bag-filtersweet-waters centration. The and water from mud-water, i.e.,the mud the tubs, is limed, diluted and filter-pressed.The press-

cake

is discarded

or

sold for agriculturaluse,

and

the presa-

^

112

REFINING.

SUGAR

partly in flushingfiltersas mentioned is evaporated to a sirup. above, and the remainder is used water, filtrate,

Filtration.

Char

53.

^The char

"

bone-black

or

filters are

and importance in refining. The economy of the refiningprocess depend upon careful control efficiency the

of

utmost

to detail at

close attention

and

this station.

The

filtration

according to a definite schedule,each step in the The entire of thne. operation being allotted a given amount filtration to the beginning operation, from the beginning of one is carried

on

of the next, is termed

the

"cycle" of the filter. The ing seventy-two hours, depend-

cycle will take from forty-eightto the speed at which the rebumed upon

is drawn

char

from

the kilns. Two

systems

of

"battery" and

or

working char-filters prevail: The the

"continuous"

system, all the filters filled in

one

the

In

systems.

"set"

as day are w6rked class doing the same

unit, all the filters in the group In the continuous time. at the same

a

group

of work

each

system,

set-

filter

through its cycle independently, a step ahead of the filter filled inunediately after it. The set-system is used by it lends itself more easily to soft-sugar refineries because the use of doubletheir pan-boiling system and also simplifies continuous The and requires a system triple-filtration. goes

given melt, so it is generally used in the hard-sugar refineries. The handling the same. filter in the two systems is essentially of any one conical The filters are cast-iron vertical cylindrical cisterns, much

char-filter installation

smaller

for

a

bottom, and usually about 10 feet in diameter door feet deep. The top is closed by a movable

the top and

at

and

20

termed

the

the

bottom

The

char

weave

filter-head. for the

serve

rests

cotton

Two

on

a

manholes

removal

of the

perforatedplate

blanket, and

at

the

exhaust^

covered

this in turn

sides

with

with

a

near

black. a

coarse-

blanket

of

finer weave, to prevent the char-dust being carried out with the filtered liquor. The inlet-pipeis at the side of the close to the top, and the outlet ^ at the bottom, below filter, the perforated plate. The outlet-pipeis carried up in a

gooseneck

on

the outside

of the filter to within

a

few

feet of

the top. The

material filtering

is animal

charcoal

or

bone-black.

113

FILTRATION.

CHAR

.

is the

This

granular residue obtained

distillation of bones.

by the destructive

"char." usually called "black" or color from the sugar Primarily, it removes solutions,but, as will be shown and later,organic inorganic impurities are removed

well.

as

melted

It is

The

ratio

of bone-black

used

to

sugar

varies

but the best widely for different refineries, burned for practice requires at least 1 lb. of bone-black melted. pound of raw-sugar The following are the various steps in the cycle of operations^ considering any one filter: Fillingthe filter with char; tion covering the char with liquor; running the liquoror the filtraeach

washing the Uquor

proper;

and

water;

the

arrangement The

retorts.

Char.

speed with which

The

kilns.

char

with

hot

the revivification of the char.

Filling the Filter mth upon

of the

out

draw

of char

^The time of

"

the char

is dependent filling be drawn

may

is controlled

by

from of

means

operating small doors at the bottom is that at which fastest possible draw

burning of the char

a

of

the cam

the

proper

The tion distribujust be maintained. of the bone-black in the filter is of primary importance. If the dust and largergrains of char are not uted evenly distribthe liquor will flow through the throughout the filter, culties difficoarser particles,forming channels and causing many distribution during the washing-off period. Even be obtained

may

in many

designed

devices delivered

can

to

into the filter by

stem, the funnel

have

a

there

of

means

being turned

several

are

this result.

secure

bent

and

ways

The

funnel

a

patented

char with

may a

be

slightly

intervals

by hand or An effective method in of filling continuously by a motor. the char is to deliver it into the filter promiscuously and man

the

received

the

enter

material

sufficient

at

cistern from

with

a

shovel.

char, this is drawn

time

to

After up

into

time the a

cone

and

tribute dis-

filter has in the

middle. **

Covering^* the Bone-black

Liquor. Air-pockets in be avoided. the char must To prevent these, the liquor is deliveried slowly at the base of the cone of char, with the head down of the filter off. The Uquor runs the sides of the filter until it reaches the blanket, then flows across the whole width

of the

filter at

the

with

bottom

"

and

rises,forcing the air

114

REFINING.

SUGAR

out

through the

the

covering.

When

the

liquor begins is closed

goose-neck tiie outlet-valve until

filter is filled.

the

is kept dry throughout

char, which

of

cone

The

to

and

head

is

flow

liquor is put

now

the

from

in

run

the

on

it under into liquor is turned pressure (15-25 feet head). The covering usually requiresabout four

filter and

the

hours. heat

Considerable to well-burned

on

is

hot

generated when With

char.

the char

liquor is first run

at

of

temperature

a

liquor at 165", the outflow during the first few hours of running will normally have a temperature tions, these condiIf covering is stopped under of 185" to 190". if filtration is suspended during the early stages, or rise to such a point that the the temperature in the filter may 140"

to

the

and

160"

liquor will be scorched.

The

should

char

be

cooled

to

at

and every precaution filters, should be observed to avoid interruptionsto the flow of liquor during the covering period and until the temperature of the outflowing liquor is practicallythat of the liquorentering it enters

before

150"

most

the

the filter. The

FiUration,

filters (99" four

washed-sugar liquor from

The

"

purity) is run

hours

or

longer

on

at

a

the filter at

160"

of about

150

rate

the

bag-

F. for twentycubic

feet per

sirups from granby dark-colored ulated this in turn strikes (90" purity) and by low-grade sugar-liquors,bag-filtered raw-sugar washings, sirup from other low-grade material which remelt strikes or any it is successive advantageous to filter. Each grade is of lower purity and in general the speed of flow is reduced and the hoiur.

is followed

This

raised

temperature

with

each

reduction

grade of liquor follows the preceding

one

of

purity.

without

a

Each

break

in

the filtration. In

where soft-sugar refineries,

the

low-purity liquors of

essential,all the liquorswhich are not used to produce granulated sugar are double or triplefiltered. The lower-grade liquorsfrom one set of char-filters will follow the washed-sugar liquor on a succeeding set and the darker runnings from this set will in turn be carried on the third set. fine color

The not

are

third

re-filtration

removes

materiallyraise the

purity of the

liquors.

second

and

color, but

does

116

SUGAR

in

and

general consist essentiallyof

the waste

the wet

char enters and

The

the kilns

from

gases

conduct The

the surface

about

with

kilns consists of

passes.

cross-section

3 inches

a

3 per

ting-plates this casing. of moisture

cent

cent.

flanked

ends and

pipe-retortsthrough which

of

The

of

20 per

fired at both

furnace

triplerows

12 feet

to

Deflec

slowly over the driers carrying about

leaves them

10

casing through which

a

drawn.

are

char

by double or char slow'y and

REFINING.

retorts

of cast

are

by 9 inches long. The retorts

or

3 are

iron, of oval

inches

by

heated

to

during the revivification. The rebuming of the black decomposes oxides"and carbonizes the organic matter

the

12 a

inches

dull red

heat

to

failed

to

This

remove.

carbon

carbonates

some

which

remains

in

the washing the

pores

such as is black, and since it has no decolorizingpower possessed by the constituent carbon, it merely clogs the of the char and decreases its filteringvalue proporpores tionately. The Weinrich decarbonizer, designed to remove this added carbon, is a revolving drum, slightlyinclined to the horizontal,with a carefullyregulated fire under it. The the char passes as vegetable carbon is burned away through the drum, thus increasing the porosity and prolonging the

of the

life of the bone-black. The

char

is

dropped from the retorts of the kilri, through coohng-pipes, upon belt-conveyors,and is carried by these and

elevators

cooled

on

through

to

the finer

remove

The

particlesand

bone-black

the dust

is

before

it

again filled into the filter. char

New

loss in

the

in

is shown

is added

dust

The

defecation The

is used or

in the

given:

in

course

making

same

to

time

to

compensate

for

gradually deteriorates,as A refineryusually renews of every

two

phosphoric acid

three years. for use in the or

is sold for fertilizer manufacture.

Composition of Bone-black

Analyses of the

time

from

screening. The char the next paragraph.

all of its bone-black

of

If necessary the char is further filters by passing it over pipes

its way the to cold water is circulated. which

screened is

to the filters.

new

bone-black

black

after

and

Its Alteration

of American several

months

by Use,

manufacture of

use,

are

"

and here

CHAR

117

FILTRATION.

After months'

Black.

New

Carbon

9.61

Insoluble

silica .

.

.

.

sulphate. sulphide.

Calcium

use.

10.80

.59

.67

.16

.55

.06

.24

.

Calcium

six

.

carbonate

Calcium

4.48

8.92

.23

.06

Iron

Undetermined.

80.70 .

83.13

.

.

100

Weight

per

Weight

per

cubic

foot,loose cubic foot,packed.

43.8

lbs.

54.5

....

between

Percentage mesh

100

16

and

48.5 .

lbs-

59.1

.

30

sieves

84.8

always contains some nitrogen, which is apparently The essential to its decolorizing properties. r61e

Bone-black

this

plays in the filtration has contains

black

be

must

efifect upon char

new

a

considerable

removed,

since

not

of ammonia

amount

they would

the color of the filtered be

must

determined.

been

throughly washed

have

salts,which a

detrimental

liquors. For this and

New

burned

reason,

before

use

for filtration. As

is shown

by the analyses,the composition of char alters

of the steadily because fication. deposition of vegetable carbon in the pores during the reviviThe calcium sulphate increases by the removal of The sulphide sulphates from the liquors and the water. with

use.

The

carbon

increases

tion sulphates increase,due to the reducof the latter by the organic matter during the burning. calcium carbonate The drops sharply during the first few washings and burnings and finallytends to reach a balance

tends

around

to increase

5 per

as

cent.

the

The

iron increases

slowly. Of all these iron are the most tionable. objec-

impurities the calcium sulphide and Appreciable quantities of these two constituents will give a greenish color to the filtered liquorsand a gray cast to

the sugars

boiled from

them.

A

bone-black

may

become

118

REFINING.

SUGAR

unfit for

if the calcium

use

addition

constant

0.4 per

burning, together with the black, will prevent the sulphide

new

becoming abnormal.

from

content

of

sulphidecontent exceeds and

washing

Thorough

cent.

"

Bone-black not Sugar Solviions. but also absorbs color from the sugar solutions, only removes organic and inorganic impurities. The black is selective in its action, certain classes of material being retained by it Solutions containing color due more strongly than others. Gums not easily decolorized. to overheating (caramel) are Action

of Bone-black

on

"

strongly held by the char and no amount them. of washing will completely remove Of the salts,the carbonates, sulphates and phosphates are readily absorbed, and

albumen

are

the chlorides and

while

Invert-sugar

extent.

than

greater extent with

the

hot

nitrates or

absorbed

not

are

to any

"glucose'' is absorbed

sucrose,

but

is

to

largely washed

a

out

great much

again

Consequently the glucose ratio of the filtered liquors is lower than that of the unfiltered,while the ratio of the diluted runnings and sweet-waters is very much combined onflow higher. The compared with the combined filtrate shows This practicallya glucose balance. water.

'

acid-liquorsor inversion In from

actual 80 to 85

the mineral

and

well-burned

burned insufficiently occur

may

control

correct

a

presupposes

With

char, heavy losses by

in the filters.

refinery practice, the bone-black 30 to per cent of the color,from

matter

char.

or

"ash," and

from

50

to

will 40 60

absorb

per

cent

of

per

cent

of

the

of the combined organic non-sugars onflowing liquors. 54. Crystallization of the Sugar. Classification of the Ldquors. The liquors are classified at the filter outlet-pipes according to their purity and color and are distributed to "

"

storage-tanks

near

the

vacuum-pans.

In

the

continuous

in which filters are at the same two no filtration, phase of their cycles,all grades of Uquors are flowing at the time. The classified about follows: as same liquors are First liquor: Filtered washed-sugar liquor, "water white" and of 99" to 99.5" purity; second liquor:Filtered granulatedsirups,off-white or slightlyyellow and of 90 to 93" purity; third liquor: Filtered or double-filtered washings or lowgrade meltings,golden yellow and of 84" to 87" purity;fourth

system

of

OF

CRYSTALLIZATION

liquor: Last runnings,too dark and of 75 to 80" purity. the "set"

Where filters of

a

set

and

are

THE

to make

119

SUGAR.

granulated

sugar

of filtration is in use, all the kind of liquorat the deliveringthe same

system

there is not

the

fication. necessityfor a rigidclassiThe distribution on the pan-flooris made to suit the needs of the boiling-system. The vacuum-pans used in refiningdo Boiling to Grain. not differ from those of the raw-sugar factory. The general in the two branches of the manipulationsis the same principle 1 but from the nature of the product, greater of the industry, be exercised in the refinery. This is due to the must care necessityof boilingsugars to certain specifications as regards hardness and of the The size the crystals. factory raw-sugar uniform aims make of size to and hardness a only usually sugars of grain. In boilinggranulated and other hard sugars, a high pan-temperature is maintained (180"), while for which small soft sugars, in a grain is desired,low spongy temperatures (120"-130") prevail. hard sugars only are to be made, a fixed system of When boilingmay be adhered to. The first hquor is boiled for the fancy grades, cubes, cut loaf, confectioners' sugars, etc. The sirupspurged from these strikes are boiled back with more liquorto make the ordinary granulated. The boilinguntil the sirups,usually of about is continued back 90" color that they are no longer suitof such able purity, are returned to the for reboiling. These sirups are now refiltered. The and are second liquor and the bone-black boiled to make third liquor are "oflf-granulated"sugar. This is a slightly"off-color" sugar which is disposed of by graduallyand slowlymixing it with the better grade of granulated time

same

"

strikes. strikes are boiled with sirupsfrom the off-granulated fourth liquorfor "high remelt" strikes of 75" to 80" purity. to a high test (98" of these strikes are washed The sugars purity)and are melted directlywith the washed raw sugar. The sirups from these strikes are boiled back on a footing strikes of about 67" purity. These of fourth liquorto make The

1

See

page

90, relative to sugar-boiling in the raw-sugar

factory.

I.J

120

REFINING.

SUGAR

where they are kept discharged into crystallizers in motion during two to three days. They are then purged and yield a sugar of from 85** without the use of wash-water be mixed with high-testraws to 90" purity. This may sugar are

magmas

and

with

be them, or, preferably it may and be submitted directlywith other low-grade raws already described. processes The sirups purged from these low-grade remelt

washed

the residual

melted to the

strikes

syrup" of the refiners. The procedure in a soft-sugar refineryin boiling the high the same that already as Hquors to granulated sugar is much described. The soft sugars are graded according to color, varyingfrom an almost pure white to a deep brown sugar. The lower grades of liquorsfrom a set of char-filters are boiled form

"barrel

sirup or

purity, which planned to yield sugars of the desired colors. The sirups are either boiled back directlyor are from soft-sugar strikes are the needs require. The varying demand first char-filtered, as for the different grades necessarilyprecludes the possibility to boil of a fixed boiling-system. It is frequently necessary for "remelt," as in the hard-sugar houses. At times sugars be so large that but a very the output of soft sugars may barrelsmall percentage of the impurities is turned out as

into

series of strikes of

a

successively lower

sirup. 55.

and

Drying

of the

Finishing

The to

white

sugars

remove

"

The

tion separa-

such

factories

very

thoroughly washed

in the machine

is effected

from

adhering

by

{42)

are sirup. The moist sugars the centrifugalsto distributing-bins above

all

veyed

are

Product.

sirup in the magmas used in the as are

the

crystalsfrom

centrifugalmachines

the

.

con*

the

granulators. The for one

bulk

of the white

drying. The another, hence The

diameter

its

granulator is and

is sent

through the granulators granulator also separates the crystalsfrom an

sugar

name.

iron drum

(Fig. 17) about

6

feet in

long, slightlyinclined to the horizontal toward the A discharge end, and revolving on trunnions. shelves attached series of narrow to the inside of the drum, to lift the sugar and let it fall through longitudinally,serves heated air as the drum The air is heated either by revolves. 20

feet

DRYING

of

means

steam-drum

a

granulator end

of

FINISHING

AND

by

or

the

drum.

The

the

granulator by

removes

the

sugar-dust.

the other.

lower

with

The

central

a

partly dried

upper-drum

is required

steam

The

and

complete

t"

should

sugar

drum.

steam

leave

preferably below

110".

special provision

for

quite the

the

cooling the

hot it is very

falls from

the

according

to

the

bins.

The

screened

containere

other

deliver

"shakers"

sugar the

as

the

during

small

machines

packages. The

in cartons. or

mixing

very

little section.

comparatively

packages.

cool, make

to

necessary

in the of

paciied

n.arkct

various sugar

is packed

The

which

screens

into

in barrels,

lumps

the

and

packingand

bags

Barrels

refineries

sugar

classify it

the

remove

requires.

such

rest

upon

equipped

are

permit the packing

used

Cubes

and

the

in filling,weighing cut

loaf-sugars

practice of wrapping

in moisture-proof

introduced

kinds oi

are

European

"dominoes"

service, has been The

hence

ot

sugars

the day-time only.

Automatic

cubes

the

hot,

products

lai^e storage-bins which

with

the

leaves

If sugar

filling. Certain

while

and

sugar

drum

crystals,

is

heater

a

sugar.

set

a

the

size of

and

dust,

coarser

to

a

17.

liable to cake

granulator

of

series,one

The

It is sometimes

Fia.

while

in

drying in the lower

lower

also

type.

is fitted with

upper

fan

(Fig. 17) is

usually operated

are

and

pipes

The

fan.

of the

dischai^

the

illustration American

the

at

over

exhaust

an

The

granulator-dnims

above

is drawn

the usual

granulator,

Two

ot steam-pipes

air

through Hersey

121

PRODUCT,

extending through the middle

large group

a

THE

of lumpproper

into or

the

loaf-sugars

grain with

a

are

two

ing clos-

packed three

or

for restaurant

paper,

United

and

States. are

heavy

all made pure

by

sugar-

122

REFINING.

SUGAR

is variously treated, This magma sirup to form a magma. to form cubes ^by pressing,molding or in specialcentrifugals, slabs

directlyor dried.

cubes

The

closets.

The

and

These

usually dried in hot ready for packing after they have been

bars.

are

slabs and

bars

cut

are

are

sawed

or

to

form

cut

and

loaf-sugar. These are broken down in making crushed loafHsugar. Powdered ness or pulverized sugars of various degrees of finemade granulated in a mill and by grinding coarse are passing it through bolting-cloth. which Brilliant or candy "A" is a large grain sugar is barreled while moist,just as it leaves the centrifugal-machine. Confectioners' '^A'' is a smaller grain-sugar packed in the sawed

same

way.

The

soft

described.

white

sugars,

These

and

yellow, have already been packed while moist, directly

are

sugars

ing centrifugals. The soft sugars are classified accordto a series of arbitrary trade color-standards. Granulated forms now a large part of the output sugar ments. of a refineryand the total product of the smaller establishThis grade is classified according to the size of the crystalsas extra coarse, coarse, fine and extra fine granulated. The ordinary commercial granulated is the fine grade. Fruit granulated is the finer screenings from fine-grained sugar. from

As

the

has

been

explained in an early chapter of this work, the size of the grain is determined in the pan-boiling. " Barrel ^The sirups purged from low56. Syrup." "

grade remelt strikes form the residual sirup which is usually As rule the sirup is packed in barrels for the market. a diluted

55** Brix

to

and

reboiled

"smooth"

before

barreling.

Certain

refineries pay especial attention to this sirup and char-filter it to improve the color before reboiling. This

sirup varies in composition through rather wide rived limits,depending on the class of sugar from which it is deand as

16 per 57.

in

Polarization

follows:

cent; ash

a

other

upon

6 per

cent;

factors. 34

per 22

water

be typical analysis would cent; reducing sugars 22 per per cent; organic non-sugar A

cent.

Yield

of

refinery is

Refined

expressed

Sugar. in

"

The

percentage

yield of terms

of the

sugar raw

^

^

124

SUGAR

REFINING.

and a sampled and analyzed, as in the case of raw sugars, weighted average analysisis calculated for the period. The barrel-sirupis sampled and measured by lots and the' density and polarization of each is determined. Weekly of made a analyses are complete composite sample and a weighted average analysis for the technical period is computed. At the end of every period usually the technical an periods include four weeks inventory of the material in process is made. All material containing sugar is measured and sampled. The density and purity of the samples determined. The pounds of solids are computed from the are "

"

of the

volume

cubic

per

in cubic

material

foot,

indicated

as

feet and

the

pounds solids density. The solids

by the

The solids less multiplied by the purity give the sucrose. the sucrose give the solid impurities. In this way the total and total impurities in the stock are solids,total sucrose ascertained.

To

these

compute

figuresto available sirup and

be assumed that all the granulated sugar, it may impurities will go to make sirup of the same composition as that produced during the period. available

Then:

Lbs.

solid

impuritiesin stock

cent

solid

impuritiesin sirup produced

Per

lbs. available

=

figure would

loss

such,

than

to

refinery

a

of

of

expense

securing

the

to

(1)

refinery,

determined.

customarily

now

exceptional

no

sirup in stock;

practical value

more

as

having and

complications

be

not

number

the

X 100

This

conditions.

temperature

accurate scientifically

aa

refers The

data

are

prohibitive. be

not

temperature C.

desirable

condition

This

A.

above The

96"

corrections

or

be

only

may to

technical

(G. L. S.)

a,

approximation

of

excessive

either more

Sugar

properly

control

a

less

or

p.

to

true

the

laboratory

nature.

Dr.

shown

that

has

260)

figures

irregular heat.

of

arbitrary

Analysis, applied

to

and

polarizing

cane-sugars

beet-sugars. of the

statements

accomplish

conditions,

of of

(Handbook

and

closer

a

locations

necessitate

control' figures and

they

in

would

Browne

corrections

that

clear, however,

It is not would

one

where

this

very

report

refinery

temperature

designed

are

successfully. is

to

fluctuations

comparable

Under with

give are

average

its

tive compara-

not

sive exces-

ture tempera-

predecessors.

125

INTRODUCTORY.

available sirupin stock X polarizationof sirupproduced

Lbs,

100

=ibs. Total

in

sucrose

available

stock"

in

sucrose

granulatedin

in

sucrose

sirup in stock.

sirup in

stock

(2) =

lbs.

stock.

Example: Assume

a

stock

of 1,180,000 lbs. solids

in process

^50,000 lbs.

sucrose

330,000 lbs. solid impurities. Assume

a

barrel-sirup produced

containing:

as

Sucrose

34.2%

Water ,

Solid

.

impurities(ash,glucose,organic)

22.1% 43.7% 100

330,000X100^ 778

lbs. available '

43.7

sirup; H,

.

(1) V /

032X34.2

^=258,261

"

lbs.

in

sucrose

in.stock: sirup y

100

f

(2) \ /

850,000-258,261 =591,739 lbs. available granulated in stock. The stock

increase in process

or

at

in

decrease the end

the

of the

available

period

as

granulated ia compared to that

the actual from beginning is added to or subtracted tion calculaproduction of granulated for the period; the same is made with regard to the sirup produced and the sirup These and in stock. net productions of sugar sirup arq fcr the period. at

the

These of

net

weights produced

melted

are

each

divided

by the weight

give the net productions per cent melt. and The. analyses of the granulated, the soft sugars sirup calculated to per cents of the melt by multiplying each are constituent of the analysis of each of these three products of the melt. by the percentages of the product in terms The of these analyses p^ various constituents cent of the raws

to

126

SUGAR

melt

be

can

totaled

REFINING.

give the analysis of the combined

to

of the

A refinery in terms of the melt. comparison of this analysis with that of the melt itself gives the

output

increase of

decrease

or

of each

constituent

during

the

of net

yields for

process

refining. To

illustrate

this,let

us

assume

set

a

refineryperiod and calculate the loss in Polarization

of the melt. .

.

for the

sucrose

a

period:

.94.9**

Net

yield of granulated Soft sugars produced Net sirupproduction

84.

3% 8.9% 4.6%

at 88.8**

polarization polarization

at 34.1"

Then, in melt

Sucrose

94 .

84 in

Sucrose

granulated %

melt

"

=

"

84

30 .

8

in soft sugars

Sucrose

3X100 '""

=

90

% melt

9X88

8

=

=

7 90 .

4.5X34.1 .

Sucrose

m

"

or

in total

Sucrose

melt1

%

sirup

^ =

"

"

=

"

^"

1

63 .

product %

melt

93

73 .

lost in

Sucrose

refining% melt of

invert-sugar,ash, water

and

same

17 .

method

Following this loss of

1

the gain calculation,

organic

non-sugar-

or

may

be traced. Rouiine

Control.

The

"

depends largely upon materials

in the

routine

control

determinations

successive

steps of the

of

of the refinery the purity of the

process.

The

char-

entirelycontrolled on a basis of purity. of these purity tests required day and night is The number in a separate so large that the work is usually conducted floor,by boys trained laboratory,on or near the vacuum-pan free to do to do only this testing. This leaves the chemists the analyticalwork involved in the technical control. filterand

pan-work

are

The work.

The

of Casamajor is used

purity method

dilute

material

any

convenient

and

the

"

"

Brix

is clarified with

is determined.

15" and

20"

to

Brix,

part of the

A

subacetate

dry

Home's

in this

sirup is diluted

or ^liquor, magma density,usually between

corrected

127

METHODS.

ANALYTICAL

SPECIAL

tion solu-

lead, if such

of

and after filtration it is polarized preparation is necessary, directly. The polariscope reading multipUed by the factor corresponding to the degree Brix givesthe purity coefficient. The

factors

computed

are

from

formula

the

Factor

=

'-

The

TTT**

-;

Sp. gr.X degree

puritiesfor

table of

of Home's

figuringis simplifiedby the

use

Brix use

in

refinerycontrol,given

p"ge 526.

on

Methods.

Analytical

Special

59.

ri^tinemethod

Black

"

Paste.

"

^A

determining the available phosphate-paste is as phosphoric acid (PsOs) in monocalcic convenient

Wash

follows:

10

Make

to the

up

Titrate

20

paste into

of the

grams

distilled water,

with

for

mark, mix

up

the

of the

flask

200-cc.

lumps with thoroughly by shaking and

breaking

of the filtrate (1 gram

cc.

a

rod.

a

filter.

normal paste) with tenth-

alkali^using methyl-orange as the indicator. hydrochloric acid. gives the aciditydue to uncombined number

of

cc.

of

alkali,with methyl-orange

N/10

This The

indicator

hydrochloricacid (HCl). 20-cc. portion of the filtrate, Titrate a second using pheThis titration gives the total acidity nolphthaleinindicator. the free acid. The culations caldue to the acid phosphates and X 0.365=

per

cent

free

made

are

follows:

as

Number

phenolphthalein indicator"

with orange

indicator X 0.35=

per

cent

of

N/10

cc.

available

cc.

N/10

alkali

alkali,methylphosphoric acid

(P2O5). Bone-black:

Preparation of the Sample, ^After thoroughly by subsampling. mixing the sample reduce it to 200-300 grams Pass a magnet through a thin layer of the sample to remove of particles and a

filters.

"

iron'that

may

have

Grind

about

100

porcelain mortar

through kept in

a a

moisture,

lOO-mesh

to

a

gotten into it from grams

of this

prepared char in

powder, all of which

sieve.

The

tightlystoppered bottle

should

pass

be sample prevent absorption of

ground to

the retorts

must

128

Bone4)lack: the

REFINING.

SUGAR

Determination.

Moisiwre

^Heat

"

of

grams

hours

during four

portion of the subsample

unground

6

'

at 110*' C.

ground char with

of the acid

and

50

water

and

weight Loss

the

contents

Residue

and

water

100

of

mix

and

in page

washed

by

sulphate -5(CaSOO.

20

and

crucible

the

wash

residue

carbon;

cent

cent

per

insoluble

matter.

Sulphate. ^To 2,0

of Calcium

"

150

cc.

about.

100

cc.

water, and

dilute to the mark 200

(

cc.

=

Proceed

with

after

water,

of

char) of with the analysis as is 20

grams

362, using the concentrated

solution obtained

sulphate precipitateshould be first Calculation: barium decantation. Weight cent 5833 X 100 calcium-sulphate X per barium

The

above.

Evaporate

about

the filtrate to

as

hydrochloric-

lamp.

temperature,

room

filter.

described

a

Add

Boil fifteen minutes.

cooling to

2 grains

powdered char, in a 250-cc. flask,add 25 cc. concentrated hydrochloric acid, gradually. cc.

of the

grams

^Treat

gently for fifteen minutes,

Boil

Determination

Bone^lack:

"

of concentrated

cc.

ignition-J- 2X100= per 2X100= after ignition-r-

on

Moiter,

cible Dry the crudisappearance of chlorides. at lOO** C. and weigh; igniteto constant

the flame

over

10

Gooch

tared

a

to

Insolvble

of water.

cc.

filter through with

and

Carbon

Bone-black:

=

.

Bone-black:

Determination

of Calcium

Sulphide, "

^To

25

of powdered char in a 250-cc. flask add 0.5 gram potassium chlorate,then 25 cc. of boilingwater and follow this with 100 cc. concentrated hydrochloric acid,added very grams

of the

Proceed

slowly. described

above.

as

in the determination Great

care

must

of calcium

be exercised

in

sulphate,

adding

the

in order that no sulphur be lost as acid, very slowly at first, sulphate obtained hydrogen sulphide (H2S). The barium of the sulphide and in this analysis corresponds to the sum for Subtracting that already found sulphate in the char. the calcium-sulphate leaves the barium-sulphate equivalent to

the

calcium

-^

20 X.

phate"bariu sul(Total barium sulphide. Calculation: calcium from the phate) sulsulphate derived calcium 3091X100= sulphide (CaS). per cent

ANALYTICAL

SPECIAL

Bone-black:

Vclumelric

Determination

of the Iron,^

followingreagents are required: potassium permanganate: (1) Standard of the salt in 1000

grams

against

solution

iron

an

Dissolve

follows:

2.5

Dissolve

of water.

cc.

129

METHODS.

of

known of

Check

^The

"

4

5

to

this solution

strength, prepared

piano-wire,or

aa

of the

grade of iron wire that is prepared especiallyfor standardizing, in a small quantity of hydrochloricacid,and dilute this solution Use 50-cc. portions of to 250 cc. in a graduated flask. this solution in

under

grams

the

conditions

of the

standardizing the permanganate. (2) Phosphoric acid and manganous

50

grams

water, add

analysis,as below, solution:

of manganous with the addition

250

sulphate crystals in about 250 cc. of of a few drops of sulphuric acid; of phosphoric acid solution of 1.3 specific gravity,

cc.

followed

in order

by 150 sulphuric acid.

and

of water

cc.

The

cc.

of

phosphoric solution

may

100

the 85 per cent acid (H8PO4). chloride solution: Dissolve 30 (3) Stannous

prepared

centrated con-

be

from

granulated tin

in 125

cc.

heating. Solution

with

Dissolve

of concentrated is

promoted

of pure

grams

hydrochloric acid,

by the addition

of

a

pieces of platinum foil. Dilute the solution with 250 cc. and filter it through asbestos. Add 250 cc. of conof water centrated hydrochloricacid and 500 cc. of water to the filtrate.

few

(4)

chloride

Mercuric

salt in 1000

cc.

Proceed

with

the

powdered

the

the

analysis as follows:

bone-black

of the

50 grams

and

Ignite

10

grams

digest the residue with

30

of cc.

hydrochloric acid, with gentle boilingduring Filter the solution through a Gooch crucible

fifteen minutes. wash

Dissolve

of water.

of concentrated

and

solution:

residue

thoroughly with

small

quantities of

contained in a largeErlenmeyer filtrate, chloride solution flask, to nearly boilingand add the stannous to it drop by drop until the yellow color disappears. Add chloride solution,all at once, and" mix 60 cc. of the mercuric well by shaking the flask; add 60 cc. of the phosphoric acid

hot

and

*

Heat

water.

solution and

manganous

Adapted

the

from

5th ed., p. 206.

Clowes

and

600

cc.

Coleman's

of water.

"

Quantitative

Analysis,"

r

130

SUGAR

The

titration of the

conducted the

in the

solution

flask be

may

The

flask,in the

and

the

the

standard

washings

REFINING.

material

placed

prepared as

above

be

may

white

background or a large porcelain dish. should be thoroughly washed a

over

transferred

latter case, added to the

to

solution

solution

in the

from

dish.

Add

burette, with until the Uquor assumes constant a faint pink color, stirring, which should disappear after three or four minutes' standing. Make the a similar titration of the solution prepared with iron wire solution.

to

permanganate

ascertain

The

iron

value

of the

permanganate

percentage of iron in the char may

calculated from Bone-black:

the

9,

the data obtained Calcium

in the two

Carbonate

be

readily

titrations.

and

The Phosphates. calcium carbonate be determined by the methods on may This determination is of less importance than 389. page priorto the invention of the mingling process (50), when it to filter highly alkaline beetnsugarsolutions. was necessary The percentage of phosphoric acid is of no particular the is to be sold on basis a significance, except spent char value. In this its the of fertilizing event, customary methods used. of agricultural analysisare Bone-black: Thoroughness of the Revivification,^The test of the efficiency of the revivification is of very great value in the control of the kilns. Tests are made at very frequent intervals throughout the day. volume of char add an To a measured of equal volume sodium hydroxide solution of 9" Brix. Heat the mixture in A a boiUng salt-water bath for two minutes. properly burned char will impart no color to the soda solution. A yellow or a brown color indicates a poor revivification (underburning), the depth of the color being directlyin proportion of organic matter to the amount remaining in the black. An excess of sulphides will give a greenish cast to the solution. "

"

O^erburning occurs part of its lime caustic soda

when

the char is heated

is converted

solution

remain

into

the oxide.

uncolored

so

hot that Should

a

the

in the test described

sample of the char should be shaken with distilled and a drop of phenolphthalein solution added water to it. Overbuming is indicated by the solution turning red,due to above,

a

132

colors

the

REFINING.

SUGAR

the

of

unfiltcred

filtrates and

liquor and

make

The absorption of percentage complete analyses of each. well as the improveas ment color, ash and organic non-sugars, in purity and the change in the glucose ratios may now of the be calculated for each char, using the constituents A supply of a good grade of unfiltered hquor as a basis. should

bone-black such

many

tests

be

kept

as

standard

a

of

comparison, if

to be made.

are

It is essential in all tests of this character

that all the

ditions con-

experiment shall be identical for all the samples Certain of black to be compared. points of the procedure best must necessarilybe arbitrary and the conditions can of the

be

chosen

to

In

so

temperature, etc., should

particularrequirements of the ment. expericonditions far as is possible,factory as regards ratio of char to sugar, density of the liquor,

suit the

be maintained. of

decolorizing power

The

of

means

a

colorimeter.

is determined

bone-black

for this purpose

instrument

Stammer's

by

form, and the results obtained by This instrument consists different operators are comparable. for comparing the depth of essentiallyof an arrangement is

color

of

convenient

very

a

colunm

a

of

glass plates. An of the of

a

solution

disk, and

eye-piece and lowered

by

column

of

sugar

eye-piece is under

that a

means

so

with

standard

arranged that

examination

appears

upon

coloredthe

color

one

half

of the standard

The glass on the other. tube containing the glasses are raised and of a rack and pinion, the length of the

solution

length is shown

solution

being varied scale

at

the

time;

same

this

pointer carried by slide. The the a theory of this instrument depends upon variations in the intensity of the color of the solution,proportionate In using the colorimeter to the length of its column. seen

a

object is

the as

on

the

on

disk

to

by

means

of

a

equalize the intensities

of the

colors

through the eye-piece, by lengthening

of the solution under examination. shortening the column The ment strength of solution being known, a comparative stateof depth of color in terms of the sucrose present may or

be made, to

an

with

or

the

reading

on

the

expression showing the the standard.

scale may

easily be reduced

depth of color

as

compared

SPECIAL

This

instrument

2

by

liter

per

heating it

is

pure

heat

portion half

of

char

hour,

an

color.

standard,

filter,

In

known

Comparable certain

conditions

The the volume Fill

of

certain take

depth

\vith

same

volume

the

cylinder, portion shows white

similar

and of

the

add

the same

depth

intensity

background.

proportional

to

The the

this

to

latter of

that

as

of

volume

decolorizing

color of

power

measured

a

described

above.

Nesslerizing,

a

burette

when

examined added the

to

a

solution; in

decolorized

of

in

determined,

the

water

of

experiments.

solution from

in

adopting

filtered

and

standard

the

of

all

Treat

in

used

decolorized

the

water

same

those

to

in

as

the

to

comparison. by

roughly

solution

standard-color

a

of

bone-black for

follows:

as

intensity

obtained

be

may

example,

bone-black

the

them

then

weighed

referred

color,

convenient

to

colorimeter,

a

cylinder,

a

power

for

standard

be

only

mine deter-

a

the

of

a

is

adhering

and

of

work

can

decolorizing absence

efficiency

capacity

results

with

determine of

all

solution,

time,

of

depth

sugar-house

decolorizing

bone-black,

length

the

the

represents

decolorizing. a

in

caramel until

C,

215"

solution

this

again

the

standard

the

of

and

difference

The

in

certain

a

about

mel, cara-

recommends

Prepare

examining

color

izing decolor-

with

prepared Duboscq

to

voliune

the

be

used.

In

of

depth

measured

a

should

cane-sugar

the

manner;

instrument.

decomposed.

the

determining

following

being

his

for

in

used

the

quantity

133

METHODS.

solution

definite

grams

of

in

char

a

standard-color a

be

may

of

power A

ANALYTICAL

a

similar until

a

solution over

is char.

inversely

a

SUGAR

CONTROL

CHEMICAL

SUGARS

ANALYSIS.

AND

OF

THE

CONSTITUENTS

OTHER

FACTORY.

OF

THE

CANE

AND

ITS

PRODUCTS.

Sugars.

60. the

of

sugars

Sucrose,

levulose,

the

showing of

classed

are

sugars

chemist

of

a

cane

are

sucrose,

those

chemical on

The

processes.

and

A

A

458.

few

of

the the

concern

in

given

are

table

physical properties

immediately

factory,

cane-sugar

of their

account

on

page

which

sugars

under

carbohydrates.

as

these.

chemists

manufacturing

given

of

reducing-sugars,

cane-sugar

chemically

is

other

importance

important

more

of

properties

of

are

carbohydrates

the

by

anal3rtical and

in

influence

work

important

most

possibly

them

glucose,"

name

and

with

usually grouped the

from

sugar

analytical

is the

cane-sugar,

and

"

the

in

of

levulose.

or

Dextrose

manufacture

importance

and

dextrose,

the

^In

"

the

following

paragraphs. Sucrose,

01.

sugar.

^This sugar

"

and

kingdom In

a

Saccharose,

in its pure

classification

derivatives

of

commercial sugar-

but

beet, the

been

the

United

Sucrose hemihedral

its

and

very

rich

are

belongs formula

in of

success,

sugar

the

to

is

though from

this

very

conunevce.

disaccharides, The the

sugar-cane,

The

palms.

from

of

vegetable

CijHjjOn.

rivaling the

sucrose,

made

annually

certain

sugar

the

are

cane-sugar

maple-tree, and

commercial

a

it

sugars

of

refined

is the

Cane-

or

in the

distributed

widely

state

hexoses,

manufacture

table-sirup of the

of the

sources

is often

cane

is very

Saccharon,

sorghum-

tropical

plant

cane,

has

not

large quantities

it, in nearly

all

of

parts

States.

crystallizes in anhydrous

the

monoclinic

transparent

system,

crystals.

The

forming specific 134

135

DEXTROSE. .

1710

gravity

crystalsat

the

readily soluble

is

crose

is

of

in water

and

to

it melts

ferments

on

in

It

light.

with

the

other the

to

lose

point

is

substances

has

the of

ray

a

is termed

right and

will be

shown

polariscopic apparatus

is also

is

for

distributed

in

in mixtures

CgHiaOe and

Dextrose

inverting

forms

rhombic

and

C,

the melt

readily soluble

is

with

it

belongs

always it and

sucrose,

the

crystalswhose

hydrate at

forms

80P-90"

in water

solubility in the latter varying with It rotates

widely

it is found

formula

on

crystals which is

fermentation

to

ent pres-

levu-

equal quantities.

144"-146"

Dextrose

of

hexoses.

and

dextrose

transparent

regard

by

promptly

sugar

is utilized, as

where

Its chemical

Anhydrous

is converted

but invert

the

to

^This sugar

"

sugar-cane, in formed

are

and

sugars.

monosaccharides,

in

of acids

plane of polarization of

construction

the

sugars.

action

other

many

property

vegetable kingdom,

the

The in

plane

This

Dextrose.

62*

poses decom-

sucrose

84.

information

rotates

analysis of

the

The

C.

sugar.

rotating the

in

100"

Moist

409.

dextrorotatory. (see 67),

C.

160"

given in

common

of

property

of

into invert

page

Sucrose

120"-125"

above

Further

given

of

be impurity, may C. without browning;

other

or

directly fermentable,

is not

ferments. is

is

sucrose

Sucrose

alcohol,ether, chloroform

raffinose

temperature

a

temperatures

on

many

of

temperature

a

at

at

salts

free

sucrose,

heated

It

glycerine.

anhydrous

Dry

Su-

alcohol.

in diluted

and

in absolute

practically insoluble

(Gerlach).

C. is 1.58046

prjs

melting crusts

or

C. in

and

its dilution

alcohol, the and

ture. tempera-

plane of polarization of light

to

the

right. The

chemical

of dextrose of to

absorbing lower

reduction of

are

dextrose,

methods based

of

upon

combined

oxides.

cupric

for

the

its property,

oxygen

The to

detection

and

reaction cuprous

reducing

oxid. 458.

estimation

in alkaline

utilized

refer to the table, page

and

For

in

solution,

metallic

oxides

analysis is

other

the

properties

136

Levulose.

63.

dextrose and

and

in sugar-cane.

sucrose

is a fruit-sugar. Levulose colorless, (keto-hexose); it forms

called

is often

usually associated with It is widely distributed,

is

^This sugar

"

fructose

or

monosaccharide, hexose shining, needlenshaped crystals of which

melt is

95"-105"

at

This CflHigOfl.

It rotates

the

is therefore

these

The

tals crysof levulose

formula in water

alcohol.

and

plane of polarizationof light to the left,and termed the cane laevorotatory. In mature

quantity of levulose is small Both

soluble

is very

sugar

system,

produce.

chemical

The

C

rhombic

the

difficult to

hygroscopic and

are

FACTORY.

THE

OF

CONTROL

CHEMICAL

often

are

sugars

compared with

as

in faint

only

present

the dextrose.

occasionallythe levulose is absent. Even though levulose be absent or present

traces,

and

quantity in the juice it always appears in defecation-process molasses. This is not entirely due to inversion and has

sucrose a

direct

low

inverted.

been

Such

polarization and

in

large proportion

increase

very

levulose

of

when

occur

may

molasses

a

small

in very

no

will often

high,

true

have

sucrose-

number. The

or

reappearance

action

A

Likewise rized

and

of alkaUs

part

and to

conditions

in

phenomenon

is due

heat

is converted levulose

the

the dextrose.

into

levulose. isome-

be

are

chemical

the

to

upon

may

There

into dextrose.

converted this

dextrose

similar

under

of levulose

salts of alkalis with

the

of

increase

ences refer-

many

and

technical

journals. It is direct

interestingto

polarization and

cane-molasses

differ but

Invert

64.

acids

note

and of

is said

Sugar.

certain

other

equal parts to

have

"

been

that according to de Haan

Clerget numbers

^

are

Verbal

used

When

carbonation

a

it is converted

reagents

and

hydrolized

synonymously

and

is acted

sucrose

of dextrose

commtinication

the

Uttle.

by

upon

into

a

The

levulose. inverted.

or

of sugars is called invert-sugar. The expressions "invert-sugar,"

"glucose"

of

*

The

ture mix-

sucrose

mixture

"reducing-sugars" and

in the

Archief, about

tories. cane-stigar labora-

1910

or

1911.

while

not

their appearance

during the

influences

products the

derivatives

of these

These as

of the and

mal abnor-

follows

:

same;

second^

firsts

fifthgaa-

esters;

,

compounds

numerous

ntuner-

of destructive

or

classified

roughly

A few

products.

eous

be

may

thirdfacids; fourth^alcohols

gums;

cane

yet

cane,

its

and

of manufacture.

process

closelyrelated

and

in the

result of fermentation

the

products, as

sugars

which,

a

are

occasionallymake ous

ucts.^ Prod-

Sugar-cane

of compounds large number occurring normally in the juice of the

There

"

of

Constituents

Abnormal

65.

137

CONSTITUENTS.

ABNORMAL

be

may

briefly mentioned:

CJEl^fi^f^^^

Mannose, have

CcHjjOq

been

of alkalies

action

cane-molasses lime

of

in been

has

perceptible

through

certain

fermentations

(CgHgOa) The

formation

of

wortliless

for

the

*

Report

gum,

have

levulose

in

Glycerol

been

such

of

polarization

gum

reported

prepared the

5th

it at

that

as

is of

by

in

canes

Browne,

La.

product

renders

a

the

the

author's

request.

Congress

p.

237,

vol.

31.

courtesy

of

The

ravages.

soon

through

the

by

occurrence

them

(+200),

serious

cane-productS| unless

International

Planter, 1905,

the

frequent insect

or

and

produced

introduces

sucrose,

of

is

common

high specific rotation

(65, 66) is included

who of

freezing

viscous

most

a

3. 383. "

excess

an

and

sugar-maker,

milling. Its that

article

Browne,

A.

this

times

This

in

occur

amounts.

(Froschlaich), and

injured by

canes

*

when

sirups.

(C^HgO^)

the

fermentations,

Leuconostoc

into

juices and

ketoP

of

enemy

various

three

They

in considerable

of dextrose

(C"Hi()05)n. This

troublesome

in

only

by^ the

Gums.

Dextran

of

produced

is formed

body

in small

molasses

fermented

cane-molasses

clarification.

This

Dimethyl

and

in

are

amounts

the

of

sugar-glucose

levulose.

and

reduction

the

amount

2d.

in

used

(C^Rifi^).

Mannite

in

dextrose

upon

'

Pellet

products

two

same.

non-fermentable

^^"

reported by

These

Egypt.

from

of the

closely related derivatives

and

Sugars

1st.

the

of

Applied

Dr.

error

gum

Charles

Chemistry,

is

138

CONTROL

CHEMICAL

OF

dextran, with

of

Hydrolysis

b^ alcohol.

first removed

FACTORY.

THE

acids,

gives dextrose. Levan.

A

found

gum

products in Australia This

formans. in

raw

sugar;

was

it

a

causes

produces the slimy A

Cellulan.

of

The

insoluble

giving

the

iodine), and

alkali

'

in

destructive

the

of

a

tions fermenta-

laige leathery dextran).

yields

cellulose

coloration

of

tanks

(distinctionfrom of

and

sucrose

in certain

consists

hydrolysis with

on

cane sugar-

a

boiling alkaH

reactions blue

in

specificrotation acids,yieldslevulose. has

Browne

with

and

cuprammonium

of

by

in caustic

all

rapid inversion

to

It is formed

treatment

on

very

sirup, and

cane-juice and

gum

and

found

gum

be

levan, with

in Louisiana.

sugar-house

lumps

of

Hydrolysis

of "40.

found

levan, which

gum,

Steel

and

produced by the Bac. levani-

and

organism

^

Smith

by

uct prod-

a

(solubilityin

with

zinc-chloride

acids is converted

into

dextrose. A

Mannan.

found

gum

deposits of fermented

juices and

acids, gives

with

mannan,

occasionallyin sirups.

Hydrolysis

substance, which

found speaking does not belong to the gums, was of hot-room in large quantities in the scums Louisiana.

is of

It

fungoid origin and

acid

hydrochloric

sedementary of

mannose.

(C1SH30N2O12?). This

Chitine

the

5^elds

strictly

by Browne

*

molasses

in

hydrolysis with

on

amine-sugar, glucose-amine

an

(C.H,jO.NH^. 3d.

Acids.

f

Formic, acetic,propionic,butyric, capric,and acids

of

fermentation-products to very

the

latter

lime

upon

through the Bac.

lactic

above,

common

The

all been

fatty series, have

of the

acid the

be

may sugars

agency

other

among

the

found

cane-juices and

sirups.

acid

mentioned

in

occurrence

various

should

juices, sirups, and

formed

of the

be

either

by the

In

tion addias

of

molasses. action

of

juice during clarification,or

of various

organisms,

Oideum

as

lactis,

lacticus, etc. '

^

^

International

a

La.

Planter,

"

"

"

Journal,

Su^ar 1905,

p.

238,

vol.

4, 430. 34.

"

140

CONTROL

CHEMICAL

OF

THE

FACTORY.

20.00%

Water.

20.00% Silica.

Si02

Potash.

0.60

K2O

50

3 .

CaO

Lime,

1

50 .

Magnesia^ Phosphoric

8.00

Ash.

MgO

0.

acid,

Sulphuric

acid,

10

0.20

PjOs SOg.

1

60 .

Chlorine, Soda,

a

0.40

iron,

NajO,

etc.,

Fe20sf 0.20

etc

1

62.00

fiusan

Sucrose

32

Dextrose

14

00 .

00 .

Levulose

16.

Albuminoids

00

0

30 .

Amids

asparagin)

(as

Amido

acids

0.30

)

aspartic

(as

1 .

bodies.

Nitrogenous

Nitric

3.00

.

70 .

acid

I6

0 .

(Tot8lN-0.6%).

Ammonia

0.02

Xanthin

bodies

0

30 .

Other

nitrogenous

bodies.

0.23 .

Soluble

( Xvlan

2.00

gums

,

acids

Combined

3.00

Glutinic,

charinic

(

acids,

Molasses

also

contains

00 .

Sac5

etc.

100.00%

TotaL

2

.

,

j Melassinic,

2.00

acids

Free

)

Pectin.etc

Araban

00

100.00%

small

a

of

quantity

carmelization

"

the

product, of

by

1

cane-sugar

bodies

of

uncertain

Caramelen,

Caramelan,

Zuckerarten,

and

evaporation

overheating

colored

of

amount

3d

ed.,

1210.

depending

these

Caramel

boiling.^ and

is

mixture

a

the

upon

is of

ture tempera-

always

formed

several

dark-

composition.

Caramelin,

tee

von

Lippmann,

Ch"unie

der

OPTICAL

METHODS

APPARATUS

The

67.

AND

Polariscope.

**

and

called

saocharimeter"

Sucrose, in has

the

ray

of

passing

it into

rhombohedron The

spar. so

that

the

into

obtuse and

of the

two

is

18.

Confining the

cane-sugar

our

Iceland

is then

prism B,

a

ground ofif

are

through

surfaces

the

polished

are

passes

upon

whose

the

instrument

of

into

from an

balsam.

an

the

Other this

but

present

ray

a

separated

chemist,

and

used,

are

passing

remarks

The

A

the

from

crystal of

68".

for the

ceinent,and

Fio.

prism is made

Canada

prism

reflected

which

by

together again, in their original

answer

it is

light is accomplished

property

prism, Fig 18,

angles and

the

On

the

parts,

positions, with will

a

in

each

are

cemented

of

othei'substances,

this

transparent

a

angles

cut

of

This

prism.

surfaces

acute

and

plane of polarization of

of

ray

from

cut

end

is

polariscope.

Nicol

a

the

used

sugars

is taken

polarization of the

The

in

polarimeter'*

names

sometimes

rotating the

of the

'*

The

many

light. Advantage

used

optical methods

by the

also

with of

instrument

sugars

are

common

property

construction

The

polariscope.

a

ANALYSIS.

MANIPULATIONS.

"

of

quantitative estimation usually

SUGAR

IN

purposes.

ordinary prism by

extraordinary

or

it

prism

this

which

ray,

the

balsam

polarized

polariscope

the

properties the to

description

light into

through

forms

ray,

and

construction

of

depends. three should

sugars be

of most noted

interest that 141

sucrose

to

142

ANALYSIS.

SUGAR

IN

METHODS

OPTICAL

fore polarizationto the right and is thereThe termed rotatory a right-hand sugar. expresdons dextroand also applied to sucrose. dextrogyratoiy are also rotates the plane to the right. Levulose Dextrose

rotates

the

plane

of

rotates

the

plane

to

hand and

the

left and

Quartz is of

sugar.

is used

due

of a sugar to power differs for different sugars. certain

under

left-

left hand,

kinds, right and

two

a

to sugar.

The

determined

or laevorotatory,

types of polariscopesto compensate

in certain

for the rotation

is

rotate

the

The

number

plane

of

polarization

expressing this, as conditions,is termed the

standard

specificrotatory power. is

passed through sugar solutions of of the solution different concentrations, or through columns If the

polarizedray

of different

rotation

will be

lengths,it with

varies

observed

strength of

the

that the

the

of

amount

solution

and

the

length of the column. These

properties'of

utilized in the them

construction

the

view

in

instruments,

as

transition

of the

given farther be divided

on,

the

and

quartz

The

are

keeping

various

will be

into two

tint-instruments.

types of stood. readily under-

classes,viz.,shadow shadow-instruments

polariscopes using white light,as from a kerosene-lamp, and those requiring a monochromatic The former usually employed are light, the yellow ray. and the latter in scientific investigawork in commercial tions. may

A will

be

subdivided

spar,

polariscope,and

descriptionsof

Polariscopesmay and

Iceland

sugars,

into

description of the polariscopes in general use will be given in the following paragraphs and

brief be

sufficient referred

for

the

hand-books

to

of

purposes

of

descriptions of the

the

this book.

polariscope for

theory and

reader

The

tailed de-

more

construction

is

of

the

instruments.

Polariscope. Compensating ment ^The optical parts of this instru(Schmidt " Haensch). The in indicated in Fig. 19. polariscope shown are 68.

Half

-

shadow

"

the

figureis of the singlecompensation type. modified At 0 there is *aslightly Jellet-Corny Nicol prism,

COMPENSATING

HALF-SHADOW

at

(r

is

wedge

plate ot levorotatory quartz,

a

movable

by

quarts-wedge, vernier.

The

rotation an

is

of

fixed

in

scale

upon

E

quartz-wedge

has

the

of

means

plane

cane-sugar.

for

These

M,

screw

to

wliich

which

to

note

moved,

work,

quartz-wedges

is

and

a

quartz-

at

the to are

P

is

a

attached

the

the

distance

the

in compensating

is attached

technical

"

is

polarization due

of

optically active body,

graduated,

the

at

position,

t"een

143

FOLABISCOPE.

to

wedge.

read of

for

the

interpoaing The

percentages

scale of

dextrorotatoiy

144

The latuB, of

parte G, E, and i.e., that

observation-tube,

observing

the

right

are

lamp

in

field, and

for

K

lines

the

is placed

of

is

the in

reflector extreme

from

light

prism,

the

used

the

at

in

H

telescope and

Nicol

the

At

be

to

telescope

rays

plane

Hubstance

lenses

two

the

to

the

appa-

the

of

figure.

is

are

transmitting

parallel

the 7

The

scale.

The

solvent,

in

at

deviation

the

above.

at

compensating

the

suitable

a

prism;

the

reading

for

shown

as

Mirol

a

for

in

ANALYSIS.

BUGAR

constitute

explained

as

dissolved

analyzer,

F

compenaates

polarization,

examined,

IN

METHODS

OPTICAL

the the

forming

polariaer.

The

described

instrument A

type.

in

having

of the

The the

and

neutral

of the

is

a

in

uniformly

right other

left, one-half

or

and

the

the

compensating

light.

It

wedges

of

scribed de-

opposite

The

arrango-

23.

shaded

Of

shown

already

instruments,

controlling the compensating

the

that

verniers.

Fig,

above

is

wedges

quartz

scales and

is shown

wedges

point,

of

sets

two

field of vision

screw, to

two

tion angle-compensa-

instrument

differs from

polariscope

optical properties ment

is of the

double-compensating

This

in Fig. 20.

above

the

is from

this

that

this

disk

be

set

If the

disk.

wedge,

when

at

milled

slightly turned will

half-shaded

in^rument

be

shaded

disk takes

and its

HALF-SHADOW

FOLABISCOPE

GLASS

WITH

double-compensating instrument

A

is shown

in

145

SCALES.

construction

of recent

The

optical parts of this instrument are by the cap (7, and h"y plain exposure gla,ss plates. This protectionof the opticalparts is especially peculiar important in the tropics,where, owing to some with an climatic condition, the lenses often become coated opalescent film that can only be removed by polishing. These spiders and other insects plates also prevent minute in the tropics from The scale damaging the instrument. is lighted from the lamp, the lightbeing reflected by means of a prism and mirrors. Th^e telescope F is focused by a The screws for adjusting the position of the quartz screw. Fig. 20. protected from

.

have

wedges

long

stems

upon

table.

of the

observer

glass cell filled with a three of potassium is placed at B per cent solution of bichromate and serves ray-filtershould always be as a ray-filter.^This quirements used, varying the strength of the solution to suit the rein hand. The of the work prism at P is more readily accessible than in the older instruments, and all and other lenses optical parts are protected by glass An is the substitution important improvement covers. substantial stand of a very for the ordinary tripod support. rest

may

the

the hand

that

so

Half-shadow

69.

A

Glass

with

Polariscope

Scales

shown in Fig. 21 has Fri6). ^The instrument double-wedge compensation for use with white light. The for protection optical parts are enclosed in a metal case

(Josef-Jan

dust.

from

and

"

are

The

scales and

lighted by

verniers

engraved on glass are part of the polarized rays which

a

reflected upon them. Fri6 also make Messrs.

are

quartz-wedge polariscopewith of adjustable sensibility,designed for the U. S. Bureau Standards This instrument is double by Frederick J. Bates. ^

This

cell

strength of solution

lengths, the

of^the

ray a

white

100"

and

Z. Ver.

be

filter makes

assumes

of

product

should

solution

9. a

Deut.

the

length

difference

it 100.12".

Zuckerind.,

cell 3

a

According With

light instrument. without

a

1904,

the

in

filter he

(Circular

No.

521-558.)

For

the

the

other

streaa.sth

percentage

Schonrock

of 0.12"

the

pp.

by to

in length.

cm.

use

of

a

chromate bi-

polarization w"th

obtained

44, Bureau

a

'

reading

of

of Standards;

146

OPTICAL

METHODS

IN

quartz-wedge compengating Readings

Byetetn. The

Frifi inBtrumenta

Gcation

of the

the normal

weight

Fig.

principle

to

and

ANALTSIS.

baa

a

to

according

Commission

with

Lippich polorizingmade

accurately

graduated

of 26 grams

at

the 100

20"

0.01" to

sugar.

the G.

apeci-

and

true cubic

use

meter centi-

C.

Polarfscope

Hall-shadow

instrument.

are

International

flask at 20" 70.

be

may

SUQAB

22, is

the

(Julius Peters). "

double-compensating.

other

compensation

This

It is sinulor

in

polariscopes. The

r 148

OPTICAL

According and

is

to

IN

METHODS

Wiley

this inatniment

'

72.

Laurent

19

constructed

only

use

are

ecopes are

with

now

also white

(Maison

Polariscope

(Fig, 25)

Laurent

uae

extremely

eensitive with

the

for the

careful scientificresearches.

very

and

ia

capable of results but tittle inferior to those

which Landolt-Lippich polaiiscope,

for

ANALTSIiS.

BUQAR

with

originallya half-shadow

was

a

monochromatic

made

with

provided

with

either a

light, but half-shadow

Aaiiculturid Analysis, -1. HI.

The

inBtrument these polari-

or

triplefield,

compensation attachment

light. "

Laurent),"

for

LAURENT

In

the

Laurent

for

compensate of

plane measured

by

vernier.

The

rotation

of

of

means

As

read

for

which

the

to

the

also

and

has

a

the

is

the

compensating polariscope,

a

Laurent

be

may

of

screw,

directly.

stated, there

device

milled

a

cane-sugar percentages of sugar

which

be

may

of

scale

a

instrument

scale, called

scale, on

end

means

polarization by the sugar The is angular rotation

solution.

second

the

by

light,

monochromatic

polariscope,using

analyzer is revolved

the

149

POLARISCOPE;.

attached

instrument,

Fig. 2Q, and

the

to

shown

as

permits the

front in

of white

use

light. A

distinctive

scope

of

of this

polariis the adjustable polarizer. The

prism

Nicol a

feature

through

angle,thus varying the

small

light that

and

passes,

glass, half

is

is

strument. in-

passed

covered

Ito.24.

through

with

disk

a

thin

a

half-shadow

the

producing

thus

quartz,

which

of

same

the

of

polarized light

The

amount

the

at

sensitiveness

the

time

be rotated

may

of

plate of

feature

of

the

instrument.

type of polariscopeis much

This *

since

it has

no

quartz wedges

used be

to

in scientific

affected

research,

by variations

of temperature.

Transition-ttnt

73.

Scheibler.

^This

scribed that deinstrument, Fig. 27, resembles in general appearance, but actually differs

"

in 68

radically from

it.

in

having

an

which

produce the

plate B varied

by the

by rod

L.

It

The the

differs from

additional

of

means

polariscopeare half-shadow

Soleil-Ventzke-

Polariscope.

the

Nicol

color.

the

half-shadow at A

prism The

instrument.

as

those

a

tint of the

spur-wheel and optical parts at the

same

and

ment instru-

quartz field is

pinion, revolved front

in the Schmidt

end "

of the

Haensch

150

The

point the

eyes

revolving 74. scopea

is the

Remarks

general

are

The

Laurent

in France ments

in

countries.

and

The

tint for

varied

be

may

Polariscopes.

upon in

construction

by-

type

of

Belgium, work

is

very

necessity of

the

except but a

the

is

typies

room

ally gener-

reliable.

extensively

higher-grade

little used

dark

most

are

sensitive and

saccharifneter and

to

Polari-

"

of construction.

in detwls

polariscopes are

research

tint

is set at the

eensitive

triple-fieldinstruments

and

These

The

The

aimilar

described, differing only used.

instnuneDt

the

L.

rod

Half-shadow

ANALYSE.

is unifonn.

rose-violet.

a

General in

tint

aUGAB

when

field ia colored, and

neutral

most

IN

UETH0D8

OPTICAL

and

outside a

used

instruthose

monochn"-

GENERAL

BBMARKS

light render

matic

tor

factoiy The

in the

use

for

modified

the

with

use

UPON

originalLaurent polariscope u industry. The Laurent cane-sugar

white

light is

ion-tint instrumenta

trauHit

exclusively, especially in

the

or

be

cannot

less color-blind, and

All 200

polariscopes

with

half-length

a

lengths A

400

are

analysis of dark-colored

to

solutions

milling

the

fiOO-mm.

75.

The

Normal either

will be

materials

that

dear

are

COO

of this size is also supplied tube.

Other

polariscope

nun. a

satisfactorylength (or

but

process,

observation-tubes

tlie diffusion

with

a

factory

process

the

Scale.

Polarlscoplc

Veatzke

Polariscope scales

"

instruments

usually

divided

are

liave

only

the

The to

of cane-sugar

percentages

or

Scale.

read

oii.both. Ventzke

or

scale.

Ventzke

weight

solution

under

receive

to

100-mm.

and

circular degrees

cane-sugar

certain

more

preferable.

Weight.

Commercial

The

is

"ze

persons

,

fitted

or

mm.

by

accuracy

secure

polariscope is

400-mm.

using

the

in the

instrument

an

been

polariscopes. Tint instruments, with

are

long, and

mm.

almost

have

States, but

for observations.

enough

used

formerly

were

used

frequently difficult

it is

instrument.

convenient

a

United

largely replaced by shadow obviously,

151

POLARI8COP"B.

cane-sugar

of

the

diluted

standard in

or

to

material

of

be

cubic

100

conditions

percentages

scale is

in can

a

so

divided

dissolved centimeters

200-nim.

tliat,if

in water and

tube, the

a

and

observed

reading

152

OPTICAL

METHODS

used, the reading these "

conditiona

normal

to

weight"

^lommercial

the

will

divudoDs

of

be

100.

the

"

The

weight required under of the

the

instrument.

In

polariaation of

the

scale

cane^migar

is termed

readings

factor"

eepecially in

the

ANALYSIS.

BUQAB

give percentage or

work,

IN

are

sugars.

usually tenned

"degreea." nonnal

The are

very

the grams.

weight

generally

International The

used

for

throughout

Congress

flask used

German

the

with

of this

the

instruments, which world,

Applied normal

as

adopted b;

Chemistry, weight

must

is

26

hold

MANIPULATION

100

cubic

true

20" C. to The

is 26.048 Mohr's

100

cubic

and

100

be

cubic

true

at this

centimeters

of

Manipulation

dissolved

clarified the

and

fillan polarized, solution and place it

is to

Mohr*s

be

units

observed

the

The

light from

observer

at

geneially

dissolved

in

80)

of

'see

at

17i" C.

20" C.

and

be

observed

is not

his eye

if not, the

The

with

a

material

portionof

and

of the

or

ing deeply colored, accord-

more

should be

the

or

than polariscope,

should

telescope/

small

the

the

other, provided the

point. The be

vertical line

shaiply defined,

backwards

moved

and

forwards

or

sharp focus is obtained. observer the

moves

Having

weight of the

at the

set at the neutral

ocular

in 80.

of

corresponding part Peters polariscopeswill notice that

half -disks

separating the

Methods

"

trough of the instrument, suitable lamp through it.

Figs. 19, 20, 23, 27,

the type of

a

normal

of the disk is shaded

instrument

Polarlscope.

a

in the

Laurent, Fric,and

one-half to

a

with

in

instruments of the

at

observation-tube

to be

should

the

field appears the scale as directed

until

read

the

making the observation of the

turn

now

quartz-wedge compensator,

Laurent,

tinted, then

to

stillmost

one

will be -described

solutions

axis

or

prepared and

preparing the

In

made

temperature.

76.

the

be

is 16.29 instrument weight fcr the Laurent of material, which should be dissolved diluted and

grams

until

observation

tion solu-

The

normal

The

pass

20" C.

at

the material

centimeters

is to

solution,and

the

weight and the

grams

153

FOLARISCOPE.

results.

correct

secure

A

of solution

prepared and

originalnormal

used

to

centimeters

be

must

OF

instrument, and

milled

analyzer of or uniformly shaded or

the

in page 154. should be in the

the eye should not

which

screw,

be moved

optical

from

side

side. A

little

practicewill

enable

the

operator

to

detect

very

tint and or depth of the shadow in this manipulation. to attain great accuracy The polariscope is as manipulation of the triple-field described above, except that the field is in three sections,

slight differences

in the

in shading it uniformly. giving greater facility The double compensating polariscopesare providedwith

164

OPTICAL

METHODS

IN

SUGAR

two

scales,in the older instruments,

and

the other

the red scale is set at

work

the black

with

Since

red

the

and

screw

the

abandonment

check

readingsshould To

make

equalized

of their ivory scales on account certain atmospheric conditions,metal marked

are

to

indicate

whether

at

the the

the

direct

the

scale,the

same

instruments

Laurent

dark-colored

time

same

the

invert

and

single-

readings

graduationsextending

This

solutions.

with

fitted

are

small

a

A

in

both

device

for

varying

polarizingvery

in

slightchange or

a

angle, thus

is convenient

adjusting lever will increase

lightthat

With

zero.

sensitiveness.

the

readingsshould

algebraicsign minus.

rotatingthe polarizerthrough the

readings. Both

The

scale used.

other

instruments

compensating sides of the

used

screw

ize equal-

or reading,i.e.,one with a Isevorotatory the black, or right-hand, scale should be

with

on

for invert

and

invert

and

be recorded

The

the

sugar,

zero

made

the observation-tube

agree.

an

left-hand

of

the field is

and

zero

nary ordi-

For

one.

of

the scale,remove

the field with

are

by the brass

operated

right or left readings.

To

set

scale is

black

screw.

length changing with scales are usuallyused, and for

graduated in black

one

The

frequently in red.

by the black

ANALYSIS.

the

decrease

position of the

amount

through the instrument, though at the of increasing or decreasing the sensitiveness passes

polariscope. Having equalizedthe

the

described, the the

scale is to

scale is best

shown

field of the read.

be

by

an

polariscope as The

method

example.

Let

of the

already reading position

.11 i 1 11

Fio.

of the

scale and

of the vernier lower

number

vernier

is between and

note

be

28.

shown

in

The Fig. 28. zero 30 and 31 of the scale; record the line on the point at which the a as

156

OPTICAL

It is

METHODS

quite essential the

to

respect

light should

be

suitable

Landolt

of

that

as

by

to it

has

should

Bunsen

the

for monochromatic

light,and

provide

to

Laurent

Laurent

of

type

gas-sodium,

eo'ipyle,the requirea flame

Laurent

lamps

last such

yellow color is imparted

the

sodium

chloride.

M.

soduim

salts for

finds that

sodium

various

experimented with

changed, the i

the

the

are

These

fused

if

factoryconditions

burner, and

with

contact

The

light for

gas-sodium, and

a

light with intensity of the

be verified.

the usual

burning alcohol.

named

position of the

possible,and

lamps used

The

ANALYSIS.

fixed.

as

monochromatic

instruments. the

the

constant

as

It is difficult under a

that

SUGAR

polariscope be

reading observation

zero

IN

F.

*

Dupont in

use

lamps

chloride

and

fused together in molecular phosphate of sodium proportions give results in every way superiorto those with sodium chloride only. The of the scale Polariscope. 78. Adjustment tribasic

"

only part liable to get out of adjustment. this adjustment, place a polariscope tube is the

of the instrument To filled with

test

in the

water

trough of the instrument observation

This

an

observation.

the

tube, but

the

adjustment

with

the

water.

made the

as

reading

The

vernier with

but

by

by

used

of

means

distance.

short water

scale

and

scale is

for all of their

in the

vernier

without

readily

so

properly adjusted

a

"

Haensch

compensating

other

key,

makers.

A

The

coincide

micrometer-

is

observation-tube, and until the

with

another.

one

the

zero

ments instru-

polariscopes

arranged to field is equalized

by the micrometer-screw

moved

do

a

If the

is not

zero

adjusting the Schmidt

same

turned

screw,

the

on

made

make

zero.

is similar to that

and

and

of

method is the

now

be

should

be

may

and

the

move

usual,

as

vernier

lines of the The

scale

through several degrees by the milled the field is again equalized as before,and if the zero moved

not

coincide

manipulations successive

^Bulletia

the are

vernier

be

is to

again adjusted.

repeated until the

observations.

de 1'Association

These

des

zeros

is

coincide

adjustments

ChimiBtes, 14, 1041.

screw

lines These

in are

is

eral sev-

very

I ADJUSTMENT

fatiguingto

the

OF

which

eye,

1^7

POLARI8COPE.

A

should

rested

be

short time

a

making the final observations. Certain compensating polariscopes, of the older especially models, are exceedinglysensitive to changes in the position of light. It is advisable to follow or intensityof the source directions as to the positionof the lamp with the maker's regard to the instrument and arrange the latter so that it be jarred out of place. The distance of the lamp cannot from the instrument is usually 15 to 20 cm. The position the lamp should occupy should also be marked, that it may be properly replaced after refilling, and the intensityof the light should not be changed after adjustingthe instrument until the observation A change in the has been made. position or intensityof the light,with certain instruments, before

will sometimes In

adjusting the

of 0.5"

error

an

is next

focused

field into halves; the of the

means

zeros

the

zero,

to

are

The

G.

screw

more.

the upper limit,the ocular vertical line which divides the

the

on

or

polariscopesto read

Laurent

U, Figs.25, 26, is lifted

lever O

cause

made

now

field should

now

coincide

to

be

by uniformly

adjustment,and if not uniform, The adjustment should be F. equalize it with the screw factory. tested as with the other instruments, and repeateduntil satisshaded, ifthe instrument

is in

It is advisable to have

for checking quartz control-plates

of the adjustment of the instrument and the correctness scale. Standardized platesof the highest accuracy may be obtained from the makers and in use take of polariscopes, solution and a standard the place of the observation-tube of pure sucrose. One plate should read approximately96" the

and

a

second

in the most

about

these

60", as

parts of the scale control-tube

scale may be tested with a Schmidt " Haenschi and shown in control-tube

is filled with

flows into the tube screw.

The

as

it is

Fig. 29. a

sugar

The

of the

Applied Chemistry

by

funnel

T

lengthened by turning the milled

tube

committee

made

solution, which

length is read on the scale N. describes this apparatus. sufiiciently The

used

important polarizations.

The

of the

are

Fourth

also recommends

The

tration illus-

International Congress of the

use

of pure

cane-

168

Bugftr for

IN

METHODa

OPTICAL

ANALYSIS.

BUGAB

The

testing the polariacope.

of

method

preparing

this sugar and precautions in using it are described in 393. The micromeler-acrew at H, Figa. 19, 20, 23, 27, is for the

adjustment be

of the analyzer, should

unevenly shaded The

analyzer and be

should All

adjusted except

or

the

m

event

returned of

parts

especially the

the

at

set

the

to

of the

are

the

by

dealer

exposed

parts

Observation

shown

in Fig. 30.

repairs.

lower

the

be

*"

has

tube

(fm

feM^^^

'tmf

\J^

old linen

of

glass and

screw-eaps is

slip-cap undue

prevent

designed pressure

cover-glass. The

"Pon

the

tubes

of the French

instrument

^

have

catchea.

arranged

inside

FiQ.

and

30.

upon

hold

the

must

be made

are

used

in many

of the expansion

careful work, especially if the

spring ia

the

cap

to

cover-giaaa

it in position, without

unnecessary

observation-tubes

with

bayonet-

coiled

A

bear

Laurent

supplied

are

slip-caps that

Account

be

should

j-"

__^

Metal

dean

very

tubes

usual

slip-cap. The

Landolt

kept

wiped with

and

upper

man, work-

polariscope it

lenses; these

the

Tubes.~The The

the

to

polariscope should of

from

removed

experienced

an

for

polariacope

pomt.

be

not

accident

an

occasionallycleanaed with alcohol

79.

neutrel

polarizer should

and

instrument

the

when

the field of the

pressure.

laboratories.

of the metal

laboratory temperature

in very fluctu-

OBSERVATION

tubes

greatly. Metal

ates

handling and

careless

of silver

sometimes

are

liable to distortion

are

or

gold

plated with

are

through tubes

These

acids.

with

corrosion

to

15Q

TUBES.

to

prevent

corrosion. Tubes

of the tjrpe shown

be

Fig. 30, must illustration, the solution to be polarized. The in the

completely filled with cover-glassshould be slipped sidewise onto the tube, pushing off the surplus liquid. The glass body of the filled tube should will with the hands, since the warmth not be touched striations

cause

immediate should

observation.

be left in the

clears. Observation in

form

to

Tube

trough of the with

of

Enlarged End.

^This tube

"

upper

obviates

the

for

room

part of the

field

is shown

a

small

to

for

This

of rangement ar-

severe

this Bureau

usage,

the

overcome

prevalent defects in the theoretical design, as well suitable

the

bubble

enlargement.

order

"

tube

tube

necessity of excluding air-bubbles,

the tube. and facilitates filling Baies^ Observation Tvbe.^ "In

a

an

31.

polarized,leaving

rises to

air, which

prevent

the striations, polariscopeuntil the

the event

In

FiQ.

solution to be

liquid. These

using this tube, it is nearly filled with

In

Fig. 31.

in the

as

secure

(U. S. Bureau

wssssam

Fia.

Standards) has brought

of

in

shown carried

1

upon

Copied

ardsr

p.

Fig.

39.

from

It will be

32.

two

out

32.

the

observed

shoulders, which

Circular

No.

44,

"

new

are

Polarimetry,"

Bates that

type of tube the

weight is

integral parts of the U.

S. Bureau

of Stand'

160

OPTICAL

and

tube

not

METHODS

IN

ANALYSIS.

thereby eliminatingall danger

the caps,

upon

SUGAR

The turning while in the trough of the instrument. bore is 9 mm., permitting the utilization of the full aperture of the polarizingsystem. This also reduces to a minimum the light depolarized by reflection from the walls of the tube. from

The a

field of the instrument

thus

bright, sharply defined

and

the

ends

are

circle with

Both

accuracy.

advantages, yet

33.

size of

is required. The cover-glass and washer unusually heavy, eliminating all danger from

one

walls

as

overlying haziness,

no

reading can be made with increased enlarged with all the attendant

Fig.

but

for the first time

appears

are

bending." Observation

Fig.

33

Tube

is very

with

Side

convenient

Tvbvle.

in

The

"

rarely be removed. the risk of error by compression

Fia.

tubes

The

should

be

in

general sugar-analysis. The

cover-glasses need reduces

shown

tube

This of the

arrangement

cover-glasses.

34.

frequently cleaned

with

diluted

acetic

acid. Tube,

Pellet's Continuous for very

of

material

raw

tube

This

tube, Fig. 34, is designed is especiallyadapted to the

rapid polarizationand

of laboratories

use

"

on

for beet-seed a

basis

is also convenient

selection

of its sucrose

in the

control

and

content.

of the

the

purchase

The

Pellet

char-filters in

sugar-refineries. The without

Pellet tube

removing

provides it from

for the

the

rapid change of solutions trough of the polariscopa.

OBSERVATION

The

is

tube

arranged that it

so

connecting rubber, tubing the syphon terminates in

by of into

the

opened.

then

solution.'

The

This

scientific

in

and used

in its

to wash

Pellet

before

short

leg which is dipped the long leg is previous

used

tions only with solupolarization and not when

desired.

be

The

be used

funnel when

arrangement is

accuracy

quantities of the solution

sary, neces-

should

the funnel. should

tube

be

period of idleness

a

The

syphon

a

hquid displaces the

same

Uberal

use

tubules.

glass tube pinch-cock on should

35 should

Fig.

the

part of

a

a

a

arrangement is

form

may

to

incoming

accuracy

illustrated

The

and

approximately the

of

be

solution

new

161

TUBES.

washed

and

with

distilled water

be

left filled with

should

water.

The

descriptions of this tube

first of the

hands

made

were

These the

author

before

experiments

construction

secure

a

were

very a

of the

tube

for immediate

tube

with

made

a

into

came

several

and

meager,

satisfactorytube

not

were

that

the

ments experi-

constructed.

was

view

to

improving

designed by Pellet, but to The tube finallyadopted

as use.

in Fig 35 and differs from Pellet's by the writer the solution to distribute design only in having four grooves is shown

instead annular each

of

The

one.

canal,

of the four

solution

funnel

which

shown

end tube the

a

of the tube to the

at

against the

FiG.

glass,and by

by

connects

grooves

is delivered

directs

displaced

inner

and

solution

waste-jar. The observation

|)revioussolution

is

end

The

of the tube.

surface

of the

canal at the flows

cover-

the field will not

opposite

through

a

So

long

bent until

be made

cannot

entirelydisplaced.

of the old solution remains

an

openings wilh

separate

the

into

36.

similar set of grooves the

solution

the

as

be clear.

any

162

METHODS

OPTICAL

The

Pellet

tube

in the

accuracy

with

IN

the

SUGAR

ANALYSIS.

funnel-inlet

analysis of

may

The

sugars.

be

funnel

used

with

should

be

shown in Fig. 35. An preferably of the form improvement to the funnel would be an overflow attachment solution. to facilitate the washing with the new The author has proposed substituting a grooved tube, such as a rifle-barrel, The swirlingmotion for the plain tube. would imparted to the solution by the rifling probably promote the removal of the previous solution, especially in

small

and

Experiments made

testing sugars.

FiG.

FiQ.

with

vided

a

with

a

Pellet

tube, pro-

38.

37.

glassbody, indicated

the

of desirability

the

grooves.

Tube; Wiley^s Modification, ^This tube. Fig. 36, is arranged for the control of the temperature of the solution under observation, especiallyin the Clerget LandoWs

Irwersion

method. double-polarization

"

The

glass observation

tube

is

is circulated jacket through which water while polarizing. A side tubule, enlarged to funnel shape, the tube and in taking the temis provided for use in filling perature A solution. of the centigrade thermometer ^aduenclosed

ated

to

Wiley

in

a

metal

fifths of devised

a

degree should be used. the desiccator-caps shown

in

Fig.

37

to

164

OPTICAL

METHODS

IN

SUGAR

given only approximatelyon

be

in the

materials

themselves

ANALYSIS.

account in the

and

of the

variations

illumination

of the

polariscope. In general the minimum quantity of the leadsalt that will yield a clear and sufficiently tion light-coloredsolushould

be

used. into

errors

refer to cubic per

sirup,7 control),5 to 10 80

cc; 6

analysis. The of the lead

introduces

cc; raw

solution

of 54.3?

98"

6

sugar,

7

to

cc;

Brix

juice, 1.5

Raw

of 20" Brix

2 to 4 cc;

sugar,

portant im-

following numbers to

(vacuum-pan final molasses,

first molasses,7 to 10 cc;

second

89"

molasses

to 10 cc;

96"

to

of lead

use

weight of the material:

.2.5 cc;

25 to 30 cc;

the

centimeters

normal

one

Excessive

raw

1 to 2

sugar,

filter

press-cake,

often

replace the

page

179.)

cc

Home's solution

of the

salt with

1.25 100 .

cc.

of lead may

dry subacetate

of

advantagp. (See

1.5 grams juiceand a like

raw

the sugars consulted.

and

Alumina-cream of lead

of the

to

Paragraphs 83, 84, relative

upon

very

be

required

proportion for other

per

materials.

to the influence of the lead-salt

the volume

should

salt is

proximatel Ap-

of the

used

precipitatesshould

in addition

the

to

be

tate subace-

in

clarifyingthe solution in testing a sugar. The alumina-cream alone is usually sufficient in the analysis of high-grade sugars. It is

usually advisable to add a little of the lead reagent to the sugar solution,mix thoroughly, await the subsidence of the precipitateand then test the supernatant liquid with whether lead is reto ascertain a drop of the reagent more quired. An the experienced operator can readily judge by of the

precipitatewhether the lead has been used in sufficient quantity. The in reagent should be measured appearance

routine should The

always

be used

materials

weighed in

in

and

work

a

in

nickel

or

far

so

with

as

is

possiblethe

same

quantity

similar materials.

analysis

sugar

German-silver

conveniently capsule,made especially are

most

for this purpose. (Fig. 38.) The solutions do not adhere to the polished surfaces of the capsule and the shape of this

is such

that

the fiask. The

the

The

material

may

be

very

readily washed

capsules lose weight graduallythrough

counterpoiseshould

not

be filed to correct

for this

into use.

loss,

SPECIAL

the stem

but

be removed

SUGAB

165

APPARATUS.

plug should be unscrewed

or

ajod sufficietitlead

the

cavity to compensate. If the sugar-flaskhas a narrow neck, as is prescribed in careful work, it requires skill to wash other material or sugar into it. This operation is facilitated by insertingthe ste.ii of

from

German-Silver

small

a

of the flask.

into

the neck

the

neck, thus

should

be

must

left in

the

flask

reach

from the

just below

to

with

capsule and

about

"

purpose,

contact

jetof

a

the

for

should

into the flask with

be washed

room

This

keeping the sugar solution adhering to

The

latter.

funnel, made

cc.

funnel

Sufficient

water.

20

the

permit

to

"

liquida rotary motion, The flask should be held by its neck to prevent the hand time to time it should From from warming the solution. the

giving

for

be examined

below

from

to note

Fio.

remains. with should

subacetate

drops of

adhere

water

absorbed

with

preparing

the

free of

water

The

be

centimeters

and

its clarification

described, the with

mark

should

be

volume Should

water.

flas"they should

of the

either

The

funnel

The

the

be

be

used

water

distilled

in

other

or

thoroughly mixed

poured immediately

suitable of paper fluted or '^star'^ folded

flask.

above

been

to the neck

especiallyin analyzing of the

38.

of the flask should

filter should

used.

the

material

opticallyactive substances. be

be

to

solutions

shaking and be

undissolved

strips of filter-paper.The

contents

should

has

as

completed

be

whether

solution of the material

After

lead

dissolvingthe material.

and

paper

sugars,

filter should

edges of the

of the

should

ribbed

should

to receive

be

funnel.

filtrate should

and filtering-cylinder

a

never

then

filter.

The

and rapid filtrations,

for or

the

upon

by

be

so

large enough,

large

as

first few

to project

cubic

rinsing the rejected. If the

used be

should

the entire contents

The

be

funnel

in

166

filtrate should

is not

this

filter,but

the

be bright and

not

is Eilnays

preferable

requiring

considerable

filtrate until it is best

to

except

littie common tion

be

may

used.

be

pint

If

Fig.

Steniless

tin-^late or

makes

thin

a

C

and

by

a

funnels, of

so,

is

A

39.

precipiUting-jar,

the funnel

advantage

little of

a

with of

a

by refiltra-

salt and

kieselguhr

due

be

Home's

dry

to sub-

stemless a

4

inches

the

glass precipitating-jars or

funnel,

small

closer joint with

copper,

of

filteringarrangement

in

a

the

to

ia

quarterA

plain

Up-cylinder,

the edge. made

diameter,

planished,

metal

B

cyUnder.

chemists

many

except for invert solutions,than The

tempted at-

addition

followed

the

both

convenient

A

"

cylinder is preferred as

be

never

of

added.

F'OieTing Devicet. in

quantity

Occasionally the difficultymay

should

illustrated

the

The

cane.

phosphate

this,or

subacetate.

insufficient acetate

sodium

or

remedy

will often

cle"r, it

not

clear solutions

be difScult to obtain

salt

the

perfectly clear solutions.

with

products of unsound

juice and

the

filtrate does

polarization should

The

It

reject portioca of

to

If the

to

materials

other

and

sugars

returned

recommended.

be

to

solution, changing

new

a

sometimes

It may

analyzing

clear.

lead.

of

usually

be

it may

clear

accuracy

runs

prepare

subacetate

in

ANALYSIS.

SUQAB

IN

METHODS

OPTICAL

are

more

of

good

convenient,

glass. stemless

cylinders

funnels

is the

ease

and

heavy

with

which

SPECIAL

be

washed

they

may

very

convenient

and

167

APPARATUS.

SUGAR

dried.

jar and

The

cylinderare

supports for the funnels.

Sugar-flasks. ^The flasks used in sugar-work are usually They graduated to hold 50 cc. 100 cc, or multiplesof 100 cc. also graduated with two marks, viz.,50-55 cc, 100-110 are then called sugar-flasks'' by the dealers. cc, etc, and are Orders should to dealers for flasks and other precisionware in stating the system of graduation, whether be very specific It is important that all to Mohr's cc. or units,or metric cc. in the laboratory be of the same such ware tion. system of gradua"

'^

Mohr's

should

units

weight of 26.048

be

and

grams

with

used

the metric

or

the true

old cc.

normal C.

at 20"

R 110 "0

Fig.

with

the

weight of

normal

International

26

40.

for Uniform

Commission

that

grams,

adopted by

the

Methods.

glass tubing of uniform The and circular cross-section. shape of the body of bore the flask should approximate that of the diagrams in Fig. 40. A flask of this form gives little trouble from air-bubbles. necks of larger often have work for commercial Flasks Flasks

internal

should

of

S. Bureau

in

used

work.

specifiedbelow error

in the

the

S.

Customs

should

is unnecessary be adhered t9.

of the neck

capacity of flasks

of Standards:

U.

This

internal diameters

following maximum the U.

from

those

in research

or

diameters

of tolerance

made

than

diameter

laboratories the

be

are

and

and The limits

specifiedby

168

OPTICAL

small

such

of

of

is

writer

all calibration,

and

flasks

of

hundred

several

flasks chased purfor the laboratories under the

bearing the maker's

well within

were

ANALYSIS.

apparently large for

prominent dealer

of the

SUGAR

Of

diameter.

neck a

direction

IN

of tolerance

limit

Tbis

METHODS

the tolerance

certificate limits

given

in the table. The

specifiedfor use in the U. S. Custom These have a height laboratories are like B of Fig. 40. in length and its internal The neck is 70 mm. mm. 100

House of 130

diameter 12.6 30

mm.

flasks

cc.

The

mm.

from

less than

be not

must

11.6

graduation marks

the upper

end

and

and

mm.

shall be

16

not

than

more

less

not

than

fyom the lower end

mm.

of the neck. The

flasks shown

in

in

Fig. 40 all conform

shape of the body the U. S. Customs tions. regulaThey should be distinctly

with

jnarked the

with

system

"Contains

true

capacity and graduation, e.g.,

of 100

for the Mohr 100

their

cc,

flask and

20** C."

cc,

C* 17.6/17.5"

for the metric

cubic-centimeter

graduation-mark encircle

"Contains

flasks. should

the

neck

or

The pletely com-

of

the

flask. Pellet's conical are

of

rubber bottom Fig.

41.

facilitates the escape

flasks.Fig. 41, strong glass and have a to tfie cover sUp over and a ring for the neck

to reduce

breakage. Their form gives them great stabilityand

of air-bubbles.

^

SIECIAL

SUGAR

Referringto Fig. 40, the fill most

of

The

the

169

APPARATUS.

and

flasks A

requirements of

Stift (C) and

of various capacities

B the

Kohlrausch

oratory. sugar-house lab-

(D) flasks

used

are

in the

analysis of Alter press-cake. The flask C if narrow the graduation may be used in all classes of work. The

flasks should

at

be

frequently and thoroughly cleaned. * C. A. Browne recommends solution cleaning with a warm of sodium hydroxide and Bochelle salts,such as is used in the film of lead preparing Fehling's solution. This removes '

that

carbonate commercial

the walls of the flask.

deposits upon acid is

muriatic

Strong cleaning in nitric acid, followed

used

usually

for this

Treatment with sugar-house laboratories. by washing and then a strong solution of chromic acid in concentrated sulphuric acid,is good preparation of flasks for calibration.

It is advisable

to

the chromic

use

acid

solution

the frequently in cleansing flasks. After this treatment drops of water will drain from the neck of the flask properly instead of adhering to it. Calibration of Sugar-flasks. No flask should be used in "

important capacity.

work

without

There

is much

confusion

the true

and.Mohr's

between

being sometimes

system to

having first verified its marked

marked

the

on

cc,

part of

having been

as

facturers manu-

flasks of the

one

graduated

the other. Cleanse

the

flask

dry it in moisture return

The errors

has

an

has

as

On

oven.

condensed

the flask to the

balance

hand

be

walls

and

case,

counterpoising. Remove counterpoise the weight on

Cool but

the do

not

flask

Fill the flask to the mark

""

Hai^book

so

to

the

the

This

with

left-

be used

the balance

right-hand pan

flask.

perature tem-

room

wipe it again, and

the flask from

for the

flask to the limits of

1

if

eliminate

to

accurately counterpoise it, placing it upon balance-pan. Pieces of metal or weights may

weights substituted

oughly thor-

whether

note

substitution

by

itself.

in

the

inside

the

and

oven.

in the balance then

above

cooling the flask

upon

weighing should of the

described

been

and

accurate

gives the weight of of the analyticalweights. accuracy with recently boiled distilled water

of Sugar

Analysis,"

p.

171.

170

of

METHODS

OPTICAL

running

the

wetting

the

neck

the flask,with

of

neck.

Remove

of the

flask by

with

the

graduation

part

of

Place

the

the

odd

level

filled flask

and

the

upon

pieces the

note

and

of

is

the

Our

the

to

100

Mohr's

to

The

and

of 100

the

hne

neck

lower

with of

means

the small

a

before

as

weights.

or

the

of

and

Remove with

water

an

42.

weight

weight whether

cc.

the

correction

99.958

shows

at 20"

to

the

of

the

metal that

as

the

with

the

of the

flask

flask

balance

C, hence

to

of

water

be

the

gives the

ie in prop"

at

20"

of

C.

and

452

Mobr

to

or

For at

20"

apparent

453,

to

the

example: C.

Refei^

weight

of

the flask is correctly graduated

Similarly using the table

pages

temperatures.

grams this

tables,

(according

cc.

various

at

table

this system.

water

had

weight

flask contains

ence

metal

this

the

water

now

table)

cc.

ing fill-

not.

or

Reference

true

record

of the

weight

showing

by

Counterpoise the

Deducting

adjustment

in

the

of the If

balance-pan

temperature

thennometer.

water.

correct

is not water

Verify

eye.

the

to

bring it into line.

analytical weights and

the

in

is possible

as

part

upper

of

remove

Fis.

accurate

the

meniscu?

or

count"rpoiBe it with

fla^

the

at

of

it by

used

adhere

may

roll of filter-paper.

a

be

far

bo

that

water

holding

curve

graduation-mark, pipette and

ANALTBIB.

into the flaak to avoid

water

the

SDOAB

large pipette should

A

temperature.

room

the

IN

corrections

same

for

i3+0.282, which

flask and true

cc.

added

weight at to

20"

of C.

99.95S

172

OPTICAL

shown

in F^.

Fig. 43, b

a

the

same

In

the

balance

Two be

is suitable.

quantity,

for

'weights,

One

set

of

verifying and

The

balances

with

a

should

at

importance than weights The

bulhon

venient

capacity balance it from

several

for

speed

and

should dust

be

and

is

a

to

currents

That

suitable

half

should

sensitive

within

2

in

of air. of size.

5

other

pan.

in

kept

the

others.

milligrams materials

of sugar

usually sufficiently through

weighing

in Fig. 44

weighings are

in

are

ation evapor-

of

more

This

hood

instrument

kilograms, It should

is very which

eon-

large

essentials.

glass-framed

a

back

milligrams.

shown

rough

sugar.

the

be

two

to

are

in alow

a

normal, should

weight of

the

manipulation

placed

capacities.

milligrams,

of

and

the

be introduced

may

so-called

in

milligrams

of balance

type the

2

of moisture

absorption

or

gram

of at

pan

though weights

that

errors

weight

weights

least be

for polarization,to within The

normal

checking

full load in the pans,

accurate.

1

in

rapid weighings

in the

grams

these

balance, shown

for very

normal

counterpoiee

of sugar

provided.

reserve

the

e.g.

ANALYSIS.

decimal

type

illustrated,10

instrument

sets

The

convenient

very

o(

of the '

43

S^QAB

IN

METHODS

to

protect

is made

sensitive

have

This

to

in 100

agate bearings

HEATING

and

knife

use

in

bagasse analysis and and

Washr-hoUles, solution bottles

for on

should

This scale is suitable for

edges for tropicalwork.

of massecuites

have

determining the degree Brix

in

molasses.

Stock-bottles.

in sugar shelf above

The

"

work-table.

the

glass syphon-tube with

a

and

water

analysis,should

use

a

173

DEVICES.

the

lead

be

kept in large

The

water-bottle

rubber

connections, a

glass-nozzle,forming a convenient ment arrangeing for washing samples into the sugar-flaskand for dilutthe solutions to the graduations on the necks of the flasks. This is a very satisfactoryform of wash-bottle, and several about the laboratory. The of these should be distributed

pinch-cock and

lead

subacetate

bottle

should

be connected

with

reservoir-

a

FiG. 45. ,

The

burette.

burette

has

a

three-way cock,

connecting with the stock-bottle and

rubber

a

tube.

The

by

means

air-inlet to the

of

a

one

opening

glasssyphon

subacetate-of-lead

ing containprovided with a small wash-bottle caustic soda solution,to absorb the carbonic acid and prevent

should

bottle

be

precipitationof the lead. since

a

small

is not precipitation

large stock-bottles should he employed.

very

lead -subacetate

Where

This

are

used

solution

is not

strictlynecessary, objectionable,but where the washing arrangement

is used

in

storing samples

containing the concentrated should also be provided. of

juice a

stock-bottle

hot-plate is the heating device for laboratories having

Heating

Devices.

"

The

solution

electric

most a

venient con-

24-hours

w

174

OPTICAL

METHODS

electricservice. Where

IN

SUGAR

ANALYSIS.

the generatorsare

only operatedat

night the hot-platesmust be supplemented by stoves. The Norma alcohol stove Fig. 45 is satisf^^ctory for heating in etc. extractions, inversions, Notes 82. The on Polariscopic Manipulations. should not bear heavily of the observation-tubes screw-caps the cover-glasses,since glass is double-refracting upon does not quickly recover under these conditions and its condition. normal A largeerror be introduced through may excessive pressure the glasses. The cover-glasses should on be of the best qualityof glass, perfectlyclean and with parallel sides. A glassmay be tested with regard to the parallelism of its surfaces by holding it in front of a window and looking through it at a window-bar; on revolving the glassslowly if the bar appears between the thumb and a finger, to move and the should be the surfaces are not parallel glass rejected. become Old glasses which have scratched should slightly "

.

not

be

used.

frequentlywashed

Glasses

and

observation-tubes

should

be

with acetic acid.

should planes of the ends of the observation-tubes This may be tested be perpendicularto the axis of the tube. by placing a tube filled with a sugar solution in the trough of the polariscopeand making an observation; on revolving the tube in the trough, and making observations at different should the readings vary, the ends of the tube positions, have not been properlyground. The manufacturers of polariscopesand their accessories in their methods that faulty have attained such accuracy apparatus rarely leaves their workshops, nevertheless the scales and accessories should be checked to verifygraduations, and tube length. The polariscopeshould be used in a well-ventilated room. It should be protected from the heat of the lamp and, so A confrom light from other sources. far as practicable, venient in 'a box, arrangement is to place the instrument The end lamp is placed outside the leaving one open. box, oppositethe open end, and lightsthe instrument through In making a reading,the observer stands a small opening. end of the box, his body cutting off the greater at the open light. The inside of the box should part of the extraneous The

VOLUME

painted black.

be the

bottom

THE

OP

LEAD

175

PBECIPITATB.

should polariseope

The

of the box

table,so

or

that

be

fastened to

it may

readily

not

jarred out of position.

be

The

illumination the

light from

scale

polariscopelamp

models

of instruments.

in the

absence

by

the

of

is effected

by

reflecting

it,except in the old A small electric lamp should be used

of reflectors.

upon

The

current

may

be

supplied by dry-batteriesand should be bell push-button. A gas-jetor candle should

a

for this

used

lightingon

of

account

iently conven-

controlled be

never

overheating the scale

or

damaging the polariscope. The

the

settingof

zero

polariscopescale

verified,using standardized bichromate

filter-cell(see page

this verification

and

plates. The always be used in

must

removed

from

of the dark

account

quently fre-

the

In

fact this

polariscope

color of the solution

tested.

Influence

83.

be

be

quartz

adjusting the vernier.

in

ray-filtershould never or on except for refilling to be

145)

should

Volume

of the

of the

Lead

tate. Precipi-

precipitateintroduces errors into the polariof which are probably offset by compensoopicanalysis,some sating notably in the analysisof low-grade products. errors, The error due to the volume occupied by the precipitatewill be considered in this paragraph, and those due to influence of ^The lead

"

lead

the

will be

the

upon

discussed

It is evident

occupied by

farther

that

if

so

high.

This

part of the volume

a

bodies

on.

solid, and

there

be

of the flask be

compensation

no

for the

polariscopicreading will be too has been studied by numerous chemists,

matter

especiallyin

more

opticallyactive

other

occupied, the

volume

but

a

and

sugars

connection

with

the

beet-sugarand

refiningindustries. and others noticed by Rafe and Pellet,Commerson, It was that in low-grade products, the saline coeflficientof which is of the high, there is apparently no error due to the volume laige precipitate.They attributed this fact to an absorption of

From is

at the by the precipitate

sucrose

no

concluded

experiAientsSachs*

numerous

absorption of

sucrose,

and

attributed

Universelle

de la Fabrication

the

there

results with

'"'"""

"

Revue

that .

"

1

of its formation.

moment

da

Sucre, 1. 451.

176

OPTICAL

METHODS

low

products

and

sodium

the

to

formed

This

sucrose.

view

ANALYSIS.

of the

with

acetic

the

is strengthened in the

juices,due

of

acetates

acid

the

salt, upon

perceptible error,

very

SUGAR

influence

lead

of the

IN

from

rotatory

potassium

the

position decomof the

power

by the fact that there is a

of polarization

both

beet

and

the

precipitate. In the precipitation of the impuritiespf juicesbut little of these acetates is

sugar-cane

to

with

formed, whereas

low

products the quantity is laige. Sachs's made experiments were tration by increasingthe concenof the solution instead of by dilution as practiced The following data are from Sachs's paper: by Scheibler. *

dissolved

He

x

in water,

sufficient

added

lead salt for clarification, completed the volume

af the

solution

100

to

increases frpm Since

of molasses

grams

the.

volume

ratio.

same

The quantity polarized as usual. experiment to experiment by equal increments. and

cc,

quantity of

the

of the

of the

An

if this

nere.the

volume

of the

molasses

is increased

with

in the

ment experi-

increase

precipitate must

increase

each

volume

of the

x

in the

precipitate,

should incf^9ase only dist^urbinginfljiejace, is due to the sugar, since the than the, polarization, mpre

solution is decreased. .

Letting ajF=the weight of molasses, and 2/=the polariscopic

reading,the

ratio "

if there

is

an

error,

compensated

by

should

-

increase

to

other

the volume

substitutingthe

values

1st Series *'

2d

the

errors

of thb In

a

x

and

y

in the

not precipitate,

used

grams

1.900

1.900

2.14

2.13

2.14

following numbers

1st

Series.

quantities

in 100

and

cc,

ratio and

reducing

1.906

1.896

2.14

that minus

of the ratio shows

for that

due

to

volume

the

beet-juicesSachs

obtained

:

0.5446

0.5474

0.5800

0.5836 !

.

"^ Revue

35

1.906

precipitate. similar experiment with

''

concentration,

followingfigures:

the

2d

of

Sachs

5 to

value practicallyconstant have fully compensated

The

of the

influences.

ranging from

obtained

the

I

due

of beet-molasses

he

with

X

UniverBelle

""

'

I

...I.

0.5480

.

de la Fabrication

0.5842 "

du Sucre, 1, 451.

0.5497 0.5860 ,1

.(i

,

"

The an

VOLUME

OF

increase

in the

due

error

sufficient

not

results

by the

similar

unpublished analyses the

at

Juice

writer's

25 gr. :1

1st Series "

2d Series

No.

2

is

that

dividing the

precipitate and

there

is

Cuba

with

of Sachs, and

several

series of R.

L.

by

Cook,

following results:

the

50 gr. :2

cc.

cane-molasses

75

ck.

gr. :3

100

cc.

gr. :4 cc.

0.628

0.632

0.633

0.628

0.630

0.633

0.634

times

weight

in

normal

the

of 0.13

error

in the

error

2d

The

1. 100

polarization of

cc.

4

100

and

cc.

16.49, shomng

was

of

cent

per

16.36, and

was

weight in

polariseope reading by

uncompensated

it.

correct

0.628

uncompensated

an

is

duplicate of No.

a

using lour

in

gave

juice using the normal

the

there

cane-juices made

instance,

lead

and

of

that

to

error

those

to

juices shows

of the

author

177

PREOIPITATB.

ratio with

compensating

Experiments gave

LEAD

volume

tha

to

THE

The

sucrose.

Series, ttsingthe

juice,

same

0.15*^

was

In

experiments by Cook, in the first and the polarization was inunediate in the second

of which after Juice

1st

series of

other

two

forty hours,

lead. .20 gr. :1

and

Series..... "

2d As

in the

of Cook

results

the

cc.

40

gr. :2

flask.

Wash

add

0.692

0.693

0.694

of Sachs's

experiments with beets, this work is

there

that

the

of

and

dilute

the

as

Revue

determining

cc.

tall

of

ume vol-

the

juice with

sub.

cylinder instead

water, until

precipitateto

the

weight of solution

all of a

ICO-cc.

100

cc,

observation-tube.

a

cold

sucrose

flask and

dissolve

cane-sugar,

to

the

of

the

mix, filter,and The

results

are

follows: "

'"'""'"'

hot

400-mm.

a

a

precipitate.

of the

precipitate by decantation, first with

normal

^

volume

the

usual, using

Transfer

polarize,using t^'mim^^^^'^^

as

the

calculated

to

in the

perceptible error

very

a

following method

one-half

sugar,

:5 cc"

gr.

0.690

finally with

is removed.

cc.lOO

0.687

the

and

water

gr. :4

0.696

of lead

acetate

80

0.694

precipitate: Clarify 100

of the

cc.

0.690(?)

case

used

CO gr. :3

0.691

analysis of cane-juices due ^

cc.

follows:

as

0.690

shows

Sachs

were

"

Universelle

"

.

"

de

.^----1

I

'

"""""".

la Fabrication

du

Sucre,

1, 451.

178

OPTICAL

Let

IN

METHODS

P""per

of

cent

BUGAB

in the

sucrose

ANALYSIS.

sugar;

P^"the

X

polarizationof the solution,made of the precipitate; presence of the lead precipitate. ="the volume

,-i50^ziOOP

"

Then

Let

Example:

P="

99.9;

P'"

100.77.

^^(100X100.77)-(100X99.

Vh^r. Then

X

^^^j;^

followingis

The for the

the

of the

"Scheibler's double-dilution

termed

9) ^. ^ ^-0.86cc. ^^

of Scheibler

method

due to the volume

error

in the

up

^

ior

correcting

predpitate^and usually method":

To

100

cc.

of juice add the requisite quantity of sobacetate lead for the clarification, to. 110 cc. of complete the volume of

the

and

polarize as

juiceadd lead polarize. Calculation subtract

as

:

by

reading. The calculation

to

Multiplythe 2.2

and

portion of 100

per

cc,

of and

polariscopereading by 2, first reading,multiply the

the

product from the first required reading for the

this

is the

cent

to 220

cC:

second

deduct

remainder

of the

second

a

before, complete the volume

product from

the

remainder

usual;

sucrose:

Example, Degree Brix of the juices First polariscope reading (110 cc.) '*

Second

2X28.7"57.4; 300

we

(220 cc.)....

have:

15.18 .03 .02 15.23 ^

67.6 28.7

57.6-0.44 2.2X0.2=0.44; polariscope reading. By Schmitz table,

67.6-67.4-0.2;

"57.16=corrected page

''

18 .0

=

required per

Zeit. RUbenzucker-Industrie,

cent. 25, 1054.

1

80

caused

by excessive of 0,5

excess

2

cc.

of 0.11" and 3

scale. excess

with 6

cc.

of

1

cc.

in

reaches

and continues

excess

added.

of lead solution

returns

A

to

0.12**;

the cane-sugar value when an

the initial value

to increase with

sugar

of

cc.

An

on

minimum

a

is present and

co.

0.1**;1

of

diminution of 0.90"

a

rotation

The

diminution

a

of lead.

of subacetate

amounts

causes

cc.

ANALYSIS.

SUGAR

IN

METHODS

OPTICAL

the amount

polarizing99.9"

used

was

experiments.

in these

followingobservations relative to constant the influence of certain inorganic salts: "With chlorides of barium, strontium, relation of sugar to water, the decrease in the and calcium cause a rotation,which continues to decrease as the salt is increased; calcium chloride causes a

made

^

Famsteiner

decrease, but

addition

the

the salt reaches

when

whieh

increase

an

causes

a

maximum

further

finallyexceeds

that

of

sohition. the pure-sugar "If the relation of the sugar to that of the salt be kept in all constant, it is found that the addition of water causes cases

the

specificrotatory power, i.e.,the The specific rotatory power unaffected by varying the quantity of sugar with

of the salts is lessened.

action

is almost a

in

increase

an

lithium, sodium, and

of

'^

examination

An

the salt and

relation between

constant

The

water.

potassium behave

of the action of the

in

a

chlorides

similar

ner. man-

quantitiesof different salts shows that in the ease of strontium, calcium, and magnesium the depression varies inversely with the molecular weight,and that the product of the two quantities chloride does not act Barium is approximately a constant. in the

same

relation, however,

similar relation.

The

within each

of chlorides and

The

group

rotatory

to

as

much

In his

1

power

modified

potassiumeven

and

Berichte

not

alkalis show

only holds

for two

salts

a

good

belonging

groups."

solution is not

[_

but the clilorides of the

manner,

to different

same

as

of

by

when

sucrose

in

the presence

iSO per cent

chem.

in

or

alcohol

of nitrates of sodium

the

quantity of the nitrate amounts of the sucrose (E. Gravier).

of the influence investigation deut.

water

Gesell.

of the lead

23, 3570; Journ.

Chem.

precipitate,

Soc, 60, 283.

1 INFLUENCE

*

SUB

OF

ACETATE

OF

181

LEAD.

that the presence of acetate of potassium very the rotation. The diminution was perceptiblydiminished Sachs

found

also noticeable

with

sulphatesof potassium

the

salts. corresponding sodium also states of Sachs that citrate of potassium, carbonate sodium, and several other salts have an influence analogous not

was

of the

use

of tannic

Sachs

further

solutions decolorizing

of the volume

of the

that

states

is very

tionable objec-

precipitateformed

lead.

the

with

of free acetic acid

presence

in part.

acid in

account

on

the

The

acetates.

this influence

reduces the

marked

so

that

to

with

lead,but

and

^The rotatory power of dextrose is not modified, if at all, but very slightly, by either the subacetate oi

Dextrose. or,

"

lead, under See also Invert-sugar. neutral

The

I.evulose. "

diminished

by

added

acid

of

acetate

of levulose

rotatory power

the

presence

of subacetate

acidity restores

to

analyticalconditions

the

the

is very of lead.

rotation

precipitated

a

lead salt in the presence

Acetic levulose

of the

(Gillin 1871, Spencer in 1885, Pellet). Levulose as

greatly

is

of certain

partly

chlorides,

quantitiesgreater or less,according to the relative pro* portions of the salts,lead, and levulose (Pellet,Edson). of lead precipitateslevulose in part, when Basic acetate in

salts

in the

occur

basic acetate

same

solution with

of lead forms

constituents

of which

insoluble combinations

(Prinsen-

GJeerligs). Invert-sugar Dextrose^ and

Levulose.

In

"

the

J

the

salts formed

in the

decompositionof

the

lead, dextrose, and levulose are The influence of the basic lead salt Edson).

presence

subacetate

precipitatedin part

of levulose (seeLevulose)

is not

dextrose, which

Increasingamounts

affected

of subacetate

the left solutions decrease sugar rotation is to the righton account

C. the

H.

Gill called

Chemical

^

Revue

attention

to

of that

dc la Fabrication

in the

du

to

invert-

finallythe

of the in the

error

to the

plus error.

a

added

rotation,and

Society,April, 1871, and Universdle

prominence

of lead

this

(Pellet,

of levu'osate

results in

and

of

the rotatory

on

the formation

or power little lead of of opticalactivitygivesundue

of

dextrose. Journal

of

early editions

Sucre. 1, 151.

182

OPTICAL

METHODS

of this book, the the

restore

Acetic

author

rotatory

hydrochloric

acetate

and

sodic Wm.

and

acids

with

warming

rotation

the

Malic acid

is

the

effect.

rotation

Sodic

(H. A.

Sulphuric and hydrochloric

rotation; oxalic acid has

effect.

no

The

the

as

its

^This acid is Isevorotatory. The

"

Malic

opticallyinactive.

is

acid

requires

artificial malic

precipitated by

of lead.

Pjrapectine.

and

Pectine

"

and the

to

of invert-

power

opposite

an

increase

to corresponding

acid.

subacetate

and

rotatory

dilution, which twenty-four hours' (Gube *).

about

acid

quantity of the mineral acid is the invert-sugar solution be diluted after hydrochloricacid, it does not quickly reach

If

increased.

has

McPhersons).

increases

rotation

of a"etic

use

levulose.

the

chloride

the

increase

acid

ANALYSIS.

the

of th"

slightlylowers

acid

SUGAR

advised

power

sugar;

Weber

IN

by normal

second

Not

Asparagine. "

substances

lead salt.

precipitableby solution

In water

and

rotatory dextroof

leadt

of lead.

acetate

dextrorotatory instead

is rendered

are

precipitated by subacetate

both

are

^These

lead, but Isevorotatoryby the

subacetate of

of

alkaline solution

asparagine is laevorotatory;in acid solution,dextrorotatory.* Asparagine is insoluble in alcohol,and in the presence of acetic acid is inactive.*

Isevorotatory; in

is

in the with

and

additional

presence

it is

mineral

of acetic acid the of the

acid

asparagine

tory; acid, dextrorota-

rotation becomes

is diminished

0", and

with

dextrorotatory (Degener). Asparagine

in

salt is found

lime

a

solution

from

immature

cane;

aspartic acid by the action of lime, and

to

Aspartic Acid. the

of

that cane-jiiice, especially

changed

lime

is

acid

alkaline

and

presence

molecules

10

is present in

a

neutral

In

as

molasses.*

asparagine by the action of lime; In alkaline solutions,aspartates salt is soluble. From

"

solutions in acid laevorotatory and dextrorotatory. Aspartic acid is precipitatedby subacetate of lead.

are

Chimistes

Aaaoc

"

Bulletin

2

Optical Rotation

of

de

Organic

France, 3, 131. Substances,

Landolt

Dr. Long's "ng.

"

ed., 541. "

Champion

"

W.

and

Maxwell,

Pellet, Compt. Bui.

38, 2d

Rend.^ 83, 819.

Series, La. Expt. Station,

p.

1380.

183

ERROR.

BONE-BLACK

Error. Bone-black Bone-black absorbent action on an sugars.

85.

"

anknal

or

exercises

it is desirable to

avoid

using it

possible. It is advised quantitiesranging from black

half-normal

the

to

solution;

advise

others

solution

For

qharcoal

this

reason

in

analyticalwork whenever by different experimenters to add of powdered, dry bone1 to 3 grams weight of material in 100 cc. of filtration of 50

the

small

of the

cc.

bone-black

of

sugar

the through quantity and then the filtration of sufficient rejectionof the filtrate, a

and

for the observation. In

experiments the writer adopted the following method: Place a small quantity of bone-black, about 3 grams, in a small plain filter, rather slow filtering-paper. a selecting Add volume of the solution equal to that of the char or a just completely moisten the latter,and let this liquid filter recent

off.

After

which

be

five similar

or

rejected,test

are

and

four

the

as

tion observapolariscopic

a

reading varies. Solutions must evaporation during the filtration. So

protected from

soon

filtrates by

the

whether

note

the filtratesfrom filtrations,

the

reading is constant, showing

record

it

the

further

no

number.

tion, absorp-

is required tedious,but apparently gives very satisfactory results very when the coloring matter is not difficult to remove. If the color persistsobstinately, it is preferable to filter the 8olu" tion through the bone-black and reject thf first half of the filtrate.

The

as

of the

use

This

.method

nitrogenfilled concent|*atedfilament

Mazda

in polarizingwill usually enable electric-lamp dispensewith animal charcoal.

"

86.

Influence

The

compensating type

readings The was

the

at

17.5" C 1898

adopted 20" C.

of

temperature

standard

former

about

of Temperature

and

temperature

it for

only give correct

to this standard.

Commission

for Uniform

26

the normal

as

Methods

weight

standardized.,

was

these

usually all the instruments

conformed

grams

which

to

Polarizations*

upop

polariscopecan at

one

instruments

made

In oi

and

1897

pijor to the International

Sugar Analysis 100

true

cc.

at

the

The instrument makers corresponding volume. with this specification. have conformed The rotation due to the quartz wedges increases with rise as

of temperature

and

that of

sucrose

decreases.

Dr.

H.

W.

184

METHODS

OPTICAL

Wiley called the the

to

and

into

prepared

SUGAR

ANALYSIS.

of the IT. S. Treasury

attention

introduced

errors

conditions

IN

polarizationsby these

sugar

A. Browne

made

*

The

table of corrections.

a

in raw-sugar

applies a temperature correction based upon Wiley's observations. Charles

Department

a

ury Treas-

testing

full study of the influence

very

in the

and cluded conpolarizationof raw-sugars that it is impossible to devise a simple reliable method In view of this conclusion, of corrections for cane-sugars. he has equipped his laboratory (New York Sugar Trade in which all Laboratory) with constant temperature rooms solutions are prepared and polarized at 20" C. This sugar

of temperature

obviates

arrangement Brown

questionof

?*[!-0.0003 (t- 20)], formula, P^" is the corrected polarization,P*, the observed

P*"

=

polarization,and t the temperature serious error be applied without 96** and

above

Few, if

any

of the

Neither

of lower

polarization. equipped for polarizations

sugars

are

conditions.

Obviously certain precautions can, and should, be observed reduce errors: The laboratory and polariscoperoom should well ventilated

be

should

and

of the

be in the

not

gar,

in

used

part

reports), should

be

as

vicinityof

basis

a

rather

iiii tropicallaboratories

a

wall

ariscope polor

the

be

prepared and Composite samples of

a

than

technical

time

(run

reports

of low

temperature

in the heat

of the

noon. after-

required for the instrument itself when of the Laurent liglt. type using monochromatic Limits in Saccharimetric of Accuracy 87. sis.* AnalyNo

temperature

"

Dr.

*

Handbook

*

Dr.

C.

C.

of Sugar A.

Browne,

the

title before

20, 1914.

A.

The from

New comments

this paper,

correction

heated

should

of the

polarized at

The

temperature.

same

solutions laboratory-ovens. The polarized at room temperature. 8

also be used.

may

factories

sugar

observation, may polarizing cane-sugar

to

applicable to

are

standard

under

to

Wiley'stable

that

formula

table, nor

corrections.

that the

states

in which

all

Browne

Y.

twelve

notes

Analysis, N.

is

and

may

255-262.

pp.

Sugar

Orleans

that

errors

Trade

Section

of

conclusions

Lab., read the in

including the summing

Am. this up

a

with

paper

Chem.

paragraph of the

this

Soc., Nov. residual

are

stracted aberror.

ACCURACY

into

enter

analysis. While

sugar

sugar-testingthey apply also other

to

185

ANALYSIS.

SACCHARIMBTRIC

IN

these refer specifically to exto^it in all

considerable

a

analyses:

1. Loss

of moisture

during mixing.

of moisture

during weighing.

Loss

2. 3.

Error

in normal

6.

Error

in capacity of flasks.

7.

Imperfect mixing of contents of flask* Evaporation during filtering. Error in length of polariscopetubes.

weights. 4. Volume of precipitatein clarification. 5. Precipitationof levulose.

8. 9.

of bichromate

10. Omission 11.

Variations

12.

Defects

The

errors

vary

3, 6,

results. but

with

weights

near

and

9

careful

each

slightlyon

may

balance.

12

flasks

Since

disappear

errors

the

in temperature.

in scales of saccharimeters.

and the

cell.

in

the

and

tubes

do

not

in

appear

that

numbers, the The of duplicate tests.

averages

correct

of easilybe kept within the limits of accuracy be checked The scales of the jK)lariscopemay

be

corrections

scale may

Haensch

control-tube,Fig. 29.

the

following plus

are

numbered

as

errors

in the

Other checked

be

may

standard

accurate

made.

of the

Dr.

enter

quartz

points and with

Browne

the

in fact

Schmidt

estimates

These

previous list: Sugar

to:

Mixing on paper 2. Evaporation during weighing of precipitatein clarification. 4. Volume 5. Precipitationof levulose of the 7. Imperfect mixing of the contents .

.

Degrees. 05

+0

.

-f0.02 +0

18 .

-|-0.03

+0.05

flask

Evaporation during filtering of the bichromate

cell

10.

Omission

11.

Temperature variation from the standard Total

" that

in careless work.

1.

8.

pensating com-

selected

be

may

side of the

all parts

due

general mutually

management

important points with

the

plates and

Error

iii

are

error

-|-0.04 -f-0.07 +0.04 +0.48

186

The and

last the

in

Error

four

first

careful

0.20**

to

may

be

reduced.

should

not

exceed

four

ANALYSIS.

SUGAB

amounting

6iT0ts

work

due

IN

METHODS

OPTICAL

The

preventable

are

final

+0.12

residual

error

follows:

as

Sugar

tor

Degrees.

.

1.

Evaporation

in

mixing

2.

Evaporation

in

weighing

'Volume

4.

Total

There

are

considered introduced the

or

upon

The in

previous

alumina

of

permit,

will

Home's

dry-lead

precipitate

would

which to

"

0.5**

in is

tests or

in

defense

an

use

is

improbable this

morning

of arbitrary

that

admit.

the

most

addition error

during

lies the

temperature

so,

both

will

a

constant

in

a

lead

the

volume

these of

may

the error.

errors

in

lead

important

This

to

of

levulose

acetate

deal.

Since

cases.

the

dried

must

of

when

acetate,

nearly

or

of

one

that

acetate

eliminates

color

tion prepara-

from

normal

basic

of

use

chemist

against

the

possible

of

error

extreme

early in the the

the

conditions

tropical

the

is

It

pressure

entirely avoidable.

are

the

been those

as

cover-glasses,

removes,

by

temperature

laboratory

only

method

reduced

be

of

practically

error.

clarifying, where The

instead

such

work,

temperature

errors

or

already

quarta-plates,

different

cream

clarification

the

the

standardized a

have

this

of

pages

Such

etc.

material

of

at

that

error

upon

of the

solution

use

of

pressure

observation,

the

+0.120

the

wiping

the

of

+0.015

error

sources

by

+0.090

levulose

other in

+0.005

precipitate

of

Precipitatioikof

6.

+0.010

i

with

amount

temperature

sugar-house,

making

low-temperature corrections.

the

important

period,

188

METHODS

CHEMICAL

liter-flask, dilute

a

caustic

dilute 1000

inversion

the

completing

After

it

and

ANALYSIS.

transfer

neutralize

complete

and

cc.

solution

ths

almost

then

solution

soda

SUGAR

IN

to

with

it

volume

the

to

" .

analyzed

be

Measure*

50

of the

cc.

Collect

by

the

of

weight

this

weight in

sucrose

inversion, If the to

0.95

in

material

and

of

(B), beaker,

250-cc.

determine

using

minutes,

on

of

the

number

it to

of

terms

material

the

the of

OHiltiply of

weight

This

used.

yields

sucrose

it

of milligrams

189, 190, and

pages

in

copper

Ascertain

235.

page

the

the

plication multi-

invert-sugar,

on

100:95.

glucose

determine

Calculate

the

before

method

the

by

in

(reducing-sugar)

reduction

the

inversion

invert-sugar.

two

from

contains

after

boil

118,

since

ratio

the

and

reduce

to

quantity

sucrose,

118,

in

necessary

a

and

using the table

the is

for

methods

by

into

:

lamp.

invert-sugar

the

solution

of

cc,

416,

solution

oxide

cuprous

reduced,

copper

by

of the

the

of

one

page

sugar

flame

najted

the

397,

25

Wein

and

j

and

(A)

Meissl

of

should

and

levulose

and

foUowi^jg method solution

of

cc.

solution,

Soxhlet's add

the

by

25

dextrose

contains

solution

The

inversion described

just of

percentage

tion addi-

sucrose

as

follows: Per

cent

material

method

quantity

this

no

is present,

sucrose

paragraph are

Glucose

selected

substance

cent

per

for

in

glucose

the

sucrose.

(Beducing-sugar), glucose material

in the

depends

upon

also

and

"

th^.

whether

is present.

sucrose

If

of

of

be

to

inversion"

after

required

=the

:""0.95

Determlnatloa

90.

The

invert-sugar

present,

one

is to of

the

be

the used.

methods

method If on

described both page

sucrose

235

in and

should

the

ceding pre-

glucose be

ployed. em-

DETERMfNATlON

TABLE

FOR

THE

ESTIMATION

OF

SUCROSE.

OF

INVERTSUGAR.

180

190

TABLE

CHEMICAL

FOR

THE

METHODS

OP

ESTIMATION

OF

SUGAR

ANALYSIS.

INVERTnSUGAR.-Con"intt"l.

\

DETERMINATIONS.

DENSITY

APPARATUS

General

91.

degree

the

term

of

solution.

the

this

in

used

Brix

or

This

use

in

sense

graduations

The

"

termed

is

matter,

the

instruments

of

than

word

and

convenience.

will

work

sugar-

the

degree

be

are

Brix

the

of total

by

drying

is

in

Brix

often

termed

degrees

is

floating

understood

Balling,

to

and

the

is of

the

be

It

these

as

it

more

work.

Brix.

solution

mined deter-

as

true

degree the This

meant.

readings

in

The

"true,"

word

the

by

it

spindle

a

degree

called

a

liquid.

a

sugar-house

sugar

is often

qualified

degree

a

in

percentage

renders

apparent in

matter oven

an

when

Except

apparent

solid

the

the ^'The

spindle,

in

by

but

analysis

in

called, which

determined

as

This

sucrose

the

or

were

America. of

as

instrtunent

data Brix.

sugar

hydrometer,

Baum^

the

in

weight

Brix

eter hydrom-

Germany,

solids, dissolved

total

the

by in

by

of

system

Balling;

commercial

solution, is termed

percentage

The

In

This

names

percentage

Brix,

degree

scale

strictly

the

in

exclusively

commonly

are

convenient

spindle

and

checked

almost

the

or

feature

Brix.

"density"

is not

density

used

frequently

the

brevity

by

both

by

consider

to

customary

sugar

for

and

solution.

sugar

The

usage

devised

was

is used

Brix

is this

by

Balling."

or

is known

"Brix'*

solid

word

recalculated

hydrometer

pure

of the

book

also

Baum^

degree

hydrometers

Brix

afterwards

degree

this

on

graduation

name

chemists

Sugar the

synonymously

industry

sugar

is

"density"

expression

degrees."

Degree

92.

the

the

it is sanctioned

but

correct,

a

in

used

^The

"

"specific gravity."

with

"^

Remarks.

commonly

very

METHODS.

AND

on

its

Balling.

French

Brix-Dupont

two

use

and

the

modifications Brix-Vivien

of

this

spindles.

instrument, The 191

Brix-

19^

DENSITY

-

hydrometer reads 0" in distilled water Brix the spindle reads 0" at 17i" C, or

Dupont whereas

standard

the

to

DETERMINATIONS.

Chemistry,

Both

20" C.

at

100

in

sugar

weight and

of the

terms

of

percentage

these

well

be It may modifications

that

state

to

indicate

has

which

at

of

standard

the

is marked

of

values

relation

the

sugar

termed

are

and

Baum^

water

with

spelled the

94.

is marked of

1.8427

specific also graduated

of from

range

the

zero;

0"

50"

to

at

was

industry, but

scale.

Planters

one

at

of

the

recalculated,

Baum^

the *'new"

scale. or

time

used

The

"corrected"

given in the table, page

those

are

scale

Hydrometers

460.

almost

exclusively present chemists usually prefer

and

sugar-^maker^ still

Spindles.-^These

or

'^saccharometers"

frequently termed for

the

use

in

instruments

when

specially

the

graduated industry. "ugar A high-grade Brix hydrometer is shown in Fig. 46. instrument for

centage per-

scale.

Baum^

are

(also

spindles are

but

graduations

the

degrqps Baume

Brix

Baum6

sulphuric acid

Baum^

zero,

in

sucrose

sugar.

temperature

in pure

numbers

recalculated

the

its

required in the sugar industry. Scheibler and later Mategczek and

Gaslach

in the

spindle and

is

is all that

The

any

66".

below

for densities

the

in

sugar-house product. The hydrometer sinks in distilled

Baumd

the

correspondingpoint gravity

convenient

no

composition to

of

percentages

"

scale

Brix

the

containing only the pure The Baume. Degree

Beaum^)

water

in

of sugar

i.e.,grams

solutions

point

15" C.

at

of solution.

cc.

93,

cates indi-

hydrometer

solution

a

volume,

indicate

hydrometers

Brix- Vivien

The

percentages by weight. the

of

C,

according Congress of

International

adopted by the

15"

at

is

use

provided

ordinary work,

glass,and

without

the

standard

instruments

hag

with

in the

the

a

thermometer.

factory,are

thermometer.

made

This

Instruments of

In America

metal and

or

of

many Ger-

for the

temperature graduation of these The been, until recently, 17}" C. present

adopted by the International Congress of Applied Chemistry is 20" C, though this is not yet in general For these st^ndarda.' varying from use. temperatures standard

HYDBOMETEBS

OR

193

SPINDLES.

r\

corrections

must

be

Hydrometers

whose

is

temperature distilled water and

the

the

water

at this

a

volume 450

page

temperature

20

gravityis

words, the solution

1 7i" C.

at

of

of

The

at

the

table

for this normal

17i" C. whose

normal

is 20*^0.,

standard

or

specifiedby the try, Congress of Applied Chemisas

in water

floated

ture, reac! 0", and

the

at this

the

solutions, with

ponding

21

"H

Brix,

are

page

477.

A

tempera*

correspondingspecific The specific gravities

0.998234. of

Hl^

read 0".

weight

is constructed

International when

other

the

to

of water

lU

10

in

floated

of the sugar

is referred

Hydrometers

10

when

ings. read-

standard

or

temperature, In

volume

temperature, i 17

17J*'C.,

is 1.0000.

17J" C.

on

normal

the

corresponding specifiegravity

weight of same

applied to

In

corres^

the

given in

degrees the

table,

using the hydrometer,

it is floated

in

the

sugar

1-

solution on

the

and

of the and

17:

the

level

is at the

surface of the

liquid

ing, is selected for the readsince

varies

R'

viscosity of

the

R

at

R\ of Fig. 47.

not

point R

The

reading

scale is made

point R,

ig

the

with tion. solu-

the

It is often necessary mate estisolutions to in dark the

119::If

^

point R. the

vo-

jblOi

4(i.

FiQ.

47.

to

made

allowing for

become

the

of

the

reading of

The

scale is not

after

time

position

until

suflicient

hydrometer of the

same

194

DENSITY

DETERMINATIONS.

If the

the solution.

temperature of the liquid varies from the normal temperature for which the hydrometer is graduated,the observed reading of the scale must be corrected. temperature

as

For

instruments

whose

normal

temperature is 17}" C.J the corrections given in Gerlach's table,page 489, should be used. For instruments that are graduated at 20" C, in mission of the International Comconformitywith the specification for Uniform Methods, the table of corrections en pages 490 and work

to

491 should be used.

hydrometer

the

use

The

correction tables should

for

approximate results when Hydrometers the

the

be used the

with caution

and

onlv

differsmuch

temperature

the normal.

from

on

at near

It is necessary in accmrate its normal temperatiure.

paper

mercury

also made

writer recommends

The

with

printed with the thermometric degrees, the height of column indicatingthe correction to be applied. are

the

corrections

the iyp^f of hydrometer

shown

in

No difficulty is exbeing included. Fig. 46, the thermometer perienced in molasses soluin reading the temperature, even tions,

the instrument

since at most the

column

mercury

need

The

emerges.

be

lifted

should

stems

diameter, that the graduation may

only until

be of very and easily

be open read" A range of 10" Brix per 5 to 5.5 inches of stem is advised. Hydrometers should be tested from time to time, employing small

standardized solutions of the

at

temperature

which

pure

the

sucrose,

instrument

cylinder should

at

approximately graduated.

was

be

wide, so that the hydrometer-jar or spindlemay float perfectlyfreely. Balanced ^The principle of this The 95. Westphal be brieflystated as follows: A glass balance, Fig. 48, may bob is so adjusted as to be capable of displacing a given The

"

of grams,

number

five

for instance, of distilled water immersed

at

a

in the

wholly liquid and given teniperature fine wire. The bobs platinum b^ suspended by a may but for sugar-work ITi** C. graduated for any temperature; when

convenient, since this is

is most

in

employed

the temperature

is to

be

detei*mined

Adapted

Uluftration.

temperature

tables. preparingspecific-gravity

work

1

the

from

of the should

solution be

Bxilletin 13, Chem.

whose

exactly

that

For

usually accurate

specificgravity for which

Div., U. 8. Dept. Atrl.;

the also

1% '

DETERMINATIONS.

DENSITY

sponding graduations of

the

.300, .030, .003, .0003,

etc.

from

hook

of

case

The

which

bob

the

fallingupon the using the balance

of

balance

the

solution,at the standard with

riders

the

be

suspended

ia

graduation.

same

is

follows:

as

described

as

above

pend Susin

the

and

weight the beam is in equilibrium. Read

temperature,

until the

for other

weights may

one

of

method

Each

additional

than

more

graduationsr rider is provided with a

and

beam,

balance

off the

specificgravity from the position of the weights the beam. on Example: In determining the specificgravity of a sample of cane juice the position of the riders was

as

follows:

t

point of suspension of the bob

1 at 2 not

the

on

7.

3at

beam. =0.07

.r

.

4 at

"=1 .000

9

Specificgravity

=0

.009

=1

.079

correspondingto the specific degree Brix or Baum6 from the table, page be ascertained 482. gravity may bottles so are Pyknometers. structed conPyknometers 96. The

"

that

they

Given

liquid.

filled with

be

may

the

weight with the weight of an

It is not

often

necessary

definite volume

a

of this volume,

to

equal volume use

a

of

a

be comit may pared of distilled water.

pyknometer

in technical

rapid density determinations by the hydrometer accurate. being usually sufficiently in a great variety of forms. One Pyknometers are made

work, the

of the most

more

convenient

outlet

for the

in

Fig. 49.

The

side

of

the liquid when is put in place, also for the stopper, a fine thermometer, of the liquid rises. The bottle overflow, as the temperature should be filledwith the liquid cooled to a temperature lower the density is to be determined. As that at which than the pands temperature rises to the desired point, the liquid extube

provides

of these is shown

and tube.

the

At the and as

an

excess

is blotted

with

required temperature

receives the

excess

any

further

temperature

rises

the

paper cap

is

liquid that to

that

at

the^ side

placed in position

be pelled, exmay of the work-room.

197

TTKNOMETERS.

There

is

escape

of the air.

minute

a

opening

top of the

in the

cap

for the

/TN

in

It is convenient

termine de-

sugar-work gravity at 17 J**C, specific the solution at this temperature being of the with an equ"d weight compared to

the

of water

volume

Committee

Uniform

on

20"

Analysis adopted

of

4"C., the

at

Methods

C.

the

as

is indicated

as

follows:

of

that

and

standard

used

C. "-^-75 =1.07936,

of the

the" temperature

that

meaning

of its

temperature

density. The

maximum

solution

national Inter-

it to for the solution,referring

standard water

The

17i" C.

at

the

water

were

above the line 17i". The number that below is that of the solution,and

each

"

line,that of the water. of the pyknometer, described By means in this article, the weighings can readilybe made of the liquidheld by the gravity bottle at 17i"C. The specific the

under specific-gravity

these

conditions

is

by dividingthe weight of the solution by the weight of an equal calculated

volume In

the

In both

of water.

cases

the

bottle is filled at 17^" C.

determining the specific gravityat process

is

more

Fig. 49.

the standard

^

complicated,since the expansion of and

C, the

air

the

be taken into densitymust glass pyknometer The account. following description of the calculations, from

also the table,are

The

is

constant

it

was

weighed.

weight

is the

for the

The

apparent

mass

should

at the

therefore

The

weight

of the water

temperature, be

pyknometer

cooled distilled water, and

temperature

pyknometer

filledand

work.*

recentlyboiled and

is first filled with

and

Landolt's

determined

are

in the

noted.

air,a

t^,at which with

great

care.

*

Optischem

Drebungsvermogen.

kJ

K8

DETERMINATIONS.

DENSITY

calculations

The

whicli

letters have

the

TFo,the apparent

by the followingformula, in

made

are

of the

mass

indicated

values

the

below:

air at

in the

water

the

perature tem-

^oJ the

Fj

apparent

the

of the

mass

solution

sugar

in the

air at

t;

temperature

at the temperature specificgravity of water /gj coefficient cubical of the expansion of glass; 3^=0.000024,

Q,

the

"l=0.0012,

air

density;

rf|= specific gravity of the solution of the sugar t referred

The

of the

first factor

gravity, the

second

temperature

and

weights The the

in

third

the

at 4" C.

water

formula

factor

perature tem-

is the uncorrected

corrects

the

specific

specificgravity for

factor

is for

taken

from

the

reduction

to

vacuo.

of

value

end

to

at the

Q

may

of this article.

is small,

a

SPECIFIC

GRAVITY

mean

(From

be

If the

difference

value, 0.00C024, OF

Landolt's

WATER

AT

Optischem

Landolt's

may

VARIOUS

be

between used

for

table

^and

3^.

TEMPERATURES.

Drehungsvermogen.)

at

t^

GENERAL

ANALYTICAL

SAMPLING

97.

General

One

of the

"

of

the

diffezent

not

strictly repnaent analyticalwork

the

order

In

of

the

samples

material*

Or, they

a

defini^^^

composition of the material, value.

usually be of but little if any

continuously

drawing

securing rq)revarious products ait If a sample does

manufacture.

drawn

be

must

the

of

is that

the average will

Averaging.

unsatisfactory, problems

juices and

the

st.'^es of the

that

often

chemist

c^mensugar

and

Sampling

on

difficult , and

samples

sentative

AVERAOINQ.

AND

Remarks most

for the

WORK.

be

may in

representative they

proportion

secured

be

must

sample,

quantity in each

to

the

quantity intervals,

at

from

a

measured

weighed quantity of the material, the size of the sample

or

always bearing the This

sami^ed. and

by the Let

of

Importance D

and

A,B,C,

method

second

the

to

is the

of material

amount

usually practiced

one

sampling by aliquot parts.

is termed

The

relation

same

A"1000,

a

proper

which

5"800,

lot differ from

average

and

C=500, in

others

the

an

four

lots of

of the

sirup.

In

averaging

analysis. Manifestly a

and

and

analyses of

the

Thus

the volume. the

represent the average

house, it is advisable

cane-sugar

than

would

sdlids

apparent

at the

end

of

the

**

a

run

let each

Z)"*=200, and

equal patts of sirup ftom these lots would not of 10 parts o( A^S sample, but a mixture average 2 parts of D

the to

wei^ts

(Brix) "

or

sirup

sample is to be drawn.

of

C, and

trated is illus-

sampling

Given

following example: from

of

method

various use

the

of the

should

period the

mixture

be

sum

true

oi B, 5 of

composition

materials

in

a

weights rather

juice,the be

a

sucrose,

recorded of

the 199

daily

daily

200

GENERAL

ANALYTICAL

WORK.

divided weights of sucrose by the weight of the juice and the quotient multiplied by 100, will give the mean per cent in the juice and so on. of sucrose Similarlythe anal3^sesof those of the other products the sugars, and, so far as possible, should

be

averaged. For the general laboratory data, the author prefers to collect daily one composite sample of the juices and each product. This is advisable since the quantity of mg,terial estimated or represented by the analyses is usually known daily,thus giving the analytical work a definite value. the Cane in the Field. 98. It is pracSampling tically "

impossible to will be

that The

conditions, is

of iinalysis

parts of

obtain

to

even

the

from

to

of the

the

great

fields,the to

field.

a

accomplish, under sample that will in

able favorvery

a

Thfe

cane.

variations

Frequently in

day

of sugarcane

that of

stool and- also from

same

many

little from

will differ but

a

field.

small

a

receiving cane

is due

from

canes

sample

to

condition

the

sampling

in

hope

may

indicate

way

moderate"sized

a

fairlyrepresentativeof

even

chemist

best the

general

secure

ficulty dif-

in

the

various

large factory,

a

daily average

day whereas

analyses singleanalyses

widely from the average. In few stalks should be selected a sampling cut cane from second third row, or crossing the field one or every more times, according to its size, in sampling. The laiige sample, after mixing the canes, should be reduced by subsize for the laboratory. This sampling to one of convenient method is frequently impracticable, since the carts often may

vary

follow is

It

few

an

cutters.

almost

cane

fields,but

not

stools

canes

should

sample standing

impenetrable jungle.

of

entire

these

the

difficult to

more

parts of the and

behind

even

field is

the a

close

be

should from

reduced

secured

be

ditches

near

to

a

cane,

In

this

from or

since case

various

headlands,

convenient

mixing them thoroughly. of sampling the whole Perhaps the best method

number,

after

its arrival at

to

await

or

car-loads 99.

The

the

factory, then

other and apart from cane, at the the Cane Sampling

cane

is

grind several cartanalyze the juice.

Diffusion-bai^ry."

cane-chips may

be

sampled with

considerable

accuracy

201

BAGASSE.

SAMPLING

diffusion-battery.A handful of the cuttings or chips be withdrawn should shortly after they begin to fall into at the

diffuser,and

the half

filled.

this

be

taken

to

the diffuser is about

when

should

agate-ware

or

should

way

handful

samples

These

metal

covered

second

a

stored

be

in

pail. The samples the laboratory at

clean

a

drawn

in

frequent The milling

ground in the small mill. should be made very heavy by repassingthe bagasse through be composited, the The the mill. juice samples should in proportion to the number small samples being drawn be

and

intervals

of diffusers. Pellet a

*

the

recommends

period of

storage of the fresh chips during

hours, by placing an

twelve

ammonia

concentrated

open

bottle containing

in the

covered

sample-pail or

and

Exhausted

Diffusion-

box.

Bagasse

Sampling

100.

chips. ^To a certain extent the bagasse presents the same The bagasse,however, sampling difficultiesas the whole cane. in its passage less well mixed is more through the mills or be overcome and irregularities the by sampling across may "

conveyor.

Samples of bagasse should include all of that on a section its entire width. On of the bagasse-carrier, reaching the be quickly and the sample should thoroughly lalxHratory^ small mixed and sub-sampled. The sample may be analyzed immediately or stored six hours in a closed box in the presence A should be saturated with the of formaldehyde. sponge

preservativeand In

diffusion

removing

be attached

work, the

handful

a

to the

inside of the box-cover.

exhausted each

from

chips

diffuser

as

are

sampled by charged. they are dis-

samples should be stored in a covered for drainage. At vessel, with provision at the bottom should frequent intervals the composite samples so formed be analyzed and the analyses weighted, in calculatingthe of diffusers. day's average, according to the number the Juice. saturation or imbibition When 101. Sampling to secure is practiced it is necessary two samples of the These

small

"

one mill-juice,

1

from

Bulletin

the first mill and

Aasoo.

des

the second

ChimisteB,

XXII,

922.

from

all the

202

ANALYTICAL

GENERAL

mills.

It is

preferabletb draw

WORK.

the firstof these

samples from there is habilityof water the juice canal of the crusher when from the mill-bearings mixing with the juiceand in any events it is usually advisable

to

sample

Brix of this first sample is used so-called

normal

this

at as

a

undiluted

juice or

point. The degree basis in calculating the juice^from the analysis

mixed

juicesfrom the train of mills. The degrees. Brix of the two samples are also used in calculatingthe dilution of the mixed juicedue to maceration or leakage of water

of

the

the

mill-journals. in determining the factor Special sampling is necessary coefficient to be applied in reducing the degree Brix of

from

or

the crusher

or

first mill and

to terms of the norcrusher-juice^ mal be yielded in milling of equal efficiency

juice that would without a

maceration

of times

Bufficient number

tions with crusher

system

and

(or crusher are

automatic

in the

separatelysampled. devices

and

The

first mill) and

should

be

The

be determined its Taria-

to note

season

milling conditions.

and

cane

This factor should

water.

that

juicesfrom from"^ the

sampling should

continuous

for

an

the

entire be

hour

by or

sample is of relativelyhigh degree Brix, and purity, due to the comparatively moderate content sucrose The applied in crushing the cane. degree pressure Brix of the second sample is lower than that of the first on longer. The

first

crushing by the mills which and many of the impuritiesof the cane. extracts the rind-juice the degrees Brix of the two The factor is the relation between samples. The following ^utmple illustrates the calculation of

account

and

the

v"ry

of the factor:

use

heavy

Brix of the two

samples, respectively,

Brix 0.986. of the 4- 20 19.7"; factor mixed-juicesin regularmilling,19.6, then 19.6 X0.985" 19.3, undiluted the degree Brix of the normal or juice. The juice should be sampled automatically and in proportion The milling is usually veary uniform to that extracted. under good conditions of equipment and operation, hence 20"

and

=

19.7

"

ism, samplers may be operated by some part of the mill mechanpreferably a roll-shaft. Certain t3rpes of samplers may be driven by a reciprocating or other part of the juieepump.

The

Calumet

is

an

efficient type of

samplers (Fig. 50).

204

a

screw

WORK.

ANALYTICAL

GENERAL

adjustingthe

cavity and consequently inch hole is drilled at right angles to

for

of the

size of the

sample. A ^ the cavity and through it. Corresponding holes are drilled barrel for the inlet of air and the discharge through the pump of the sample from the plunger. Two rings of packing, controlled the by a follower and packing-ring,are placed around plunger, one between

the

at

end

outer

and the juice-inlet

barrel

of the

outlet.

and

should

Th^re

the be

other

an

oval

opening in the packing-ring where it passes the juice-outlet, to admit of adjustment. The barrel of the sampler is screwed into the pipe from which the juice is to be drawn is and This sampler may be clamped into place with a locknut. ing operated ^om a reciprocatingpart of the juice-pump, reducthe

such as is used in speed, if need be, by a mechanism pumping oil to a bearing. The vertical- or outlet-hole in the plunger is made the cutting of the small to reduce packing. device

A

heavy

wire

bottle. the

that may

be used

under

from

the

stream

should

be

given

leading wire

The

delivery point. It is

trash and

favorable

is

a

juice to the samplesharp upward turn at

of a

to

necessary

keep the wire free

of

cient large enough to conduct suffijuice to minimize the evaporation error. An undershot water-wheel, just dipping into the juice and driven by the current, may be used to sample from a canal. The

further

it should

conditions

axle of the wheel

should

sample spoons

be tubular

which

should

and

to

serve

be hollow

and

spokes should

take up

a

a

few of the

spokes

through the axle with the

communicate

hollow

The

jar.

be

terminate

littleof the

juice and

in small deliver

it

throi-ghthe spokes and axle to the jar. Coombs' drip sampler, Fig. 51, may be used if the juice is As is shown in the figure,a small thoroughly strained. of juice or other liquid is led through a glass T-tube stream and of the tube by properly adjusting the side branch a small stream of liquid is diverted through it to the sample jar.

Samples acting pump The

be drawn

may

by

valve

should

pressure

at

means

be

each

from of

a

discharge-pipeof a direct spring-controlledrelief-valve.

adjusted to pump

the

open

stroke.

at

the moment

of

est high-

EAMFLING

The

as

difRcultywith

most

is their hability

to

their sampling

to

and

paaaing them under

sample canal

into

Calumet is

with

canal

the

of

samplers It

draw

and

are

^th

samples if the

a

mills

When

this

sampler

from

the

crusher

it is usually

to

hand in

and

and

the

should are

be

small

one

a

when

it

and

is

ia connected

sample

is from

good approximation

very

Almost

The

all mechanical

the

mixed

juices

to

of juice at regular intervals

sample.

defecators drawn

its

pump

a

drip samplers.

sampling

composite

a

a

from

flow.

sample

correct

latter.

leading

average

an

drawing

from

form

defecators

when

line

measuring-cupful

is used

drawing

liquid

of

quantity

dischai^

necessary

these

the

the

superior

small

foul, uncertainty

to

several

representative sample.

is often a

system

a

e.g.

juices from

part ol the juice, but

a

to

necessiurilydraws

with the

clog, tendency

conditions,

the

sampler

by

met, erfthese samplers, except the Calu-

the probability of not

which

operated

205

JDICE.

in proportion

certain

connected

only

THE

are

whoii

If the

large,two fillingeach

defecation small

ured meas-

tank;

sample will suffice.

but

If the

206

GENERAL

juice flows into Bimilar drawn

ANALYTICAL

Urge

processes, the

as

in the

ttning-tanlui,as or

one

tank

WORK.

is

samples

should

enunple,

when

small

more

for

filling,one,

has

tank

three

a

into

juice is

small

sample

the

Horsin-D^oii

below

for the

the

the

The

"

of

juice to

in

on

DiffustOB-

diffusion

means

of

with

juice the

a

by

Uorsin-Dten

52,

cock

consists of for

suitable

a

connecting alternately

measuring- tank

and

float.

measuring-tank.

of juice drawn

dmw-

sample

stand-pipe

the

is operated by the

measurement

apparatus

small

each

meaaur-

the automatic

the

three-way

of

from

small

a

This

ing of

This

process

measurement

sampler, Fig.

the sample

preserva"-

farther

juice, drawn

facilitates

that

other

in regard

Sampling

ing-tank.

arranged

the

the

given

diffuser, in

BO

density

samples

requires the

placed inEide

the

be

207.

Julce.

is

should

and

for

are

102.

sampler

work.

observations

page

The

described

polarization.

of

them

by

siicilar

a

as

for

Methods

the sample-bottle and

or

samples

determination

a

drawn

be

for difFu"on

one

the

to

defecatora,

sampler

drawn,

pumped

flows

may

Duplicate

62.

when

or

the

automatic

Flo.

second

first

it

liming-tanks,

,

feet of

measuring-tanks,

which

from

and

the

nearly filled.

If the

tion

be

four

or

juice in it,and it is

and

Deming

It

is

is proportionate

PRESERVATION

battery should

the

from

in the

quantity of juice

the

to

OF

enter

207

SAMPLES.

tank.

the

The

discharge-pipe

measuring-tank from

the

sampler should be directlyover the battery, if practicable projecting a short the inlet from distance into the pipe. If this precaution is not observed, sample

the

inlet to

The

bottom.

be

not

may

the

representative of the

tankful

of

juice. Care

103. "

^In order

infection

of

that

and

Preservation

Samplers.

of

sampler itself may not be the decomposition of the

the

Samples.

a

source

of

samples, it be kept thoroughly clean and be frequently sterilized. must of a steam-jet is usually the most Cleansing by means and efficient method. All sampling devices convenient should be thoroughly sterilized several times daily. The cause

with hot after each water sample jars should be washed The chemist be thoroughly dried. should and use fully realize that in analyzing samples that are improperly drawn leading eared for he id wasting his time and is obtaining misor

results. measured

Where

at intervals by the samples are drawn be conveniently stored in wide-mouthed,

workman, they may glass^toppered jars. The in perforation

it to

stopper

should

prevent sticking when

have

small

a

the

temperature size for the jars is three of the factory falls. A convenient the mouth should be fully13 cm. Mters and (5 inches) in is to obviate the The object of the large tnouth diameter. from of a funnel and to prevent the workmen use spilling juice on the edges of the jar. Small metal-cups, with long for measuring the samples; The handles, are convenient the number size of the cups depends upon of tanks that are filled and

10-15

These time of

daily; usually cups

before

a

3-5

cc.

cup

for the

sucrose

sample

the

suitable sizes. density sample are should be thoroughly rinsed with juice each drawing the samples, and after the addition

cc.

samples the

for

contents

of the

jars should

be

thoroughly

mixed.

sampling is complicated in a factory operating more than one tandem if these are operated at of mills,especially different capacities. If the mixed-juicesare pumped through The

a

a pump singlepipe-line,

sampler of

the Csdumet

type

may:

208

be

GENERAL

with

connected

If the

juices are

ANALYTICAL

WORK.

juioe-pump and

the

be

i

operated by it.

independently from each mill it be necessary to attach a sampler to each mill-pump may and composite the sainples in proportion to the quantity of cane In some installations it is ground by each tandem. to resort to hand sampling. necessary A

pumped

be added

must preservative

samples in compositing.

to the

be Samples for use in the Brix and ash determinations may preserved during 24 hours by the addition of 0.3 to 0.5 cc. of a 40 per cent formaldehyde solution per liter of juice. also be preserved by the addition These of samples may mercuric

chloride,using

should

juice. Formaldehyde samples that

are

1 part of the

to be used

in

salt per 5000 parts of be used in compositing

not

and

sucrose

tions. glucose determina-

satisfactorypreservative of juices for sucrose oi lead. and glucose tests is Home's This dry subacetate used in the proportion is a very efficient preservative when of 12 grams a juicesample per liter of juice. It will preserve The

most

This salt must periods far exceeding 24 hours. used in excessive quantitiesand after each addition for

not

be

juice with the preservative. the sample should be thoroughly mixed of lead is used in solution,an estimate of If the subacetate of

probable volume of juicethat will be included in the days' and for each estimated composite sample should be made 100 cc. 5 cc. of the lead solution should be accuratelymeasured the into, the sample-jar. At the close of the day's work of the sample and preservative should be ascertained volume the

and

then

sufficient water

dilution 10

per

enables

use

the

cent

be added

should

of the

of Schmitz's

volume

of the

table for

juice itsdlf. This

sucrose.

preferableto composite the samples thus givingthe chemist a good control itself, It is

boys, and making regular intervals. 104. Sampling of the the press

and

sure

the

that

the

of the cake

itself.

in the

varies This

Cake.

laboratory the

over

subsamples

FUter-press

cake filter-press

the total

to make

drawn

are

"

^The

in different

makes

sampleat

position com-

parts of

strictlyaccurate

be left in the sampling impracticable since this work must The best approximations and comhands of the pressmen.

THE

8AHPLIN0

pariaoDS

are

atically fh"m The

obtained various

inatrummt

sampling. that

it may

This

latter

by cutdog

pieces

in Fig. 53

of

heavy

readily be grasped by ia fastened

209

CAXB.

of

the cake

ayetem-

parts of the press.

shown

It ia made

FILTER-PRESS

to

the body

is very

brass the or

and hand

suitable

for this

of such over

the

a

size

cover.

receptacle by bayonet

210

GENERAL

and

catches thick

and

ANALYTICAL

The

8et""8crew.

a

i inch

about

in

WORK.

is

cutter

diameter

brass-tube

a

ind'i

^

the

cutting edge. the receptacle,so

at

body of the tube is coned towards that the plug of cake will readily pass into the latter. The cutting edge should be of the thickness of the tube to prevent damage to the filtercloth. Several of these samplers should be provided so that one The

filled from

be

may

number

each

plugs in the usual

of

parts of the second The

plugs

in the

are

and

time and

formaldehyde,

with

sample should

The

is filled.

press

a

count

closing it. A

and

cover

the

after removal

a

various

and

so

on.

to

sent

holds

a

sponge

preservation of the the laboratory each

provides a check

cleaned.

of presses

cleaned

This

cut

receptacle,one remaining small tube, open at both

for

be

e.g. from

the fifth cake

to the inside of the

ends, is attached sample.

in the

should

pressmen

procedure,

cake, then from

accumulated

cutter

saturated

The

press.

on

the

sampling

The

oughly sampler should be thorof the plugs and returned to

the presses.

sample

The

fitted with be

may care

on

should

a

may

by

removing

the

piston

for

for the purpose,

employed

of risk of

account

be stored with

also be obtained

in

a

of^

means

plugs.

cork-borer

must

be

used

with

The

plugs

but

cutting the filtercloth.

covered

vessel in

brass-tube,

A

atmosphere

rated satu-

sampling of the tendency for the

press-

an

formaldehyde.

"It is difficult to control

or

check

the

cake, especiallyas there is a natural men pressWith the to sample only the hardest parts of the cakes. of washing the cake the error of of systematic methods use less important as the loss of sampling, however, becomes sugar

is small.

not samples, collected as has been described, are usually separately analyzed, but are composited, preferably

The

during six-hour periods. Each time that a filled receptacle is received by the laboratory, the plugs of press-cake should and chopped into fine pieces and be thoroughly be removed cake from each A measiu*ed mixed. portion of the minced hyde. t^ressshould be placed in a jar in an atmosphere of formaldeunited subsamples should be thoroughly mixed The and analyzed

once

every

six hours.

212

GENERAL

ANALYTICAL

boilera uauaJly fill the if the

of uniform

are

p"ns

otherwise ftlt, for

one a

there

each

convenient

the

A

is sampled

or

should

determination the

of the

These

same

by

the

Sugar.

sample

a

samples

The

with

for

glass forms

sirup,and, according

eiunples from

represent

the

time

to

of

for

method

Clerget

the

definite

a

of

sample

time

the

analyzed

are

calculation

the

The

"

from

be

at

made

represented by calculating the

true

quantity

should

frequent six

every

the

at

the sugar-scale of

padcage

be

thrown

opening

aa

ite

so

hours,

and

should

tin-box

a

receive

to

samples

into

them,

obtained

inten'als, preferably

sample

sugar

M.

composite

the

number

be

recorded

as

should

analysis

an

of

packages

for

use

in

averages.

sugar

in

(Fig. 55).

The

sampling

employed

The

workman

each

funnel-shaped

a

in Fig. 54,

analyzed

In

as

by

sucrose

samples should

remove

provided

should

of

composite

prepared

drying

Sampling

weighs it.

be

way

A

Fta.

shown

for

answer

material.

107.

'should

funnel

worii, the

the

be

of

solids

purity.

tsaees,

of proportionate meaaures,

stemless

composited.

are

final molasses

and

will

measure

set

a

small

in the

of

exigendea

separately the

be

one

in such

point;

same

measure.

Holasaee to

^ze,

should

pan.

the

to

pans

WORK,

the

packages

trier

is

a

a

"trier"

is

long trough-like

usually instru-

SAMi'LING

on

being

which,

ment,

withdrawal, which

through

to

the

air

short

as

sampling

by

U.

from

sample,

except

trierfuls

and

sugar be

it

exposing

Treasury

instructions

wooden

packages

the

in

\6ng

marks,

from

taken

furnish

required

the

each

for

bags,

baskets,

of

contents

from

samples

each When

quantity. of

use

short

the

and of

class the

sample

the

packages,

the

the

mats

take

to

In

in

short

such

mark

to

to

impracticable,

will

from

be

the

of

used, central

that

manner

of

carry

sampling

trier

shall

condition

triers

the

the

fairly

packages

hard

of

a

number

equal

necessary

sugar

regulations.

and

ceroons,

exercised

hping

of

the

constitute

an

package

the

through

to

when

shall

6"

amount

of

provisions

the

diagonally trierful

one

of small

cases

trier

chime,

to

be

shall

other

Fio.

the

the should

sample

limips,

S.

and

putting chime

package

care

of

possible.

as

the

hogsheads

in

sampled

out

This

all

time

a

are

representative

passed.

will,

sugar,

sugars:

''Sugar

of

has

reducing

following

The

be

it

of

quantity

a

sample

a

mixed,

thoroughly

into

plunged

remove

213

SUGAR.

be

the the

the

uniform

in

renders

sugar

knife

may

be

used." The

Treasury

packages

in

formerly.

a

require

regulations lot, instead

This

conforms

of to

a

certain conmiercial

the

sampling

proportion usage.

of of

all

them,

the as

OF

ANALYSIS

The

SUGARCANE.

Sucrose"

Direct

first step in the

analysis of the

of^the sample.

As

of the

sample with

the

of

Estimation

108.

THE

cane

milling

the

be

can

and

process

impossible

almost

to

has

been

Method.

is the

cane

shown

a

without

tion prepara-

representative

in diffusion

obtained

work,

special apparatus

accomplish this.

With

"

the

usual

but it is

facili-

FiG. 56.

ties,such neither

as

be

it should

be

sample

the

that

In the

to

of

state

sucrose.

noted

parts of

of the

shears, the

or

suitable

a

of the

extraction

Whole

knife

prepared rapidly enough in

nor

different

a

avoid

division

the

cane

can

by ation, evaporfor a thorough

error

analysis of whole

composition

stalks, thus

of whole

varies

canes

greatly in

complicating the

tion prepara-

sample. cane

can

be

rapidly and

properly shredded 214

by

ESTIMATION

OF

"

THE

215

StJCROSE.

""

essential Hyatt's eane-reducer,*Fig. 56. The machme a jvaumoei are cylinder,carrying parts of staggered or ''drunken" the saw^iisks are parallel saws; of

fneans

this

of

to

another

one

and

arranged to press the the machine, the saws of

account

on

the

machine-

The

fingers. A against the saws.

to

driven

at

throws

the

is

feed

operating

into

box

a

of

part

every

hair-like

and

cane

the

high speed, and

blades

the

prepared

Li

very

a

fine SBW-di"st

a

forced

or

staggering of

the

is reduced

cane

canes are

bearing lightlyon

them,

vibrators

steel

cylinder, are

between

fibers.

wiiere it

protected from moisture. With tlie author has' readily a laJrgeHyatt machine almost of the cane obtained in an coniplete exhaustioo diffusion work on a manufacturing scale, with very little dilution of the juice. In many remaiiiing tests, the' sucrose is

of the

cent

per

fnnn

residue

in the

For

weight of the

proceed' as

follows:

dish

Place

and boiling water off the liqtHd and

with

tions

during

add

another

in all

water

the

residue' in

the

portions of solution

liquid and To

100

lead

cc.

for

in

of this solution

of water,

these

after- the

clarification and

of

drain

diges-*

last press

from

the

determine

chips. Cool the its

degree Brix.

sugar-fiaskadd subaeetate 110 to complete the volume a

of oc.

filtraition

thorough mixing and

After

oc.

a

powerful press, uniting

other

ako

cc.

Repeat

times, and

drained

it and

weigh

in

minutes; oarefuUy

ten.

portion of -200

hydraulic or

a

cane

"^

minutes.

seven

0.07

whole

prepared eane approximately 200

add

ten

than

more

in the

sucrose

grams

boil

again digest during

and

never

cane.

100

.beaker and

or

was

of the

direct estimation

the

suitable

diffusion

the

polkri^e the filtrate, observati"m-tube. Divide the polariseope using a 600-mm. reading by 3, since a triple-lengthtube is used, and calculate' in the solution by Sehmita's the yer cent sucrose table, page

506.

Froto

the per

cent

weight of the latter,oakuldte nun^ber is the weight of sucrose f

^roentiageof

1

This

sucrose

macluDe

the Bffure and

it is

in the

ho^s Teoently now

known

the m

cane.

been as

in the soiiitioh and

sucrose

the

the

wieight of isudxise.^ This 100

grams

of

cane

or

the

"

somewhat "

modified

Warmoth-Hyatt

from cane

that

of

reducer."

216

ANALYSIS

of

Estimation

109. Methods.

Indirect

Sucrose.

the

laboratory control of the sucrose estimated factories, was by applying cane-6Ugar in the normal the percentage of sucrose juice to its weight In

"

derived

as

Francis

^

the

SUGAR-CANE.

THE

OF

called attention

experimenters have juice varies in the contains

water,

is almost

or

will

that

of the

of the undiluted

to terms

quite variable

and

analyses,in which The

cane

a

and. be In view

slowly pressed,

tions of these considera-

the tise of

juice. This

a

of the

sucrose

factor to reduce

factor

is

necessarily be placed upon

it is used. is discussed

method

above

the

by Soheibler, that piece of a stalk of cane

great reliance should

no

that

indirect estimation include

must

cane

If

hand-mill

an

ing assum-

water

the free end.

dripfrom

in

H.

other homogeneous. Many that the composition of the

colloidal sugar.

O.

100.

.ofthis method

part of the stalk and

same

small

a

it is evident content

also shown

termed

into

from (fflber)

error

to be

cane

of

marc

to the

quite free of

entered

water

days

by deducting the

juice of the

the

be

earlier

here

on

account

of

its

chemists and its bearing upon by many iQethodsof stating of mill-work. tike.efficiency of many As in the beet-sugar industry, it is the ""istom chemists factor from to deduce a experimental data, corresponding to the percentage of normal juice in the cane, and in calculatingthe sucrose by the indirect apply this number use

'

method.'

In order that

experimental data in

must

the

be applicable,the factor may be obtained under the same milling

such

a

extraction

of

the

juice sample upon the calculations. Such base which to factor can a only be" properly calculated froan data obtained by actual experiment deduced with the factory mills and when is so even but an approximation, since the composition of the cane is constantly changing. The following is the customary and probably the best conditions

as

in Working with analysis of the cane satmration. is taken without The weight of the cane department; the weight of mixed reported by the cane method

^

11th

The

of indirect

Royal

Agrioultural and

June, 1885.

Commercial

Society

of Britiah

or as or

Guiana,

FIBEB

WOODY

diluted

OR

217

MARC.

ftllthe mills is ascertained

Juicesfrom

by

direct

and calculation by the laboratory; by measur^nent the weight of bagasse is estimated by deducting the of the weights of weight of the diluted juice from the sum

weighing

the

is determined saturation-water; the sucrose festly juice and the bagasse by direct analysis. Maniand

cane

in

or

the

the

the

weight

weights of

of

is the

cane

of the

sum

in the

juice an4 bagasse, and this number and multipUed by 100 by the weight of the cane

divided

sucrose

gives the percentage of There

several

of the

water

parts with

more

that

less moisture

or

and

measures

conditions

mills; there

the

through

in^the cane.

sucrose

lead

inaccuracy method. The juice may be diluted by leakage used in cooling the mill-journals;the bagasse

are

in the above

where With

in the

sucrose

may

analyses. The modem

mills of

the old types of

may

to

by evaporation in passing be inaccuracies of weights,

first of these

good

need

construction

pected ex-

operated.

are

mills,however, it is often

be

not

to

necessary

bearings and a part of this is Uable to leak into the juice. Such leakage may usually very be detected relation between the the by noting percentage cooUng

run

water

saturation-water

of

the

from but

is

the

upon

and

the

evaporation of the

probably usually

number.

dilution moisture

be

cannot

in

The

error

eliminated,

given millingweights, sampling and analysis

very

Inaccuracies

constant

a

of plant. are usually avoidable. Inaccuracy in the measurement or weight of the saturation-water,which is used in calculating the weight of the bagasse, should be avoidable,but is a frequent of

source

The

error.

impossibilityof accurately sampling

usually precludes the factory control,hence given preference. 110.

The

the

Determination

samples a

of

canes

analysisin

just described should

method

of tlie

should

be

of the material

50 grams

Stretch

of the direct method

use

whole

to

piece of washed

be

Fil)er or Marc. Woody Transfer finely shredded. very beaker of 400 cc. capacity. a tared linen

"

over

the top of the

beaker,

An fastening it in place by a strong rubber band. opening should be left in the linen,opposite the lip of the beaker for

replenishingthe

water.

The

linen

is

designed

to

serve

218

Digest the cane-shreds

filter.

a

as

each

with

distilled

warm

pouring

off the

washing

back

adhere

to

solution into

the

water,

cane-shreds

and

further

loss of weight,

in

residue

time

beaker

the

not

hotter

of ten

minutes

than the

through

75**

C

linen,

and

of

fragments digestionswith

the

that

cane

water,

warm

minutes

each, in

off the

before.

Dry

an

liquid

as

100**

at

oven

until there

or

Use

times

five times, of ten

boilitig water, pouring beaker

two

,

each

filter. After

the

digest the

is

the is

C, until there

slightgain

a

no

the

over

smaller

weight in the calculation. weight of the residue multipliedby 2 is the percentage

previous weight. The

of fiber The

dried

a

the

in the

marc

or

cane.

fiber and

rapidity;therefore in

SUGAR-CANE.

THE

OF

ANALYSIS

desiccator

Preparatory

to

the

and

linen

attract

beaker

and

the

weight

should

Special apparatus

be

placed be

should direct

of the

one

on

employed

reduce

or

brass.

bagasse

is

form

made

The

diametel*

and

provided

to

body

gauze

material.

of Soxhlet*s

i!|J

hold from

bagasse FiQ.

57.

quantity of

shredded

The

above The

or

chamber

bottom

the

are

bottom

of a

80-mesh

wire-

is of

same

grams

the

this size will of shredded

larger weight of below

in

cylinder, B,

cylinderof a

inches

3.5

cylinder has

of

50 to 100

tractor ex-

of thiti copper of the extractor,

a

the A

Fig. 57.

support

cover

and

in

venient con-

long. Lugs

extractor.

removable

A

12 inches

inches

3

quired. re-

in order

error.

i4, is approximately

the

frequent are

is shown

simple

a

and

about

balance-pans.

be

sampling

apparatus is

proximate ap-

capable of comparatively large

cane

the

cooled

possible.

as

where

should

with

quantities of

or

be

fiber-determinations

operating

This

extreme

residue, their

and

This

to

quickly

as

beaker

with

should

contents

weighed

then

weighing

moisture

the

cane.

lugs is

to

A weighed provide drainage space. cane or bagasse in the cylinder B is

220

ANALYSIS

the

give

train The

the

per

78

per

=

11.72 The

method

agreement

then

cent;

the

per

fiber

cent,

per

has

writer

with

(1)

by

factories

purity

in

cent,

the direct

under

two

a

calculated methods

his

in

mill

in

indirect the

bagasse,

juice

purity, 100 "

bagasse;

25X.4687

cane.

number

fiber

superyision"

last

juicensolids;

the

large

determinations

purity

juice.

residual

the

is

the

second

sucrose

in

in

marc

or

the

from

The

residual

percent fiber

juice.

deducted

of

cent;

from

residual

bagasse.

the

25;

per

compared the

the

of

bagasse, 48

the

of

bagasse-roll that

calculated

moisture

the

4-T-.78a"5.13

=46.87

the in

of

the

is

illustrates

moisture,

cent;

be

example cent

bagasse

fiber the

from to

the

and

of

considered

Per

(6.13+48)

solids

juice

following

method:

and

sucrose

flowing

is

in

66lids

percentage

juice

the

the

the

of

sum

100

4

of

percentage

The

of

Juice

oi

percentage

SUGAR-CANE.

THE

OF

so

of method

by good of

analyses

fiber

(See

(2).

that in

also

he the

158t)

has

by The continued dis-

bagasse

ANALYSIS

Determination

111. of the

juice is be

may

used.

calculatingthe determined

as

be

may.

on

the

by

the

converted

table

of the

into

the

minutes

of

half

degrees

the

used

are

in

page

on

specificgravity pyknometer,

or

Brix

scale

482, according

by

means

to the

be

juice

floats,taking

ard stand-

not

care

in 94

and

help

to

juice

reach

of the

illustrated

and

juice should

that

be noted

for

suffice.

overflow

to

mechanical blow

above

the surface

on

the

froth.

The

juice,imtil it point to which

for the

juice, read

and

impurities,

the

remove

allowing sufficient time

few

a

cylinder, after the

the

farther; into the

the stem

to wet

from

minutes

ten

It is well to

be lowered

spindle to

directed

into

froth

siuface.

now

After

it sinks.

usually

lowered

it overflows

as

varies

required for this

it the

the

spindle should

of the

balance

hour, but

an

with

floating upon

of the

the

scale, or

bubbles, causing the

the

away

of the

convenient

more

readings

Westphal or

balance

purity.

Baum4

time

spindle should

carry

Westphal

spindle is the fiince its

hydrometer

an

selected.

The

to

escape

the

density

hydrometer, fill a wide cylinder to the brim of sample of juice and set it aside for the escape

air-bubbles.

The

of

means

or

The

the

using

with

Brix

477

page

on

temperature In

The

by

(96)

coefficient of

readings

Density."

determined

for this purpose,

hydrometer The

the

pyknometer

a

JUICE.

THE

of

usually

(94), though (95)

OF

temperature the

scale

as

The

in use

temperature Fig. 47. in correcting the observed

density. The

temperature

normal For

is

17i**C. is

example:

density

and

Let

correction made

18.15"

temperature.

with Brix

using

when

the aid of the at

24"

Referring to

C. the

spindles

table, be

the

table

whose

page

480.

observed of 221

correo-

222

ANALYSIS

OF

THE

JUICE.

tions, under the heading "Approximate degree Brix and the column Correction/' follow down 20, the degree Brix nearest 18", to opposite the temperature 24" C, and take off the

correction

been

making

to

Had

corrections

the

20"/4"C.

The

is given in page

ture temperabeen

have

is used

instruments

for

fj

18.15, mak-

degree Brix, C, the correction would Similarly,the table on page 490 18.59.

tanperature

in

standard

comparisons fot these instruments

table of

j

477. of

Determination

11^.

added

17 J "

below

subtractive.

at

be

must

corrected

the

ing

.44, which

the

Trne

Brix

Degree

or ^

Solids

Total

Prepare pumice-stone in and

sieve

Ir-mm.

the

thick

mm.

for bottles

the

on

pass layer of the

a

of

bottom

a

small

Method,^

size should

One

should

other

convenient

are

sizes.

two

perforations. Place S

Carr and Saiibom^s

by Drying.

a

I

"

pass

a

cular sieve,cirfiner pumice-stone 6-mm.

metal

dish ; lead

caps

inexpensive for this purpose.

and

thick pumice-stone 6 to 10 mm. such the first layer. Add a quantity of the juice to upon the tared dish and pumice-stone as will yieldapproximately In weighing the solution 1 gram of dry raattcT, a use weight in a waterweighing-bottle, Dry to constant hours. making trial weighings at intervals of two oven, in a vacuum-6ven be conducted The at about drying may of materials containing much 70" C. in case readilyoxidizable Place

layerof

a

the

coarse

mafcten

The used

divided by the weight of juice weight of dry matter and the quotient multiplied by 100 per cent of total

j

"=

solids. Method to

^This method using vacuum-apparatu3. from the author by that of C5ofurtonne,

differs in the Courtonne to

the water The and and

was

"

construction

heats

prevent

the

of the

bottles

the return

oven

in water, and

gested sug-

which

it

and

drying-bottles.

and

makes

re-evaporation,of

no

a

vision pro-

part of

i

of condensation. is shown

in

section,in Fig. 58, and thtt bottles double trap in perspective. The walls of the oven are filled with plaster of Paris, C; the bottom is also are oven

*

Bull.

46

Div.

Chemistry,

U.

S. Dept.

Agriculture,

p. 45.

DETERMINATION

double, and by

a

inside

OF

the

space

toy steam-engine the

oven

and

THE

TBUE

is filled with or

other

insures

a

small very

BRIX.

DEQBEE

air.

A

motor, unifonn

223

fan^ D, driven agitatesthe air temperature

in

all

paortsof it. The drying-bottles.A,

tubes

with

are

connected

by

means

of short

nected vacuum-pipe, E, which is in turn conwith an ordinary filter*pumpor other vacuum-pump. Each bottle may be r^oaoved by closing a cock G without at the disturbing the others. A small glass trap, H, shown right of the oven, in detail,prevents any moisture, from a

central

Fxo.

condensation

in the

tubes,from

58.

fallingback

into the bottle.

followingprocedure is advised: Dry a small quantity of piecesof pumice-stone in (me of the bottles;tare the bottle of and then distribute a weighed quantity oi about 5 grams The

All weighings should the stone. be made with juice over Insert a rubber the glass stopper in the bottle. stopper, with in the and the bottle neck of a glass trap, H, provided it with the vacuum-pipe, E, by means of a rubber connect tube. Heat the oven to 100" C, keeping the fan in motion. of 20 inches is usually sufficient. The calculations A vacuum as in the preceding method. are made

224

ANALYSIS

Materiab

JUICE.

THE

OF

containinglevulose should be dried

at moderate

The preferably in a vacuum-apparatus. risk of decomposition of the levulose is lessened if nearly all the water be driven off at a low temperature before heating

temperatures,

expel the last of it.

to

A

Convefiient

Vacuumroven,

^A conv"iient

"

apparatus

for

device shown in is the distilling drying materials in vacuo This consists of a glass dome fitted to a porcelain Fig. 59. with rubber vessel, the joint being made a gasket. The steamporcelain vessel is fitted into a special wateror bath.

Connection

by

bottom

means

of the of the the

under

of

and

dish

dish

A

bath.

capsule 85

factory^svacuum-system

pressure-tubing.The dishes

vessel porcelain

outlet

The

the

59.

Pellet's Method

center.

with

FiQ.

similar to that in

nickel

is made

heated

are

should

not

be

rest upon

the

to the

temperature placed directly

except this be provided with

water-trap

a

Fig. 58. for mm.

has

Total

Sdida.

in diameter a

central

"

Pellet

and

20

mm.

uses

a

deep

depression about

shallow at

the

one-third

depth of the dish and one-third its diameter. Freshly ignitedpumice-stpne,ground to pass a 1-mm. sieve, the border of the capsule,leaving the is distributed around central depression free. The capsule,including the pumiceand a small glassrod, is warmed, then cooled in a desiccator stone The material to be tested is placed in the and tared. depression and the dish is reweighed. In the case of juice, the

total

BEFRACTIVB

10

grams

This

be used.

may

distilled water

225

INDEX.

diluted with

is then

little

a

the

by by tiltingthe capsule it is absorbed distributed is now stone pumice-stone. The evenly

over

the entire bottom

and

etc., the material

of the

(about

testingmassecuite, grains) is weighed in the central

3

capsule.

In

depression and is then dissolved in about This

water.

solution

is absorbed

5

of hot distilled

cc.

by the

stone

and

is followed

with two additional manner successivelyin the same small portions of water. The rod is used to promote solution.

Finally the is dried added

is distributed

stone

in the

drop

A

oven.

to material

containing even method, Pellet makes

In another to which

sugar

tested

added.

at intervals

weighed

dish is assumed

other

Jossers Method.

"

is

time.

to

capsule containing the

The

and

it

when

pure

to be

is

sugar

to lose moisture

ceases

the

to contain

only dry matter. ^This method was originallyused

agriculturalwork. time

a

be

of

equivalent to that in the material

water

has been

should

acidity. paralleltest, using

trace

a

material

the

of ammonia

two

or

and

before

as

It has

slightlymodified

been

modification

The

in

of

from

Weil

and

Tempany

tain cer-

^

given here. A

No. stripof S. " S. filter-paper,

rolled into 2

X

a

tightcoil and

cc.

is placed in

a

cm.X2

58

is

cm.,

weighing-tube 12

cm.

thoroughly drying the paper, the tube is removed and weighed. The stopper is now

After

cm.

stoppered and 10

597,

of

juice is distributed

stopper removed

is now

over

paper.

placed in

a

The

tube

with

the

drying-chamber contained

chamber is heated with steam-jacket. The steam, while a current of air,dried by passing it through sulphuric acid, followed by travel through calcium chloride,is drawn ber through it by an aspirator. The moist air leaving the chambe passed through dr3dng-bulbs and the water be may collected and weighed as a check. Stop-oocks are arranged in

a

to

control

the

the aiiw;urrent

and

mercury-column

a

to

regulate

vacuum.

113.

Estimatton

Refractive

of

Index.

"

"

W.

"

J. Am.

the

and

^Tolman

I. Bui.

1912,

Chem.

Solids

Total

Smith's

'

12, 89.

Soc,

1906,

28" 1470.

from

the

investigations

226

ANALYSIS

showed

that

most

Geriach's with

found

that

the

Main, and closelywith

The

tables

GeerUgs, after another.

one

solids in

examination

materials

low use

of

solids.

as

correction

to

the

material

is

soUds

only

under

included

limitations, i,e,,in and

solids

agree

is affected

this is not

in

Smith,

and

Tolman

its

the refractometer

indications

accurate

He

refractometer

if the

Within

containing only soluble of non-sugars,

the

refractometer

insoluble matter

of the

^

acciu*atelythe products. Geerligs

temperature

The

Main

in refinery work.

solution, therefore

contains

in the estimate

very

first to

used

indicates

index

the

factories.

cane-sugar

by the

were

that

be

may

temperatures.

room

in all but

matter "

West

van

from

refractive

of soUd

content

and

hydrometer ccurections

the refractometer

use

equal percentage

refractive indices, also

same

to correct

error

the first to

was

the

table of Brix

small

in ^^solutionsof

sugars

composition have

JXHCB.

THE

OF

a

small

portion pro-

capable of giving contents, usually

by drying. The refractometric results with materials of low purity are usually intermediate between those by hydrometer and actual drying. The canequite

accurate

in massecuite adopt the refractometer analysis,must completely change his idea of

molasses

the suitable tiont

and

those

as

maker, in order

sugar

and

as

to

puritiesor

the

at least for

conditions

a

time.

These have

obtaining in Cuba

consideradeterred

applying the refractometer in the factories under his generalsuperintendence of manufacture. Three instruments, by Carl Zeiss of Jena, are used in the refractometric estimation of the solids in sugiur materials, the author

viz.:

from

(1) Abbe

refractometer; (2) immersion refractometer; (3) sugar refractometer, a specialform of Abbe instrument. (1) The Abbe Refractometer,Fig. 60, consists essentially of two flint-glass 1*75,cemented prisms A and B of index Nd The into a metal ing mountmounting, and a compensator. ^

be hinged at C so that it may of the liquid to A drop or two separated from the other. be tested is placed upon the poHshed surface of the fixed prism. A, and the hinged prism is carefully closed against it of

1 "

one

of the

prisms

is

Int.

Sugar Journ., 1907, 0, 481. Abt. in Chem. Archief, 1007" 15, 487.

CentnJbl.,

1008, 79 (1),80a

228

ANALYSIS

it is

range

for

suitable and

"3) The Abbe's in the

juicea

the

of

special tables

usual

instrument

and

has

dilTers from

and

the

glass forming

modified

the double

The the

interval

Tiie

comparator.

between

"

0 to

Abstracted

50

troEn

with

^"ecial

fonn

prisms

of the

the

of use

Abbe

optical nature

by

SchAnrock,

graduation

of the and

is uptm

in a

in the field of view.

of the scale read

divisions

tions Instruc-

dealers

a

quite

ai.

designed

cylindricalglass strip located

is

density.

the

this in the

prisms,

and

designed especially for

been

It has

eugar-induBtty,

a

types

of

range

supplied by

are

Fto.

having

other

T^TOcUmteler,' Fig. 62, is

augoT

instrument

JUICE.

the

than

accurate

more

THE

OF

in

percent^^ 1 per

Zeiu'

cent

inMnntiomi.

"rfdry and

Bubstanoe,

60

to

85

in

REFRACTIVE

0.5 per

'Rraduated 85

20"

Within

cent.

according

the

according

to

Main's

28"

is

engraved

or

The

62.

C,

refractomet"r The

upright

E

and

The

priamB, M,

N,

control

temperature (1).

The

covered very

prism with

dark-colored

for adjustii^ the

zero

observer

with

a

to

size in Fig. carries the

hinged telescope.

of the telescope are with

of the

Abbe

at R

window

is used

The

shown. for

arrangement

an

window

solutions.

instrument,

which

cap

is

when F

usually ing observ-

gives

access

of the scale.

Setlinn Ihe Refraelomeler. the

K

to that

This

D.

60

62.

is fitted with

the cap

is

standard,

which

hinge J

a

provided

similar

scale

from

one-third

iudependeutly

the handle are

and

temperature

in about

is fitted with an

the

60

to

the instrument.

upon

Fio.

eyepieceOK

0 table

I^e

table.

is shown

easing G, together with

The

from

mnge

Sehoiirock'B

to

229

INDEX.

"

the handle

Place B

on

the instrument the

left and

the

in front mirror

of

Sp

230

ANALYSIS

toward The

window

a

source

OF

or

JUICE.

THE

incandescent

an

of

light should

the

Sample,-"Open

electric

about

be

or

inches

18

lamp..

gas

the

from

mirror.

Applying

and

handle

B

surface

of the lower

the

JEidrop of the

place

prism with

glass rod should be used. after applying the solution.

prisma by solution

rod.

a

Close

of the

means

the matted

upon

smoothly rounded prisms immediately

A

the

that the so Regulationof the Light. ^Place the instrument of light. sides G are symmetrical with respect to the source Adjust the mirror to reflect the Ught through the frame of the mounting of tte prism M. Complete this adjustment by moving the hinged body of the refractometer as a whole. ^The eyepiece Ok Settingthe Instrument to the Critical Line. "

"

turned

be

can

of the

assistance the

the

over

and

entire range

handle

of the

First set to

K.

scale with

the

the

point

zero

of

the

eyepiece, arranging the mirror to throw a strong light. Then by rotatingK pass to the higher If need be parts of the scale,following with the mirror. the hinge, J. the entire body of the instrument turn on Up field the the certain at to a bright point middle; appears bounded by " beyond this point the bright part appears line,parallelto the division lines of the scale,which separates less intensely dark. the bright portion from more or one ness By a slightchange of the inclination of the mirror the brightof the field should be tested,while the critical line remains scfle

focus

stationary. the Scale.

Reading

Read

the cross-hairs. line

it.

crosses

In

dark

white

to

be

an

seen.

be noted

of

read

by

D

between

from

a

very

a

per

point of intersection of the point where the critical cent

be estimated.

must

the mirror

solutions,turn

over

R.

and

The

dark

and

a

very

the maker

as

brightpart has been

with

Viscous

each

of the

described

tables Temperature-correction

the scale.

Examining

until

the

field. Bring this line into (Coincidence and

of K

means

field will appear uniformly unpracticed eye and the critical line may even the telescopeand a fine limitingline will Rock

the cap

remove

with

the scale at

Fractions

observing very

eyepieceby

the

critical line coincides

the

not

^Tum

"

are

plied sup-

instrument.

Solutions.

"

Slightlywarm

the

prismsby

OF

DETERMINATION

through the mounting.

water circulating

solution

the

the

to

231

STTCROSE.

THE

Apply the

promptly make

prism and

observation. Notes

114. Solids.

is

in sugar-house materials

several

of

is due

This

make.

of

conditions

their

to

tendency

is advisable to

It

to

these

use

in

at

air-oven,the

an

same

some

moisture.

give fairly

that

and

conditions

average

If

under

occlude

to

all times.

the

is called upon

and

select methods

comparable results under

of

one

ready decomposition

to the

constituents

the

and

of the total sohds

unsatisfactorytests the chemist

most

Total

of

Estimation

^The determination

"

moisture

to

the

on

ducted drying is conweight of material,

the

!"-

the

perature temdish,and the same Eeating-period should be adhered to

size and

same

and at all times

for

a

kind of

a

given class

of materials.

A

perature tem-

"2.

/\

that is

suitable, e.g., to a high puritylarge crystalsugar is too high for a soft sugar of low polarization. The first requires a comparatively

high

temperatiu'e

occluded

perature

to avoid

the

Special

of

for

preserved with so

s

O

" "

"

low

very

"o

a u

the

off

tem^

u{

^

o

S

X

5

" -

sugar.

Sucrose.

tlie

This

Measurements.^"

applicable with

pipette,Fig. 63, is

have

juices that

lead.

subacetate

of

graduated

that

\

not

The

if filled to

corresponding with the observed (uncorrected) degree Brix, with juice, it wi'l deliver

mark,

52.096

i.e.,two

grams,

than

This

a

normal

pipette

was

carried

devised

by

C.

dealers.

stock

m

A.

in

of 5" to

25"

Crampton

and

the

"

sucrose

same

othe^

(52.096

dealers,and

the

Bpettoer,indepeitderitly and at about termed Ci'amptoa's or "Spencer's "

weights

of densities

range

Hqu*d.

the

be graduated for

two quantities grams), but it is usually 2-normal weight size,by for

weights of

normal

Evidently the pipette may

"

a

decomposing the invert

Pipette is

method been

other

Determination

115"

the

(105** C.)

and

water

to, drive

III "ft

the

uated gradBrix.

G.

It is

time.

pipette"

L.

by

'

I)

tbe

Fzo.

68

232

ANALYSIS

OP

JUICE.

THE

normal for the new be graduated to order Pipettes must which is used with the true 100 cc. flask. weight, 26 grams, These instruments, called sucrose-pipettes,are usually made with

long delivery-tube, but four inches long. With be supported by the flask

about may

chemist

free

noting

hydrometer,

Fill the

correction.

pipette draining, leaving the

while of

a

100-cc.

the

degree pipette with

Add

flask.

Brix

measurements

without .

juice to the

3 to 5

of diluted

cc.

(290), complete the volume thoroughly and filter the contents

the filtrate, using a 200-mm.

reading by

2

juice should

not

be

sufficient time

The

sucrose

the

should

pipette

by making

pipette

obviates

the

of

Polarize

polariscope The

sucrose.

thorough

age. drain-

in

connection

with

the measurement

after

observation.

of Schmitz's

that

water,

for

of the Brix

at the temperature filtration,

of the

used

be

may

dry-lead method

Home's

allowed

be

with

pipette by blowing,

the

expelledfrom

cc.

divide

percentage

This

tables, but

completion of the volume to 100 cc. be verified against calibration of pipettes should

involves The balance.

A

solution

of sugar

volume

it

dischai^e

of the.flask.

tube, and

obtain

to

sponding corre-

lead subacetate

100

to

temperature mark

degree Brix, and

solution

use

such

tl"e

in the

its observed

with

and

tube

a

analysis of a juice,proceed the density of the juice with a Brix

Determine

follows:

mix

tube

short

the

series

a

prefers

author

other

In

into

continue

to

pipettes. using this pipette

with

as

the

a

corresponding

to

a

an

in the pipette. degree Brix should be measured is correctly graduated it should deliver If the instrument

uncorrected

52;096

of the solution.

grams

advisable

It is not

these

pipettes with

liquids of a higher density than 25" Brix or of greater viscositythan cane-juice. These pipettes are usualV used in the analysis of miscellaneous samples of juiceand in the rapid testing of diluted massecuites pan

They

work.

solution 116.

Methods.

of chromic

to

and should

^The

molasses be

acid in

Determination "

use

for

guidance in the

frequently cleaned

with

vacuuma

strong

sulphuric acid. of

the

Sucrose.

General

necessityof adding subacetate of lead

to the

DETERMINATION

juice in sampling somewhat of the If

233

SUCROSE.

THE

OF

complicatesthe

measurement

sample for analysis.

formaldehyde

author

does

measured With

the

the

sucrose

agent proceed Determine

used, which

the be

the

of subacetate

solution

is

chloride

sample for analysismay pipetteor otherwise.

recommend,

not

with

mercuric

or

of lead

used

as

a

serving pre-

follows:

as

Measure

duplicate sample. the composite sample, includingthe lead solution;

subtract

the

volume

volume from

and

required

Add

Brix

of the

the

solution

calculate

juice to

calculated

the

of

lead

data

these

dilute the

to

volume.

degree

the

110

cent

total

the

of water

the amount

per

volume

from

of its

of water, and

original mix

the

juice,lead salt,and water thoroughly, filter and polarizethe The calculation of the pertube. filtrate, using a 200-mm. centage of sucrose is made with the aid of Schmitz table, 506.

page

Example showing Volume

of

Volume

of lead solution

juice and lead solution.

Volume Ten

per

of

cent

one-tenth Volume

The cent

2705

"

2580 of the

of the volume

cc.

juice

-"

of 2580

of water

cc.

125

used

juice

258

of lead solution

Volume

of calculation:

the methods

used

required to be added.

volume, i.e.,2705 + 133=2838 of the volume of the juice (2580 cc.). total

cc.

125

"

133

cc.

.

cc.

or

110

Degree Brix of duplicatesample (uncorrected) Polariscope reading.

18.0 60

'

It is advisable

acid

to

restore

to

the

acidulate normal

be present. that may is ascertained The sucrose

the

water

rotatory from

power

Schmitz

5 .

with

used to

peir

the

table

as

acetic

levulose

follows:

18, the Referring to the table (page 506), under the column nearest degree Brix to that observed, opposite 60, the whole of the polariscopereading, is 15.98; add number to this number 0.13, which is found in the small table opposite 0.5,

234

ANALYSIS

tenths

the

sucrose

JUICE.

in

be detennined

may

subacetate,as

lead

THE

completed polariscope reading. The in the juice. of sucrose per cent

the

16.11, is the

number, The

of

OP

Measure

follows:

100

sugar-flask, i.e., a flask graduated to hold add

complete the volume

usually 6-8 cc; acidulatingthe

solution

110

to

acetic

with

and

cc.

110

a

cc,

for the clarification,

of lead solution

sufficient subacetate

of juice in

cc.

100

with

stored

juice,not

a

previously

cc,

filter,and

acid, mix,

in The percentage of sucrose polarize the filtrate as usual. the juice is calculated by Schmitz table, as described above. In all juice analyses by these methods, requiring especial accuracy,

a

volume

the

lead

of the

be acidulated

should

should

correction

method

acetic acid.

with

by W.

made

be

method

This

clarification.

the

to

the solutions

D. Home's of lead

using finely powdered dry subacetate

*

due

error

and

(see 83) precipitate

analysis of the juice may

The

for the

made

be

requires no

measurements

juice. The

dry subacetate

as

lead

Home,

by

applied in the

when

of

described

is added

for

analysis of in

sufficient

portion of the juice for clarification,and aftei thorough mixirg and filtration the filtrate is polarized as usual. Approximately 1-3 grams of dry subacetate of lead

quantity

to

a

required for the clarification of

are

calculation

of the percentage

of

100

is

sucrose

of

cc.

by Schmitz's

originaltable, page 506, if the polariscopereading be divided by 1.1. 500.

page

lead

the

Schmitz's

method

This

the

precipitate in other

be used

must

eliminates

with

caution

for

error

due

processes

juices or

juice. The

to

contain

may

Home's

It may samples and

contains

so

volume

of

analysis, but it products contairing (See 84.) traces

of

damaged

much.

dry-lead method

control.

used

of

invert-sugar,owing to its reaction with levulose. contains but small Fully mature tropical cane levulose and often none at all,whereas unripe or canes

be

may

the

table,

be used does

is of great convenience in the storage of

not

little levulose

dilute

them.

in

factory

juicesin ing compositThe juice usually

that the influence

of

tLe lead

be

upon

the levulose error neglected. If necessary be may eliminated by the followingprocedure, but with the introducit may

"

Joura.

Am.

Chem.

Soc,

26, 186;

Int.

Sugar

Journal, 6, 51.

236

ANALYSIS

JUICE.

Methods.

Gravimetric

Sugars).

THE

OF

The

"

method

to

the composition of glucose tests depends upon the material, especiallyas regards the relative proportions and glucose. Three methods will be given. The of sucrose third are of general application and first and the second the juice contains but a very should only be used when few is not of glucose, which cent tenths of a per often the used

be

in

case.

Using Meissl

(1) Method lion

of

^This method

"

except juice as for polarization and

material

Prepare to the

as

the neutral acetate

that

Preparor by the

is recommended

products.

all sugar-cane

for

author the

the Solvtion,

Hiller^s Factors,

and

solution

a

of

quantity of the

of lead should

be

used.

the flask,add to the mark completing the volume on sufficient oxalate of potassium to precipitatethe excess of lead. Complete the volume, add a small quantity of dry the kieselguhr (diatomaceous earth) and thoroughly mix Before

flask.

of the

contents

Should

solution.

standing is

oxalate.

the

of

filtration should

five minutes'

since about full action

The

the

After

be

be

necessary

sufficient

filtrate not

not

ate, immedito

insure

time, filter the

perfectly clear, add

kieselguhrand refilter.

more

add

also

be

dilution as prepared without Add the minimum follows: quantity of Home's dry subacetate of lead to the sample of juicethat will suffice for clarification; follow the lead with sufficient dry sodium oxalate, in small portions with frequent shaking, to precipitatethe lead; solution

The

may

kieselguhrto promote

filter.

The

glucose

filtration and

All traces

of lead must

selection

of

a

tests is of very

comparative

tests

were

refinmes

thoroughly

and

be removed. for

deleading solutions for great importance. A large number of made the direction of the by author reagent

in the selection of methods factOTies and

mix

for

under

in the laboratories

use

his control

and

with

the

of

the

result

shows that the oxalates of potassium that present information and dry oxalic acid are more suitable deleading and sodium

agents care

than

to avoid

time and

the

must

carbonate

inversion

must

be allowed

or

sulphate of sodium.

be used for the

thorough filtration should

with

oxalic acid.

Special cient Suffi-

precipitationof all the lead

follow.

GRAVIMETRIC

237

METHODS.

The next step in the analysisis the estimation of

suitable

a

mined quantity of the material for the test. This need be deterbut once in the manufacturing season, and afterwards be readily varied as the maturity of the the quantity may advances. cane Prepare a series of large test-tubes by adding

above

and

4

1, 2y 3,

5

of

cc.

the

successively. Add

(!397)

to the contents

about

two

Measure

times

20

this tube

tube

and

described

as

Soxhlet's

heat

to

solution

boilingduring pare Com-

precipitatesto settle.

supernatant

the volume into

contained

with

mark

of mixed

cc.

the

prepared

liquid in each tube and has the lightesttint,but is distinctlyblue.

which

that

note

Allow

of the

color

5

of each

minutes.

the

solution

of the

flask and

100-cc.

a

deleaded

solution

dilute

that

it to the

3 is selected; No. example: Tube of the originalsolution,or if the second method 3X20=60 cc. of preparation is used, 60 cc. of juicein 100 cc. The volume be mult' plied by its specificgravity of juice measured must

ascertain

to

For

water.

its

on glucose-pipettes,

the

these measurements

making

in

provided

It is convenient

weight.

to

Spencer's

use

in principle of the sucrose-pipette, (115). These pipettesshould ibe

series of

The four, advancing by 20 grams. calibration of the pipettes should always be checked against of known degree Brix. a solution The

a

Reduction

let's solutioa 25

of the

cc. cc.

to

the

alkali

of the

cc.

solution,into

solution.

Measure

"

copper

400-cc.

a

50

of Soxh-

solution

and

and

add

beaker

of the beaker

the contents

Heat

cc.

perature boiling-point,taking four minutes to reach this temand continue the heating with very slightebbulition

during add

Oxide.

(397) i.e.,25

of the sugar

50

Cuprous

to

minutes.

two

100

At

the conclusion

of cold recently hoUed

cc.

of the

heating-period

distilled water

and

diately imme-

filter and

collect the cuprous oxide,using one of the described farther on in connection with the various

methods processes

All

the

of

the weight ascertaining

details

of the

method

and

conducting the reduction

that

the

results may

of copper.

of

preparing the

solution

to strictlyadhered be comparable and approach the absolute must

be

The beakers should be of Jena or gluc6se content. similar glass, and all be of one size,preferably not larger than

400

cc,

and

of uniform

thickness

and

diameter;

The

238

ANALYSIS

boiling should addition The

and

of cold water and

"

The

crucible

of

and

filtration

the

the

filtration than

(a) Provide

the

Joint

and

used

suitable

of

The

the

of

and

washings funnel

i inch

These

The

at

The

rubber should

cross-section.

be The

a

cost

rings

are

of pure

funnel

of

the

results

and

65.

the crucible itself filtration.

by

few

a

of

carried soft

the

of

funnel

prompt

walls

upper

edge

The

readily made

be

holder

thorough

so

care,

otherwise

prevent

may

Bugar-factory mechanics entjrely satisfactory.

Mse,

With

Sargent

upper

Fia.

be of the proper

any

size.

quite

satisfactory.

are

with

the entire porous crucible be thtvmay

crucible, but, with

dealers.

.

funnel

permit

not

washing

parallel.

use

of the Spencer

be

may

of the

doee

be

Other

given tot

are

oughly washed.

Spencer

crucible, ^

Gooch

modification

a

funnel

wall

brass

of the

the'analy^s.

of

the Spencer

the

rim

dum Spencer funnel (Fig. 64) or Sargent's aluncnicible-holder (Fig. 65). The

a

60"

will trap

Metailic

to

ware.

funnel

must

prompt.

the

at

the

alundum

latter is

holder

be

filtering crucible

with

stage

with

of alundum

in the absence

alimdum

as

this

should

Caiculaltan

or

bottom

He

only Juat appuent.

the

of

simplified

greatly

methoda

but

of making

of

JUICE.

Redvd,Um,

method

instead

THE

violent

invention

Spencer'a

have

be

not

FiUration

Copper.

OF

of

one

cents,

the

funnel

in stock

rubber, and

is placed in

a

the

and

is

must

by of

A

the

about

suction-filter-

GRAVIMIlTRtC

ing device

such

flask

meyer

with

filter-pump with

the

of their

The

a

of

should

copper

washing

with

only

be

"

Alundum

uidyticHl lose

weight

of

lamp

a

with Ui

preparatory should

copper

be

68,

in nitric acid

washed

with

and

itself

be

followed

crucibles work vety

ol

on

the

slowly

msy

be

(sctory ia

Bubojtide

to

in the

hot

half

filled about

may

reduction

is collected

distributes

washing

the

after

precipitate

thoroughly

on

tborou^

water.

Immediately this

washed

thoroughly

metallic

or

by solution

use

be

in the flame

Fia.

aft"r

filter-pump

efficient

very

a

The

multiple-effect evaporator,

require

be dried

oxides

removed

by

communicating

pipe

a

Erien-

heavy

a

is obtained

suction

through

the

crucible

and

The

DSe.

ot

The

in

or

large filtering area.

alundum

water

tubule.

preferably

or

enicibles

'

account

hot

side

vapor-pipe

alundum

in Fig. 66,

is shown

as

239

METHODS.

alundum

full

during

the

walls

by moistening for

tubstituted sad

due

to

The

crucible.

the

oxide

platinum the

in

and most

laborHtoriea. aetion

and

is

should

the

acricultunil

glucose work,

crucible

filtration. of

copper,

crucible

The

water.

of

of the

oxide subThe cru-

of tfa" These

alkaU.

240

ANALYSIS

cible with

pure

crucible

an

in

OF

alcohol oven

JUICE.

expedite the drying.

Dry the the flame of a lamp, cautiously over is ultimately to in which the copper

or

to

according to the form Proceed by be weighed. (b) Wedderburn^s

THE

of the

one

followingmethods

of Reduction

Method

to Metallic

:

Copper

J

"

to simplest of the methods involving reduction and its results are nearly as accurate metallic copper those as

is the

This

in hydrogen. Bend and equal to reduction by electrolysis the wires of a pipe-stem or silica triangleto form a tripod crucible. Place the tripod in a support for the alundum beaker

metal

the bottom

thg

of

beaker,covered alcohol

the

beaker

with

to

alcohol

oxide

The

metallic

copper

it from

of the

plate

hot

to

necessary

in the

a

beaker

The

beaker.

after

moment

let the

vapor

the

tripod and

replace

instantlyreduced object of

be

setting

fire the flames

them

upon

and

vapor

The

take

after

removed

cool for three the

from

is to prevetat

should

with

cover

of alcoholic

should

alcohol, after

of

warm

let it cool

the

introducing the

crucible

and

crucible.

readily extinguished by blowing the

the

down

remove

faint redness

If the alcohol

fire to the alcohol.

on

atmosphere

to very

carried

is almost

of copper

in the

cooling the crucible are

Place

plate and

the flame

disappears;

firmly to the walls

adheres

hot

a

Cover

1 centimeter

serve.

been

place the crucible

cover.

will

have

may

almost

until the redness and

vessel.

depth of about

a

watch-glass,on

a

cover-glass. that off organic matter the cuprous oxide; remove the

the

metallic

condense the under its vapors side of on the crucible to full redness, to bum Heat

until

the beaker

to

Denatured

alcohol.

with

convenient

other

or

ing cover-

from

the

crucible. or

reduction

four to

It

is

minutes avoid

Should the crucible become of the copper. with pure alcohol and cold, it should be moistened

oxidation

re-

quite this be

cooling in a desiccator the crucible is weighed and the weight of copper is ascertained by difference.

burned

The

off.

whole

copper

After

plating is

Journal

Ind.

and

Stanek, Z. Zuckerind. Chem.

Zeit. Chem.

as

good

method

Wedderbum's "

but

operationconsumes

Eng.

may

Boehmen,

Repertorium,

or

six minutes

that obtained

as

Chem.

five

be 7" 610.

32, 497; 21" 324.

the

by electrolysis.

conducted Original Votocek

and

and

with method,

a

Gooch Vladimir

Laxa, Abatract

is.

GRAVIMETRIC

crucible, but may

ehow

this

from

is

ware

occluded

to be

error

small

very

conTenicnt.

more

the

jui(", but

An

ash

from

and

usually negligible. The

farthra' "tfthe glucoee is ii;iven

calculation The

tiie alundum

enter

error

241

METHODS.

testa

an.

alcohol-burner. Fig. 67, ia suitable for beating

Barthel

crucibles. Method

(c) EUdrolytic oxide in

.cuprous

crucible

the

alundum

an

method, except

bum's

need

Iiet 4

tared. the

acid.

Fallow

wash-bottle

and

nitric

Should

of the

any

through

dissolved small the

'

Tbs

Coarse

of

and

in

oxide

of

52-meah

coppnr-wiie

cDnnectioQ

with

gauie

the

of

copper

be

must

used the

the

and oxide

filtrate.

drop by diop

of the

jet of the

latter hot

crucible

upon

platinum

must

be

be reduced

a

and

this

100

re.

aetvt

platinuRi

1 inch

as

wire.

a

be

to

a

Deporit as

gauze *

a

filtrate

filtrate

platinum-gauze probably

from

the

approximately

nould

acid

method

Transfer

wetted

thorou(^ly.

the

repass

are

water

conveniently

may

oxide.

electrolyticallyupon

cylinder

a

remain,

it to

in Wedder-

washing

fall

Wedderbum's

the

dilute

with

walls

oxide The

as

copper

beaker

a

red

instead

copper

Form

the

the crucible.

metallic

to

acid

the

67.

the a"id

wash

described

After

oxide, being careful that all parts the

by

as

Collect

receiving-veeselfor

Fia.

the

Soiuiwm."

glass funnel

a

be

not

of concentrated

cc.

crucible

that

thoroughly, change

very

Nilrie

in

follows: in diam-

tathode.

A

242

ANALYSIS

OF

THE

JUICE.

by 1.5 inch long. Connect the cylindersubmerged in the solution with the positivepole of a battery or use the directwill be described, and connect as lightingcurrent reduced anode with the negative pole,and electrolyse a platinum-foil eter

with

a

and

of 10 amperes

current

Rotation

minutes.^

from

copper

It to

a

time

to time

little anmionia

to

should

copper

cylinder within 10 to 15 anode during the reduction

the

should

solution

rapidity. The

its

increases

of

The

the

completely depositedupon

be

4 volts.

be

tested

for

by withdrawing a drop and adding neutralize the acid, then acetic acid drop of ferrocyanide of potassium

acidity and finallya solution,using a white porcelainplate to hold the solutions. this solution no longer reacts for copper, i.e.'y does not When the ferrocyanide is added, without when turn brown cutting to

off the

electric current, withdraw

the

acid solution

with

a

time replacing it with water. large pipette, at the same Repeat this operation until all the acid has been removed, then

the current,

break

alcohol

and

minutes. trace

a

in

then The

of acid

remove

ether, and

current

dip the cylinder in

dry

it in

be

not

must

remains.

and

discontinued

cylinder is

The

for

oven

an

now

pure

few

a

long as weighed, its deposited. so

weight is due to the metallic copper is direct current, this When the factory lighting-circuit be regulated by an ordinary rheostat or by a simple may device (Fig. 68) and be used in the reduction home-made to increase of

metallic

copper.

descent Separate the twin wires M (Fig. 68) leading to an incanis indicated in the figure them as lamp, and connect with the regulator. The body of the regulator,C, is a glass with sultube nearly filled with water phuric slightlyacidulated wire terminating in a A is an insulated copper acid.

platinum wire sealed in the tube C; B is a movable glass wire the lower which tube through end extends; a copper with a platinum wire E sealed into the of the wire connects tube

and

the upper

end

with

a

binding-post for connection

lamp. The wire D leads to the anode or cathode and of the electrolytic A to the opposite pole. apparatus A small tube is passed through the cork in C for the escape with

the

"-

ri)---

"

J. Ind.

,!,_

and

Eng.

Chem.,

2, 195,

R.

C.

Benner.

..

TIT

-

---

"

.

|"

244

ANALYSIS

platinum dish, the

THE

or

JUICE.

berrigdeposited upon

copper

platinum

a

cylinder. Soxhlet

A the

Gooch

tube, Fig. 69,

filter

crucible.

This

glass,6 inches long, into

be

may

filter consists end

one

used of

instead

of hard

tube

a

is sealed

of which

of

tubule

a

diameter for inserting in the long, of convenient such as shown in filtering apparatus stopper of a pressure Fig. 66. A perforated platinum disk A^ A\ Fig. the bottom, 69, is sealed into the large tube, near 3

inches

to

support

the

Prepare as

manner

asbestos-felt filter.

an

Gooch

a

small

fimnel

oxide

from

filter-tube

filter and

the

in

use

weigh

it.

same

Place

a

in the filter-tube to prevent the cuprous

adhering

asbestos-felt with the

its

to

moisten

Wash

all of the

described

in (a).

water.

filter

walls,and

the

tate precipi-

Dry th^ of pure dry hyprecipitate,then pass a current drogen time the through it, at gently heating same onto

-A

the

oxide

cuprous

burner, until metaUic

reduced 6d.

and may

the methods Methods Wedderburn

of

as

with

the

the

oxide

Cool

the

weigh it.

Bunsen

a

is reduced in

a

to

the

current

of

The

text-book"

Oxide

Copper

are

accurate

more

Weighed.

is

oxide.

Of

^The

"

to metallic

of reduction

electrolyticmethods involving the weight

of

weight of copper also be determined volmnetricallyby

the

method

fiame

copper

of the various

which

in

all

state.

hydrogen Fio.

for

copper

than these

the

and

the

methods

latter

methods, (a) should only be used for materials very free of organic other than the sugars. matter Method (") when carefully conducted

is almost methods.

Gooch

by forming

a

and

an

the

felt in

a

very oven

as

It

crucibles may

(a) Prepare

as

an

accurate

is obvious

the Wedderburn

as

that

either

or

trolytic elec-

alundup

or

be used.

Gooch

crucible

thick asbestos or

on

a

hot

to

receive

felt in it. iron

the

precipitate

Dry the crucible

plate; cool and

weigh

Immediately prepared is completed, filter the contents of the beaker through the the beaker and crucible, using a filter-pump, and wash precipitatethoroughly,transferringall of the latter to the crucible.

after

the

reduction

Care

filter.

wash-water

of

ether.

with*

Place

the

thirty minutes, then The weight of the

Uttle

a

of per copfiltrate. Follow

the

alcohol,then in

crucible cool

into

pass

suboxide

neither

that

particlesof asbestos

nor

the

be observed

must

245

METHOD.

GRAVIMETRIC

it in

with

desiccator

a

oxide X. 888

cuprous

and

water-oven

a

few

a

and

weigh it. weight of

the

=

drops dry it

reduced.

copper

(b) Collect

the

and

crucible

in

redness

a

muffle

furnace

Heat

or

a

oxide

the

Gooch full

to

oxidizing flame of a fifteen heating for about

the

the crucible in

alundum

an

in the

or

Continue

Cool

minutes.

in

thoroughly dry it.

burner.

Bunsen

oxide

cuprous

desiccator

a

and

then

weigh it

oxide is oxidized to quickly as is possible. The cuprous is very cupric oxide, which hygroscopic. The weight of cupric oxide X 0.8 the weight of copper.

as

=

CalculcUion

of

Hitter's Method, Cu

Let

P=the

IT

the

=

ihe

"

weight of the factor

used

sample in the

and

obtained

50

cc.

of the

determination;

for the

from

of copper

the

table

for

the

version con-

invert-sugar;

to

approximate absolute

weight of invert-sugar Z;

=

approximate

of

=

ii, relative

"=

ZYrz^

hy Meissl

weight of copper obtained; polarizationof the sample;

solution F

Percentage of Glucose

"

the

"

the

cent

per

=

invert-sugar =

j/;

lOOP "

"-

100"12=/,

,

,.

^

number

relative number

,

for sucrose;

for

invert-sugar;

CuF =

per

cent

of invert

sugar.

W Z facilitates to

readingthe vertical columns; and the ratio of

/, the horizontal columns

of the

table,for the

the factor (F) for the calculation Example. grams

of

The it (W)

of copper

of a sugar polarization are equivalentto 0.290

purpose to

ing of find-

invert-sugar.

is 86.4, and gram

R

3.256

of copper.

246

ANALYSIS

OF

THE

JUICE.

"*-.%

Then:

lOOP

8640

"95.1*/2;

86.4+4.45

P+y

100-i2"100-95.1=/"=4.9: i?:/"95.1:4.9.

By

table

consultingthe

column

headed

column

headed

Where

these

CuF

:

GnaX

meet

W

to the ratio of R we

find

"

"

o

AND

horizontal

/, 95.1

:

4.9.

which

51.2

..

per

cent ^

THAN

MORE

p.

"

FACTORS 1 PER

^ of mvert-sugar.

THE

FOR

CENT

OF

TION DETERMINA-

INVERT-SUGAR.

735.

show that this method Experiments in the determination good degree of accuracy of glucose in cane juices. (G. L. S.) "

to

factor

the

_.

=4.56

rtgg

KILLER'S

Zeitschrift,1889,

Note.

the

vertical

o.^oo

OF

I

Z, 145, and

the

calculations:

.

=

that

seen

.290X51.2

-^liT"

MEISSL

to

5 is nearest

columns

into the

enters

is nearest

150 95

it will be

be used leas than 1

may

of

with per

a

cent

DETERMINATION

247

REDUCING-SUGARS.

OF

"

(2) Gravimetric

Place Methodj using Soldaini^a SoltUionJ 100 Soldaini's solution (29S) in an to 150 cc. Erlenmeyer flask; boil five minutes; add a solution containing 10 grams of the material, previously clarified with lead if necessary, the excess of lead being removed with oxalate of potassium; boil

"

five minutes.

Having the

the

completed and

flame

boiling always

In

add

reduction,

100

cold

cc.

immediately through a Gooch in the precipitate by copper the

collect

described

oxide

cuprous

244.

in

the

use

naked

the

remove

distilled

flame.

flask

from Filter

water.

the crucible,and determine the electrolyticmethod, or filter-tube and

a

reduce

it

as

The

weight of the metallic copper multiplied by 0.3546 gives the weight of the invert-sugar. It is very exact, and that invert-sugar is claimed that this method be

can

on

page

determined

within

to

(3) Gravimetric

.01 per

with

cent

of Sucrose

Determinaiion

certainty.

and

Glucose.

"

glucose by the Meissl and Hiller method (1); determine combined invertand the invert the sucrose (89) and glucose by the reduction method given on page 188. sugar Determine

the

of

Determination

119.

Methods.

Volumetric

cose).

(Glu^

Beducing-sugars "

^Volumetric

methods

of

factories determining glucose are usually used in cane-sugar results of their rapidity,but when accurate account on very are required,the gravimetricmethods are preferable. imder the same If the analyses are always conducted ditions conof heating, of dilution,containing-vesseland method

by the volumetric methods are comparable. ^Transfer a definite (1) A Modification of Violette's Method. weight of juice to a sugar-flask and clarifyit with a solution of acetate of lead. of lead Precipitate the excess the results

"

oxalate

with

solution

of

to 100

potassium

in small

excess

and

dilute

the

Filter off the

precipitate. calculations are simplifiedby the use The of 5 grams, or A sufficient quantity a multiple of 5, of the juicein this test. iDf the juice should be used, if practicable,to give a burettecc.

reading of approximately

20

in

the

titration

about

to

be

described. The

of

measurements

the

standard

solutions

for

.

1

Trait6

d'analyse

des

Mati^res

Sucr^ea,

D.

Sidersky,

148.

this

248

Such

mort

are

process

burette

mouth-piece The

tube. a

conveniently

burette, designed

a

The

to

OF

ANALYSIS

point

at

reagent a

mouth-piece solution

shown

syphons

end

is drawn the

released.

burettes. in

ia shown

Fig.

70.

applied at the of

rubber

the

into the

burette

zero-mark

The

automatic

with

by Squibb,

the

little above is

made

by suction

is filled

JUICE.

THE

and the of

excess

the

into the reservoir, leaving

back

filled to the zero-maric.

the burette

JIL Jl

The solution

by

test

is made

(296)

9 inches

as

into

long,

a

and

follows:

Measure

large test-tube, dilute it with

10

cc.

1.5 inches 10

ec.

of

Violette'a

in diameter

of water.

Heat

DETERMINATION

solution

the

to

add

lamp,

boiling-pointover

few

cubic

249

REDUCING-SUGARS.

OP

naked

the

centimeters

flame

of

a

of the

prepared juice, and boil two minutes. Repeat these operations until the blue color almost disappears,taking care to add the juice little

drop

little-as

by or

a

two

at

this

point is approached and then only a time until the blue color disappears. After

a

the

first

boilingof

the

liquid a few seconds, after each addition. for

is convenient

minutes, it is only necessary

two

timing

the

just disappears, filter off

using

copper,

convenient

Wiley

a

portion of

a

of the

inch

for

test

filter-tube

piece of

a

other

or

form

linen

is

stretched

over

into

water

and

by mouth-suction

this tube

using

whijch

In

is of

small

diameter

tube

into

of

to

In

is

the

then

shoulder.

A

a

this

One

end is

and

dipped

asbestos,

with

of

film

a

of this filterthe tube

perforatedplatinum disk takes In usingthese the place of the linen,as indicated in Fig.71,b. the solution is filtered through the asbestos film by tubes mouth-suction and with the Wiley filter is poured from the asbestos

the

must

liquid then

and

long. lamp and

finelydivided

modification

Knorr's

a

is covered

linen

pieces of

filter end

the

suspended

from

inches

ten

wood

in

asbestos.

by

of

tied

in

bore

block

washed

place.

made

are

a,

in the flame

is softened

tube

pressed against

the

color

the

filter.

glass tubing one-fourth end

sand-glass

When

liquid to

the

Knorr-Wiley

or

Wiley's filter-tubes. Fig. 71, .

boiling.

first

A

boil

to

test

a

solution.

be

wiped expelled by

With

off the

the

end

blowing. nitric acid

Knorr

of the The

filter the

tube, and

tubes

after use,

the

should

dilute

chemists Many and place it on

a drop of the solution prefer to remove The piece of end-reaction filter-paper.

a

precipitateremains with

water.

the

center

the filtered solution around

In

whatever be

must a

in

10-per

tested cent

way

the

of

the

moistened

spot,

it.

filtered

solution

is obtained

it

This filtrate is acidulated with for copper. solution of acetic acid and then a drop of a

dilute solution

very

then

be

dipped into very thoroughly washed

with

and

be

of

ferrocyanideof potassium, 20

grams

tion colorato it; a brown salt per liter of water, is added indicates the presence of copper, and if this color appears.

of the

250

ANALYSIS

of the

more

OF

THE

JUICE.

solution be used.

juicemust be added decreases in intensity until

sugar

The

the color test carefiilly as all of the copper is reduced finallywhen very

further coloration.

followed, after

a

there

will be

no

The

be readily progress of the test may little practice,by noting the appearance of

precipitateand the color of the supernatant liquid. The test should be repeated, adding nearly enough now

the

of the

proceed

then

at

before.

as

of the

end

the

at

solution

sugar

The

all of the

reduce

to

once

should burette-reading

operation. The

calculation

copjjer; be made

is made

as

follows: TF="the

Let

weight of juicein

1

of the solution;

cc.

burette

B^ihe

reading; "-the required per cent;

X

0.05X100 then

x^

a;

is .05 gram

W

When or

.

^^^

the

=

reduces

formula

to

rc"=

"

5

reciprocalof the burette-reading multipliedby of

table

A

the

reciprocalsis given

page

on

484

for

use

"

"

100.

in

calculations.

these

multipleof 5 grams of juiceis diluted to 100 cc. for this test, the reciprocalof the burette-readingmultiplied multipleof the per cent of glucose; by 100 is the same tion, If 5 grams of juicein 100 cc. should give too strong a soludilute to 200 cc, 300 cc, etc., and multiplythe reciprocal of the burette-reading etc by 200, 300, is instead of weighed, the measured If the juicesample still be used, but the value of x table of reciprocals may be divided by the specific must gravityof the juice. Pipettes the principleof the sucrose pipette (115) may be used on the juice and obviate the necessityof dividing to measure gravityor weighing the sample. by the specific If

a

Violette's This

of each are

be avoided

may

copper

solution

and

the

of these

other

on standing. decomposes somewhat by preparingtwo solutions,one of the

of the alkali.

solutions

are

In and

used

making the

10

a

cc.

test 10 cc.

of water

omitted.

(2) Soxhlet^s

analysis and

volumetric

make

a

method.

"

preliminarytest

juice for described in (1),to

Prepare the as

252

in

OF

ANALYSIS

100

sufficient

add

water,

CO.

clarifiQation,dilute

to

200

of the filtrate add

cc.

of

lOO

cc.

100

sponding cc., corre-

of the material, for the reduction. grams Soldaini solution five minutes fiame over a naked 10

to

in

To

for

solution of carbonate

concentrated

a

filter.

mix, and

cc,

*"

lead

of

subaoetate

mix, and filter;of this filtrate take

of sodium;

Boil 100

25

JUICE.

THE

cc.

Erlenmeyer flask,then add the sugar solution,little by additional five jninutes. little,continuing the heating an an

Remove

flask,add

the

precipitateon under

Wash

are

felt in

a

Gooch

Add

Three

the

to

collect the

crucible, filtering

precipitatewith hot

longer alkaline.

no

sufficient.

usuallv

are

the

cold distilled water,

cc.

asbestos

an

pressure.

wash-waters

100

until the

water

four

or

washings

oxide

cuprous

25

cc.

two acid, and sulphuric acid, i.e.,the standardized heat -three crystals of chlorate of potassium, and gently or oxide is completely in soluti"Hi. This until the cuprous

normal

operation should solution

the

with

by difference volume use

the

a

half-normal

a

solution

lettingthe sulphate of solution

ammonia

the

ammonia

with

800

of this solution 2

of

cc.

by

solution

to

of

of

cc.

It is

Mix

200

to which

cc,

sulphate of sufficient

it one-half

titration,

the

strength

been

added

solution, against

acid

water

Prepare

of commercial

has

copper

sulphuric acid, adding the make

cc.

this

preferable to

this

Determine

water.

from

indicator.

the

as

:

for

Titrate

determine

and

up,

ammonia

act

titrating25

disappears. Add

color

acid used

fallows

as

flask.

or

reduced.

copper

concentrated

a

normal

the

of the

of copper

amount

beaker

a

alkali solution, and

standard

volume

the

in

conducted

be

until

to

the

the

blue

ammonia

normal.

titration

proceed as follows: Oool the of the copper-sulphate solution resultingfrom the treatment oxide with sulphuric acid and chlorate of potassium ; cuprous In

add

making

50

cc.

of the

addition

long

The

after

as

ammonia

lead

The

acid, but

blue

reappears

solution. color on

should

acidulation

be

with

removed acatic

Titrate

stirringthe is not

(G. L. S.).

the each

solution

saturated.

color of the

by precipitation with acid

with

disappears with

which ammonia is any is saturated, the ammonia

there

all the

When

^

half-normal

sulphuric acid.

normal

as

the

potassium

liquid

oxalate

is

longer blue but

no

reading, which Cach

cubic

is

a

faint green.

Note

the

copper

equivalent

centimeter

253

REDUCING-SUGARS.

OF

DETERMINATION

to

the

burette-

precipitated.

sulphuric-acid solution is Multiply the weight of equivalent to .0137 gram of copper. by .3546 to obtain the weight of invert-sugar. To copper simplify the calculations multiply the burette-reading by .1124 to obtain the per cent invert-sugar. General

120.

Olucose and sugar

the

of

Remarks

the

on

(Beducing^sugars).

Determination

of

Geerligs, Pellet,Edson that a part of the reducingother chemists have shown is carried down with the lead precipitatewhen subof lead is used

"

The writer, clarifyingthe solutions. acting on the suggestion of C. H. Gill,^used acetic acid to and Pellet decompose the lead levulosate in optical work acetate

and

Edson

normal and

of acetic acid in

use

cose glu-

expressed a preference for the use of the lead in preparing solutions for both glucose

of

tests.

of lead must

traces

proceeding with have

the

also

acetate

sucrose

AH

advised

afterward and

tests

in

been

the

be removed

the solution before

from

Several

reduction.

deleading agents

used

As a result of an by various authorities. extensive series of experiments recently made for the author, in the interests of The Cuban-American Sugar Co., he has or provisionallyadopted oxalate of potassium or sodium * that states dry oxalic acid in deleading. Bomtrager sodium

with

The bonate carsulphate is preferable to the carbonate. is Very generally used in deleading and of sodium

manipulation it may give good results. The experiments quoted, however, indicate that the oxalates oxalic acid are preferable. It is advisable to use a' little or very

careful

kieselguhr in conjunction with the oxalic acid or filtration. The to promote experiments mentioned

its salts

that

of

the

deleading agent

of the volume

the mark

to

percentages of glucose are be immediate. of the

Ample

be added

may

on

small.

time

The be

must

in advance

the

J. of the

3

Zdt

Chem.

a^-gew.

filtration should allowed

Soc, April. 1871.

Cham ,

pletion com-

flask,provided the

deleading agent.

"

showed

1892, 333.

for the

not

action

254

'

ANALYSIS

OP

Determination

121. Normal

Ash.

Dry

"

10

platinum dish, then temperature, and

of

the

grams

of

incinerate

afterward

JUICE.

THE

at

a

Ash.

Carixmaled

"

dull-red heat.

low-red

a

carbonates should

heat.

wei^t rise

never

ash consists

largelyof alkaline quickly absorb moisture from the air, it in a desiccator and be weighed as quickly

which cooled

be

the

low

a

The

should

or

teured

juice in a shallow the residue, first at

of ash X 10 =per ash. cent of normal In this determination the temperature above

Ask

As

possible.

as

This

incineration- may

be

accomplished

the flame

over

of

electric or An lamp, but it is preferable to use a muffle. tory. gasolene muffle furnace should be used in the factory laboraa

The

ash is

carbonated

only in research usually determined and not in commercial work analysis. It is difficult to burn sugar-house products to obtain a large quantity or sugar of the carbonated ash for analysis. The usual method^is conducted

follows:

as

The

material

platinum dish until it takes fire and swells the to

greatly and

is washed

with

hot

to the

dish and

bum

evaporated contents

to are

a

large It

out.

dish.

a

After

The

powder.

is

fflter and

powder thoroughly

filtrate is reserved

The

filter and

platinum dish and

now

to

paper

water.

The

treatment.

is rubbed ashless

an

in

sufficiently charred, it is transferred

and

upon

extracted

is

been

glassmortar

a

the flames

is difiicult to confine to the

has

material

is heated

insoluble

matter

are

for further

returned

The ffltrate completely ashed. dr3rnessin the platinxmi dish and the are

heated

then

to low

redness

to bum

off

remaining organic matter. of juice in a shallow tared Sulphatedrosh, Dry 10 grams fused silica or platinum dish. Add a few drops of pure concentrated

any

"

sulphuric acid the

carefullyover carbonized

mass

flame porous

to

moisten

of

a

and

the

lamp. converts

residue

The the

acid

and

heat

renders

carbonates

it the

into

sulphates. When a

muffle

the charred heated

temperature but

care

must

to

may

be

be

mass

ceases

redness

to

and

bum

higher than

observed

not

swell,transfer the dish for

to fuse

off the the

carbon.

carbonated

the ash.

to

The

ash,

DETERMINATION

^^^^e ash be

\'"in The in

OP

should

reheated

heatingin the

weight

is

before

for the

This

of

number

and

often

(See 136.) is shown

"

A

narrow

drilled in the walls ", holes are heavy platinum c, df Fig. 73, and

a, at

wires

inserted.

are

for

supports the

dishes

the

is

is

is

in the

cut

a

upon

heated

Fig.

72.

Fig.

73.

Fig.

74.

which

dome The

i, Fig, 74.

at

placed

and

form

tion. incinera-

during the

rest

muffle

muffle

wires

X, y, z, upon

Wj

hcde

A

These

trough of platinum-

a

foil.Fig. 72,

of

imates approx-

be determined

^A convenient muffle MujBte for Incmerationa^ is made in Figs. 72, 73, 74, and follows: as slot is cut the length of the bottom French of clay-muffle, Fig. 72, a

.

The

usage.

factor should

factory and each material.

centage, per-

stead sulphates in-

follows beet sugar

A correction

the

calculatingthe

formation

variable

very

25 per cent. for each

decompose sulphides. reduction of the sulphates

of carbon.

is deducted

a

and

to

in the

compensate

correction

sulphuric acid

"sulphated-ash" method, one*tenth

ash

of carbonates. true

256

NITROGEN.

with

muffle

formed

customary to

the

the presence

of the

TOTAL

moLstened

in

sulphides are

In

be

THE

suitable support

by

wing

top

burners.

and

Nitrogen "

of the

Determination

123.

Total

method

the

Total

Albuminoids.

termined Nitrogen. ^The nitrogen is decombustion by the moist tions, modificaof Kjeldahl with

as

"

of Official

adopted by the association

Agricultural

Chemists.^

(1) Th3

digestion. 10

capsule, xure brought approximately .7 gram The

sulphuric acid.

position,and

of the

cc.

"

into

oxide

mercuric is

heated

placed

below

on

the

a

Journ.

Am.

'Adapted

Cbetn.

from

Soc.

Bulletin

16,

small

a

and

20

frame

in

cc.

'

46, Div.

Cfaem.

U. S. Dept.

the '

"

151.

Agrto.

of clined in-

an

of boiling-point -

"

in

with digestion-flask

550-cc.

a

of flask

juice,dried

256

acid

for from

added

acid

boils

the is

badly,

froths

of the

contents

small heat

further

briskly. No

JUICE.

flask have

frothinghas cea.^

until

or

a

The

prevent it.

to

THE

minutes,

15

5 to

If the mixture be

OF

ANALYSIS

piece of paraffinemay

is then

a

the

is

attention

become

until

raised

required till clear liquid,which

color. The pale straw from flask is then removed frame, held upright, and, while still hot, potassium permanganate is dropped in carefully in small quantity at a time, till, and after shaking, the liquid remains of a green or purple color. of the (2) The distillation. ^After cooling, the contents

coloriess,or

only

has

very the

a

"

with about 200 cc. distilling-flask of water, and to this a few pieces of granulated zinc, pumicestone, or .5 gram zinc-dust,and 25 cc. of potassium-sulphide its contents. solution are added, shaking the flask to mix flask

are

transferred

Next

add

from

nitrates,

50

cc. or

to the

of

saturated

a

sufflcient to

alkaline,pouring it down mix

not

with

at

the

with

once

should

condenser, which

The

all of the

generally contain U3ually requires from

40

Tive distillate is then

titrated

the

calculations

which which

will

by

otherwise

one

a

blank

ary

escape

the

has

hour

the

passed

operation

and

half.

a

ammonia,

Previous

to

that

and

use,

experiment with

nitrates

flask

tin, mix

This

standard

usual.

partially reduce

might

with

as

be tested

reagents should

to

it does

of the distillate

cc.

ammonia.

minutes

made

are

Connect

of block

first 150

strongly

that

so

distil until all ammonia

acid.

will

be

solution,free

reaction

the

solution.

acid

the

into the standard

over

make

the side of the flask

by shaking, and

contents

caustic-soda

the

sugar, present

are

notice.

nitrogen, ^The albuminoid

Albuminoid

mined nitrogen is deterof Stutzer,and the percentage

"

by the following method of nitrogen is calculated to albuminoids

by multiplying

by the factor 6.0.^ Prepare cupric hydrate as follows: Dissolve 100 grains of pure cupricsulphate in 5 liters of water, add 25 cc. of glycerol, of sodium dilute solution then and hydrate until the a ,

1 uae

W. of

Maxwell, the

analysts. albumin"Hd

La.

factor He

bases

matter

6

Expt. instead

Sta. Bui.

38, 2d

of 6.25

this factor

6

of cane-iuioe.

on

as a

Series,

is customary

study

of the

p.

1375,

by

advises many

composition

the

plantof

the

OF

ACIDITY

257

JUICE.

THK

liquid is alkaline; filter;rub the precipitateup with water containing 5 cc. of glycerolper liter,and wash by decantafiltration until the washings are tion or no longer alkaline. Rub the precipitate with water ing containup again in a mortar 10 per cent of glycerol, thus preparinga uniform gelatinous that

mass

be

can

of

quantity

the

measured

with

out

cupric hydrate

per

pipette. Determine

a

cubic

centimeter

of this

mixture. Place

boiling;'add containing about 0.5

heat

to

cold, wash

filter when

bes^er, add

a

100

of water*

cc.

quantity of cupric hydrate mixture of the hydrate; stir thoroughly, gram a

with

precipitatefrom

the

juicein

of the

10 grams

the

cold water,

and, without

filter,determine

removing,

nitrogen according

of total nitrogen, given for the determination adding sufficient potassium sulphid solution to completely The filter-papers used precipitateall copper and mercury. method

the

to

practicallyfree

be

must

is rich

examined

of

centimeters

adding

the

serves

to

nitrogen.

from

alkaline

in

phosphates, add

concentrated

a

alkaline

the

decompose

mix

done, cupric phosphate and

not

free

substance few

a

of alum

solution and

cupric hydrate,

If the

cubic

just before

well

by stirring.This phosphates. If this be alkali may be formed,

dissolved be partially protein-copper precipitate may in the alkaline liquid. is always ^Normal cane-jiiioe 123. Acidity of the Juice. of the The acid. acidity is usually expressed in terms alkali required of decinormal of cubic centimeters number of preparing 100 cc. of the juice. The method to neutralize and

the

"

a

alkali solution, preferably caustic

normal

by diluting 100

normal It

using

logwood of

an

1

In

a

case

a

of the

excess

the

very

solution

assumes

cDnvenient

as

paper

be

logwood

of

cc.

difficult to

is very litmus

should

it

decinormal

The

417.

page

on

to

solution

when

If litmus

sensitive neutral be

may

purple

or

alkali.

proceed

of sorghum-cane

as

used a

In

violet

an

heat

A

the

indicator.

a

water-bath

20

drops The

presence

titration

Measure

on

is used

few

color in the

making

in

reached

paper

paper. as

follows:

5"*W,

cc.

neutralityis

indicator.

the

prepared from

of the latter to 1000

note

an

is

soda, is given

cc.

it is

juice

10 minutes.

258

ANALYSIS

into

beaker

a

one-tenth

few

and

5

in

juice

in

normal is

the

additional

bonation, limeitcontainQi

is

juice

in

If

very

treatment and

little,

a

the

as

at

acidity

before

test

dish,

separate

with

neutrality 100

per

the

in

except

of

cc.

special

made

by

Juice. the

The

methods

same

carbonation

factories,

few with the

tigations, inves-

defecation.

Clarified

the

with

neutrality,

carbonic

analysis,

juice

the

acid, to

that

as

is

process

used,

precipitate

the

which

an

first all

the

of

receive

must

after

of

analysis

"

juice. case

in

required

of of

by

the

alkali.

not

control

juice

burette-reading

product

is

Analysis

clarified

the

this

little

approaches time

to

decinormal

test

or

124.

the of

terms

time

from

Multiply

record

above

The

the

it

solution.

logwood

by

of

drops

liquid

drops

lew

a

into

solution,

the

As

add

and

Measure

caustic-soda

stirring.

JUICE.

dish

it.

to

normal

constant

THE

porcelain

a

solution

logwood

of

a

or

OF

car-

of

the

260

SIRUP,

the

MASSECUITES,

This

sugar.

of the

are

non-sucrose,

is

with

the

with

the in

a

Since with

having such high cpecificgravity, as carbohydrates, infhience the density marked degree. very

compared

sugars

of

ratio

massecuites

indicated

the

these

remarks

as

Brix

from

percentage

hydrometer, and

caution

similar

and

spindling

condition

number

hydrometer Thus, for example, if

dissolved in two

higher

dissolved

in

only

of the

and

one

one

salts in the

to

similar

a

molasses.

been

yet that at

tioned. men-

calculated

another

tion. dilu-

final molasses

a

this solution be this

This

spindlingwill been

difference is partly

contraction This

be

spindled,

part of the-molasses

solution of sugar

of the

partly

from

calculated from

part of water.

contraction and

water

and

solution calculated from

part of

one

be had

it would

than

not

ascertained

water

of the molasses

the

to

parts of

a

has

is different

dilution

one

the

Brix

that

density (Brix) of

at

massecuites

maintained.

analysis are

of

is another

The

of the

density of the product, must be accepted then only for comparative purposes when

the

conditions

There

calculations

that

solid9 in

total

apparent

or

molasses, from

with

apparent

is

sugar

larger.

degree

from

increases

sucrose

commercial

as

the

between

tions determina-

the true by ascei*tained by actuallydrying the material,

It is evident

with

the

to

non-sucrose

difference

the

percentage,

due

in the

as

molasses.

of total solids,as

becomes

cane-

hydrate regards the carbofor the inorganic salts which are

stage of the manufacture,

each

as

and

the

removed,

be

far

so

salts

These

the

MOLASSES.

specificgravity

same

true practically

bodies, but is not associated

AND

on

dilution

of the

tion solu-

difference would

be

dealing with a pure sucrose instead of molasses. solution Obviously massecuites and to be directly spindled,hence too dense molasses are one obtained numbers dilution by and must accept spindling The chat are at best only comparative. true solids of a observed

though

even

final molasses

may

indicated The

methods

by

one

be from

were

5 to

dilution and of

dilution

10

per

cent

below the

bers num-

spindling. and

spindling,given in this

customarily used, and the results must not be considered absolute,but only as suitable for comparisons. book,

are

those

SIDERSKY's

GRAVITY.

SPECIFIC

Specific Gravity.

127.

261

METHOD.

Method.

Sidersky's

i"

boiled applicable to samples of massecuites blank and to molasses, but not to grained strikes. The required is a 50-cc. sugar-flask,a suitable apparatus is

method

This

heating arrangement, Grind

stopper. the

into

massecuite

object of the

When

3

or

not

as

the

to

sample hot

a

cool

air, then

few

flask in cold

water.

then

the

reduce

and mark.

Weight

of flask and

''

''

it

' '

''

of the funnel

of

of the

top

on

material

the

shown

in the

to

molasses

295

66

and

ti

(I

water

"

It is very account

direct

.

.

the

to

.

molasses

94.672

:

*'

grams grams

91.570

(also its vo'mne

in cc.)

3.102

grams;

of the

molasses; 66.295-51.4136, the required specific gravity at 17i" C. find the degree Brix of the table, page 482, we

By means corresponding on

water.

=46.898, the volume

50-3.102

46.898

and

and

J" C,

grams

25.276

of flask,molasses ''

17

molasses,

91 .570

the molasses

''

contents,

followingexample

empty

''

of the

escape

weigh the flask and

and

are

very

.

Weight

heat.

the

by immersing the

temperature

flask

calculations

The

a

latter to within

facilitate the

to

room

the

cylindrical lamp.

a

carefullyso of the flask with molasses. Keep

temperature

into

water

run

the funnel

minutes

Dry

fillthe

and

Remove

It to the

distribute

to

a

emery with a

it in

set

lower the stem

is

the neck

smear

for

funnel

carefullywith the flame of

cylinderis

of the mark.

cc.

Fill the

molasses, and

quite warm, into the flask, lift the glass rod 2

glassrod

a

glassrod with moistened

or

iron

the material

with

stopper.

a

iron support, and heat The

funnel

a

of the

end

one

funnel, to form of the

sample

and

to

this

specificgravity to

difficult to of the

method

heavy molasses

for

make

a

the

by this method the only It is, however,

specificgravity

of

that is used. iZeitschrift, 1881,

79.6".

test

correct

air-bubbles.

be

p.

192.

massecuites

and

262

128.

paragraph volume

be used

depend

The

of

convenient

This

and

mze

cubic

strip which

foot

cylinder to

and

certain

a

or

metal.

should

be

will,

gallon

or

partly

in

ade

supports

The

ground

should

from

be

in

rim a

provided, of

glaas tube

a

of

true,

side

to

shown

capillary, as

a

of

metal, CC,

extends

of

cylindrical veasel

a

preferably

of

previous

is shown

of

cylinders

of the

A

of the unit volume

the

conHista

ia the

weight

the

this measurement

making

for

Massecnlte."

desuribed

selectbn

whether

upon

in Fig, 7S.

section

Volume

to ascertain

of massecuite.

device

any

Unit

a

MOLAB6BB.

AND

of Sidersky's methoii may

course,

A

of

Weight

modification

of

UASSECUTTEB

SlBTJFj

the

drawn

TT'.

Pins

'

PP'

the

m

in

rim

of the

in

insure

the

in

run

until

cautiously the

instant rises

previous determination the

of the

bottom

this volume with

volume

ascertained

if

plainly

76.

should

of the

and

that

the

massecuite,

and

colored

of the

tube

be

may

be

of

and

more

A

cylinder

to

With

water.

cMnplete

to

is

weight

the

it

used.

massecuite

with

compared

The tube

is

with

of the

very

by capillarity.

the

required

water

that

it

water

made

position,

the

noted

volume be

in

masee-

is reached.

into

readily

may

tube

cylinder

burette

a

reaches

water

distance

some

This

from

the

always

with

lo

of

strip

latter

capillary-tube

water

fitting

Fill the

point

the

the

the

position.

same

cuite, place the then

in

replacing

approximately

to

FiQ.

holes

corresponding

metal

cylinder and

the

readily of the

material. In

making this at

made

the It

in

which the

the

evident

be

that

and

and

correction

be of the temperature to

be

expansion

of

product

for

the

are

applied. this

are vibrations of machinery Degree 139. Apparent

Dllntton

should of this

measurements

factory,

cylinder should is

the maasecuite

test

method

cannot

be

Uaed

\"iiere

felt, Brix.

SpllndUDg.^Di3solve

DetermlnatloB a

weighed

quantity

by of

DILUTION

material in

263

SPLINDLING.

AND

Transfer equal weight of distilled water. its a portion of the solution to a cylinder and determine degree Brix. Correct the degree Brix for the temperature the

error

an

described

as

number

by

This

material. method.

on

2

is the

The

ascertain

to

several degrees lower

commercial

the

and

number

apparent

Brix Solids by Befractometer. or Apparent has been described method of using the refractometer

The

"

page

are

this method

those If the

material

sample closely approximate

gives results that

be crystals of sugar these must refractometer only indicates the solid

the

calculation

solution.

is made

solution

When

is indicated

as

methods

Dilution

paragraph.

clarification of the

contains

is in

that

and

by drying.

dissolved,since matter

dilution

When

225.

unnecessary

the

the

factory usually ling. by spind-

130.

on

rected cor-

of solids is

percentage

or

than

multiply the degree Brix of

the

customary

Brix

true

and

222,

page

involve

by working with

very

concentrated

farther the

by spindling. The

of similar methods

employed in

on

contraction

error

sr

is

this error

be reduced

may

lutions.

If

volume

a

solution,for example, the is not the sum volume of the mixture of the volumes, but is smaller number, and the concentration is higher. It is, a in hydrometer methods that the same as therefore,necessary of water

definite

be

added

to

conditions

molasses

a

observed

be

that

results

the

be

may

comparable. In the event

testinga highly colored material,the method

of

of Tischtschenko

equal weight and determine

may

of of

the

a

as

solution

high

refractive

of solids in the mixture The

used.

be

Mix

of pure

by

means

percentage of solids in the

as

with

of known

sucrose

concentration

index.

material

the

is

Ascertain

position com-

practicableand the

of the table material

an

on

percentage 492.

page

is ascertained

by

solution from deducting the per cent of solids in the sucrose The principleof the method twice the solids in the mixture. of calculation

for other mixtures

dilution formulae If necessary

is made

to as

is the

same

as

that

of the

(307). dilute the follows:

material

with

lation water, the calcu-

264

MASSECUITES

SIRUP,

Let

x

MOLASSES.

AND

the required percentage of solids

=

(Brix);

weight of the material

used; weight of the diluted solution;

TF== t^;'^

then Wx^bw

and

True

131.

method

x^bw/W,

Brlx and

of Carr

recommended

are

method

and

Sanborn this

for

1

use

the

method

vacuum

material.

of distilled water

in order

to

distribute

latter

both

methods

small

quantity

In a

The

(IIS)

the

In

weighing the material, dissolve it in

after

Drying."

by

determination.

the

of

gram

Solids

Total

or

it evenly

the

over

pumice-stone. In Carr and Sanborn^s method, dilute the of about 20 to 30 sample in a weighing-bottleto a content dry matter, using a weighed quantity of distilled water, and transfer a weighed portion of the solution con" tared 1 gram dish. of dry matter to the taining about per

of

cent

Dry the sample and 112, and the

to

the remarks

the percentage,

in the

same

directed

as

in

paragraph in regard

decomposition of levulose. Determination

132.

of

note

calculate

determining

molasses

or

the

of

Sucrose."

the of

percentage

sucrose

depends upon

majssecuite

The

in

the

method

sample

a

of

purpose

of the'

analysis. the

For of

the

various

the

apparent

cent

per

especiallythe

absolute

the

percentage relation,however, between

The

required.

factory, for the control

manufacture,

work, crystallizer

is not

sucrose

of

processes

and

vacuum-pan of

of the

ordinary purposes

and

sucrose

the

degree Brix,

purity, is frequently needed, but not with The most a important great degree of accuracy. in is to adopt certain connection with this work point

the

coeflficient of

conditions similar

For

of

analysis

and

materials, otherwise the

of

purposes

produced in the various

adhere the

to

molasses avoid

error

results

them

with

will not

be

all parable. com-

comparing the commercial sugar of the and periods crop determining

the total loss of sucrose, conrniercial

to

it is very samples be and

to

essential that

the

final

analyzed,using every obtain

absolute

or

caution pre-

results

as

DETERMINATION

OP

THE

265

SUCROSE.

.

nearly the "

the

processes of analysis will permit. considerations for what methods may

as

above

factory tests" be given:

and

Determination

of

of the

modifications

In

of

view

be termed

Clerget process

will

massecuite

molasses

or

after

and

solution

the

of

little

a

in water This

and

Brix.

15"

approximately

factory tests.

sucrosCf

dilute

Dissolve

"

the

solution

the

is

to

usually quickly the degree Brix experience. proceed as in 115, using the sucroseplished accom-

Ascertain

pipette. dry-lead method

Home's

used

be

may

to modify the usually advisable of the high levulose account content

method

it is

Dilute

molasses.

the

massecuite

shghtly to

on

and

massecuites

of

molasses

or

tests, but

in these

between

Brix; add sufficient dry subacetate of lead for than is necessary. the clarification, being careful to use no more ing. Also add a little dry sharp sand and mix thoroughly by shak15** and

16"

The

clarification is most

glass cylinder which while shaking. hand a

50-55 to 55

up

massecuite

or

to

a

conical

these

compensate

of

cylindersmarked

at

"struck"

a

and

spoon

of the

measure a

measure

of

dry

sand;

of the

cylinder by shaking and then add a of powdered oxalic acid (dry) and another of kieselThe quantity of acid must be insufficient for the precipitation

extended

The

200-mm.

table, page 494, and opposite the degree Brix

number

measuring

purity by Home's

most

to

a

100-cc.

of all the lead. the

a

in

make

the solution.

purityof

molasses; add

the contents

guhr.

acidityand

point and to modify the method Fill the cylinder to the mark with the diluted

follows:

measure

Home's

in filtrate,

of the

cc.

reading by one-tenth

to have

approximately the

mix

50

this solution

polariscope reading and

It is convenient

lead from

Polarize

Refer

find the coefficient of

as

to

dilute acetic acid to

the

increase

the

under

Filter and

water.

dilution.

the

for

^ith

cc.

and

tube

may

fiask,add

cc'

conveniently effected in a small be covered by the palm of the

to

cover

Shake, filter and

table,page wider

a

range

526.

The

polarize. Find table should

of densities

at

the

be

places

used. coefficient of tests.

purity is all that is usually required

It should

be noted

that

on

account

of the

in

large

266

i!ie coefficient is lower

dilution of the material otherwise

MOLASSES.

AND

MASSECUITES

SIRUP,

than

it would

be. Method

Clerget's

133.

for

Sucrose.

This

"

is often

"double-polarisationmethod," since two polarizations made, one before and the other after inversion,in are order to eliminate the influence of the invert-sugarthat may be present. Cane-sugar products usually contain the three termed

the

rect (+), dextrose (+) and levulose (" ). The dipolarization is therefore the resultant of the polarizations sucrose

sugars,

of these three sugars.

originalClerget method, 50 cc. of the sugar solution inverted by the addition of 5 cc. of concentrated chloric hydroare acid in a 50-55-cc. flask,with heating to 68" C. during fifteen minutes, followed by rapid cooling. This method quires rethe use of Clerget^sconstant, 144. The calculations In the

made

are

in the

as

described

modifications

The

usually used in been

following modifications

view

a

Modification.

The

"

slightlyfrom

factory conditions:

those

of Herzfeld

Dissolve

65.12

molasises in water, contained

65

grams

for

dilute clarification,

true

a

to the

of the filtrate contained

acidityand dilute

to

to 55

temperature, and

the

tube

mm.

and

a

in

normal

through

error

in

to

meet

500-cc.

a

Add

are

cane-sugar

massecuite

of

(Mohr) flask,or of lead

subacetate

mark, mix and filter. To 50 50-55

a

flask add

cc.

cc.

acetic acid

Polarize this solution,noting

cc.

reduce

have

given here

grams

flask is used.

cc.

risk of

instructions

or

if

those

are

simplifythe work.^ man) Herzf eld's (Official Ger-

to

or

Method.

Clerget's

modified

reducingthe

to

decompositionof levulose

following pages

method.

All the modifications

work.

cane-sugar

devised with

134.

in the

of the

the. reading

solution.

to

Correct

terms for

the

of

a

200-

dilution

increasingthe reading by 1/10. Enter this number ."Ni the direct polarization. Delead a portion of the originalfiltrate by the addition of It is not necessary that all the lead be dry sodium oxalate.^ 55 cc,

to

removed Cross

1

in

in

recommends

preparing

uoed

in

filtration

deleading,but

excess

may

for

the

both of

be

the

the

use

of dry

direct

quantity

difficult.

the

Lt

and

quantity left should be oxalic

required ^xpt.

acid

invert

Sta.

to

as

a

deleading

polarisations.

precipitate

Bui.

the

135, p. 29.

If

very agent this

is

lead, the

268

SIRUP,

duoe.

Herzfeld

Prof.

MOLASSES.

AND

MASSECUITES

requested

International

the

mittee Com-

Congress Meeting of the International of Applied Chemistry) to revise his table of constants, as several investigatorshave reported apparently high results York

(New

in its

Steuerwald

use.

^

has shown

that

Herzfeld's

constants

these numbers give high results and has redetermined table: published them in the following convenient STEUERWALD'S

(Hersf eld's

The

Steuerwald^s

constants

to the

and the

Inversion

is calculated

sucrose

substitute

invert this for

by

Method).

Herzfeld's

follows:

as

Select

formula, using a

constant

polariscope-readingand *'

constant"

invert-reading is always

1

CONSTANTS.

OF

TABLE

Archief., 1913, 21, 1383;

Int.

and

minus

Sugar

in the in

temperature

formula. cane-sugar

Journ., 1914,

sponding corre-

16, 82.

Since'

work,

CLBRQET

divide

the

S

of the

269

METHOD.

direct-

and

invert-readingsby the minus half the temperature in centigrade degrees constant and multiply the quotientby 100. tion, Example: Direct polarizaThe 30.4; invert-reading,"17.9; temperature, 24" C. at 24" is 143.06, therefore constant corresponding to "17.9 Per cent sucrose substituting these values in the formula: sum

48.3

30.4+17.9

"

~

="

=36.85.

=

143.06-12

131.06

inversion

The

within

complete wlien

and

there is certaintythat

the

is

above

20**

always above

sixteen hours

as

twenty-four hours C.

temperature

four-hour

20** a

is sufficient.

with

be avoided

heating may of freedom

lose.

The

flask

shown

in this The

with

tainty cer-

of levu-

modification

acid

FiQ.

76.

of the

section is for the acid and

the sugar the top mark

Method

by

inversion

increased

with

and

body of the flask

The

"

inversion

special inversion in Fig. 76 eliminates pipette

solution,the middle completes 100 cc. 135. Clerget's wald.*

venient. con-

convenient

measurements

method.

twenty-

that, when

destruction

from

fact

short

so

most

this it appears is available, the tedious

a

ture tempera-

The

period is usually the

at

in

period

From

time

at the

inversion is always

The

temperature.

room

conducted

be

may

serves

to

measure

Modified

as

is conducted

at

Steuer-

temperature

room

strength. A specialtable of

is

constants

required. Prepare the solution Measure add

and 1.188

sp.

30

and as

hours

two

of the

been

filtrate into

if the temperature is between

if above

25" C.

polarize,observing the have

in the

preceding paragraph. a

100-cc.

flask

hydrochloric acid of 1.1 sp. gr. (acid of diluted with an equal volume Set of water).

aside three hours or

cc.

described

of

cc.

gr.

50

as

described

Dilute same

in the

20" and

the solution

temperature

to

25** C. 100

cc.

conditions

preceding paragraph. The

^Archie!,, 1913, 21, 831; Int. Sugar Journ., 1913, 15, 489.

270

MASBEGUITES

SIRUP,

followingtable of the

Herzfeld

consianits

fonnula.

of the normal

terms

before

AND

TABLE at

be

reduced

to

tion of solu-

cc.

of

in I2I9 except

burning

use

normal

to

30

Ash."

acid.)

cc.

Proceed

as

is directed

2 to 3 grams

of the material.

is facilitated

by dissolvingthe

alcohol and

in diluted

with

the

from ash

CONSTANTS.

OF

temperature

room

Determination

material

readings should

with

making the calculations:

(Inversion

The

in connection

weight of the material in 100

STEUERWALD'S

136.

be used

must

The

MOLASSES.

then

incorporating 50

mg.

be deducted from oxide, the weight of which must the ash before the calculations. Or, incinerate with benzoic of zinc

Dissolve

acid. cent

alcohol.

caramelize it at

25

Moisten a

of the

grams

the

low heat*

acid in 100

sample with Add

2

cc.

For From

of 90 and

water

per

then

of the benzoic solution

and, after evaporating the alcohol,incinerate red heat

cc.

at

incipient

in the muffle furnace.

proceedas sulphated-ash

is described in

3 to 5 grains of the material is

a

paragraph l^Sl. suitable quantity for

the test. 137.

Acidity

and

Solutions of massecuites

Qualitative Tests." molasses are usually so dark-

Alkalinity. and

CRT8TALLIZED

that

colored be

Buiaaon of

cc.

flask; add of

The

the ether

and

In the

be

of the

138.

applied

of

of

the

Masseculte.

Method.

^"TWm

method, will be

sugar

and

BURftr

30

Weigh

taiting

it to

transfer

place

fused

over

Mix

acid.

sulphuric

to time

This

the

distilled

in

of this metliod

for

He

eorallin.

staining in he

uses

uses

copy. micros-

several

and

glass

a

desiccator

a

strong

or

mixing

molasses

in

the

formly uni-

glycerine work

preparatory and

quires re-

Upwards.

in plug of dry filtering-cotton

a

funnel

of the

apparatus

transfer

Fig. 77; funnel

with

the

fifteen minutes Place

be

be.

con-

crystalsare

distributed

may

faw

until the

separated, and

eorallin

aa

the

well

case

must

solution

Repeat

time

the

as

The

drous anhy-

sugar

chloride

from

solution.

of

of pure the

the dish

calcium

the

few

masse-

a

glass dish

a

glycerine intimately

rod, and

a

first described,

grams

equal weight

an

glycerine. and

50

to

wait

cc,

tallized Crys-

then its application to cui["r

10

in alcohol.

in

raw

and

tlien

upon

of the

the

Sugar

to

gloss-atoppeiied

success

prepared

as

drop

one

Estimation

Kara

red

the

quality

of the eorallin dissolved

drops

reacts

or

author

the

upon

of

fer Trans-

neutral.

soluble eorallin

Instead

"

yellow

a

and

cannot

rise to the surface.

and

alkali

or

a

dissolving the material

must

largely

alcohol

the

in

experience

depends

to

method:

eorallin solution

separate

its color to

used

water

to

of acid

excess

changes

material

the

alkaUnity

or

followii^

Agitate thoroughly

ether.

slightest

of

the

of neutral

drop

for the ether

seconds

for acidity

tests

271

HASSECniTB.

IN

advises

'

solution

n

one

washed

a,nd

usual

the

made. 25

8UOAR

and

the

re-laco

shown

mixture

the

'Zeit.

The

mixttire

should

Rubeniucker-Indugtrie,

the

Filter

cover.

off the glycrine solution, using pump.

to

in

a

be

Pio.

77.

filler-

protected

31, 500.

from

the moisture

272

MASSECUITES

SIRUP,

of the air

during filtration by

chloride of calcium

a

at the top of the funnel-cover

shown Since

the

in the

with

contact

moisture

air should

moist

tube,

as

figure.

glycerine absorbs

anhydrous

great rapidity, its

MOLASSES.

AND

with far

so

as

possiblebe avoided. Polarize obtained

above

following formulae:

P~per

cent

p^sper

cent

x^

attached

sucrose

in the

sucrose

in the

and

V

crystallizedsugar

the

as

by the

*

in the molasses

sucrose

x="

calculate

and

glycerine filtrate

the

of

weight

normal

the

P"

x

to the

crystals;

sugar;

raw

glycerinefiltrate; the

=

of

percentage

crystallized

100-p sugar.

Example.

Polarization

"

of the

tion 95.6; polariza-

sugar*

raw

of the filtrate =6.75.

=7.55; "^^1^X6.75

"=

the

percentage of

view

In

present in cuites

cane

the

and

95.6-7.55=88.05

of

crystallizedsugar. the large proportion of glucose usually to masseproducts, to apply the method

sucrose

work, should

p, in accurate

P, and

x,

be

This by the modified Clei^et method, page 266. of Karcz' method the case in the following modification

ascertained is not

by Perepletchikow: Transfer with

an

normal

the

indefinite

described

above,

weight of the Karcz'

Wash

the

funnel

from

the

the

the percentage

of

apparatus

"

cane

Zeitschrift

"

Zapiski, 1894, 18, 346. Manuel-Agenda

293.

This

as

filter ofif the

and

and The

the

wash

crystals into

a

polariscope reading is

des

method

usually requires double

products.

j. Zuckerindustrie

1

*

glycerine,

crystalsin the massecuite.

Duponi'8 method* polarizationwith

anhydrous

treated

crystalswith repeated portions is no Remove longer colored.

polarize them.

sugar-flask and

massecuite,

apparatus

glycerine until the filtrate

of

of

quantity

to

glycerinesolution.

p.

*

Bui.

Bohem,

Jan., 1895.

Association

Fabricants

de

des

Chimistes, 12, 407.

Sucre, Gallois

et

Dupont,

1891,

SUGAR

CRYSTALLIZED

Heat

example

of

quantity

a

500

massecuite 85*^

to

grams

and

such should

centrifugal

shown

be

the

Calculate

molasses.

Fig. with

possible

as'

Polarize

in

covered

thoroughly

as

sugar

is

as

by

of

for small

a

sieve

of

flannel.

the

crystals

crystals

the

Dry of

means

the

percentage

in

sugar

The

87. thin

massecuite,

the

polarization, the

purge

,

centrifugal,

known

of

C.

573

MASSECUITB.

IN

the trifugal. cen-

and

by

the

the

foUow-

formula:

ing

Let

x="the

of

weight

crystallized

sucrose

in

one

of

part

massecuite; a

p

"=

polarization

-polarization

p^s=

polarization

the

massecuite;

of

the

crystals;

of

the

molasses.

d'

d

.'.

of

"

and

x"=

crystallized

100x=the

".

sucrose

in

100

P-P

of

parts

massecuite.

Example.

Let

a

p

=84.5; =

100;

p'"60.6.

"'^^~^'a^0.eO^

and

100aj"e0.66,

the

percent-

-

age 138a.

described

of

crystals

of

Determination in

paragraph

in

118.

the

the

massecuite. Glucose."Proceed

as

is

ANALYSIS

Polarizadon."Weigh

130. in

sugar

SUGARS.

OF

nickel

capsule. Add sufficient for the water waiting a moment

a

the sugar, The

moist

weight

normal

the

water

of

the

moisten

to

penetrate the

to

usually be poured slowly into 100-cc. narrow-neck flask without a difficulty.A little to accomplish this expeditiously. If practice is necessary is experienced, a special funnel of nickel {see page difficulty 165) should be inserted and extend just into the body of the mass.

flask. The

The

sugar

sugar

with

jet of

a

flask should water

prevent

by imparting above

be

a

neck

Care

60

of the

should

of water

cc.

well

from

readilywashed

and

water.

about

than

more

be

may

capsule, funnel

may

cleaned

adhering

rotary motion

the level of the eye

through the funnel.

flask must observed

be

in these

before

use

the

washed

not

to

use

operations. The (see

169)

page

to

Dissolve the sugar

to the neck. to

be

flask.

ocasionallyto

see

Hold

the

whether

flask

all the

Jt is essential that no sugar be left crystalsare in solution. undissolved before proceeding to the clarification. Having dissolved the sugar, add from 0 to 8 cc. of subacethe quantity depending upon the grade tate of lead (54.3**), the

of

White

sugar.

sugar

requires

no

lead, but

should

to facilitate filtration. cream usually receive a little alumina High-grade centrifugalsrequire from 1 to 2 cc. and low according to their grade, up to about 8 cc. of the sugars, After lead solution. mixing the sugar and lead solutions add about 2 cc. of alumina-cream ume (392) and complete the vol-

i

J

the neck of the flask. If washing down down interferes with this operation it should be broken

to foam

100

cc,

The water should be of the temperature drop of ether. and the flask should be held by the of the polariscope room part of the neck during the manipulations, to prevent upper with

a

warming

the solution.

drops of

water

adhere

to

the neck

be absorbed

by a stripof filter-paper. finished these operations, cover the mouth of the

of the flask they should

Having

If

*274

276

ANALYSIS

of

Determination

141.

OF

SUGARS.

Glucose."

The

method

be

to

selected

and glucose depends upon the percentages of sucrose should in the sample. A modification of Herzfeld's method be used for sugars polarizingabove 99". The Meissl and Hiller method, page 236, should be used for sugar containing than 1 per cent of glucose. more Method for Sugars Potarizingabove 99**. Dissolve 40 grams of sugar, contained in a 200 cc. flask,in water, add normal dilute to the mark, solution for clarification, lead acetate mix and filter. Add dry sodium oxalate to the filtrate for be predeleading and refilter. If preferred,the lead may cipitated by potassium oxalate solution before diluting "

cc.

and

Measure

50

to 100

solution and and

add

50

thus

cc.

be avoided.

of Soxhlet's cc.

25 solution, i.e., of the alkali (297) into

of

the deleaded

cc.

25

filtration may

one

sugar

of the copper 400 cc. beaker

cc. a

solution.

Heat

the

boiling,taking about four minutes to reach this temperature and continue the boilingexactly two minutes. At the conclusion of the heating add 100 cc. of cold recently mixture

to

boiled distilled water

to

the contents

of the beaker

and

then

oxide in a Gooch or an immediately filter off the cuprous crucible and proceed by one of the methods alundum described The percentage of glucose is ascertained from the in 118. followingtable by inspection: HERZFELD'S

TABLE

FOR IN

OR CENT

LESS

OF

SUCROSE.

MATERIALS

INVERT-SUGAR

THE

DETERMINATION CONTAINING AND

MORE

OF 1 PER

THAN

VERT-SUGAR IN-

CENT 99

PER

ESTIMATION

OP

Estimation

142. driven

of

by drying in

off

the an

operation is conducted

the

sugar.

the temperature

sugar,

fact such

factories

sugar

the

depends

drying

of

temperature

in

off until

driven

should two

receive three

or

be

dried

for

conducting

hours

samples

both

be cooled

in

method

moisture

is reached.

of sugar shallow dish is

a

vacuum-oven,,

and

water-oven

a

recommends

considered

dry.

moistened

that

ceases

sugar

after

air-oven and

an

Pellet

water

that

the

sample

lose moisture

to

dried

The

sugar

"

described

as

to

desiccator preparatory to weighing. of the Ash. ^The sulphated-ash

a

Determination

143.

of

granulated

are

be heated

granulated sugar,

with

percentage

the

in

of

105** C.

at

C.

3 grams

transferred to

be

period

paralleltest

a

When

contains.

should

should

short

a

absence

the

preliminarydrying

estimated

the

with

a

in

105"

at

of 105** C.

A

usually sufficient. Low-grade sugars,

raw-

comparatively

dried

drying period of three hours for 2 to of a broad the bottom spread evenly over

in

product, hence

even

may

temperature

a

be

of

molasses

a

Modem

vacuum.

liable to occlude

Large crystalsare

at which

lOO"* C. and

usually be

may

is

character as

little low-grade

high. A sugar of large and exceptionallyhigh-test sugars is not

the

upon

rise above

not

moisture

temperature

crystal should

110** C.

The

grade, such

dried

be

produce

now

The

should

should

sugars

Moisture."

is of low

sugar

277

MOISTURE.

oven.

the

If the

THE

on

270

page

for massecuites

testing. factory and commercial Iron in 144. Sugars. Sulphide

is used

in

both

^Prepare a stock solution containing 10 grams solved discrystallized ferrous sulphate, FeS04-7H"0,

Method.' of

"

pure

in addition

Colorimetric

50-60

a

of

few

a

per

cent

solution,with the

sucrose

pure

drops of sulphuricacid,and dilute

to 1000

The acid should be very with the sugar solution. diluted before adding it to the sugar solution.

largely

cc.

Dilute to

time

as

solution The

required, e.g., 10

to 500 tests

are "

1

solution with

this stock

cc.

distilled water,

to

100

cc.

and

50

time

from

of this

cc.

cc.

made '

Eastick, Og^lvle and

in Nessler's

cylinders,a number '

J

Linfield, Int. Si"gar Journ., 14, 428.

of '"

278

OF

ANALYSIS

of the

which

SUGARS.

diameter and

same

height should be provided.

cylindersmeasure increasingamounts of the diluted stock solution,noting the quantity of iron in Add 2 cc. of recently preeach, and dilute each to 100 cc. pared of ammonia to each and stir. solve Dismonosulphide Into

series of these

a

in

of the sugar

3 to 10 grams

the solution to 100

add

and

cc.

2

a

cc.

Nessler's of the

cylinder,dilute

sulphide solution.

cylindersStand ten minutes and then match the color of those containing of that including the sample with one then contain Both the same the stock solution. quantity used. of iron,t.c, the quantity of iron in the sugar The Let the

cylindersshould stand

white

on

in

paper

the

making

sulphide is prepared by saturating ammonium with sulphureted hydrogen and then adding an

The

the

In

of dark

case

incinerate the sugar,

sugars,

sulphuric acid, burning

of iron-free

addition

droxide hyequal

hydroxide.

of ammonium

volume

parisons. com-

at

with

the

the

lowest

the ash in a Dissolve minimum possible temperature. quantity of iron-free hydrochloricacid and proceed with this solution

as

The

145.

described.

has been

Color

Dutch

Standards."

Foreign sugars duty according to their

entering certain countries,pay If their color is No. 16 Dutch polarization and color. standard, e.g., or lighter,they pay a higher rate of duty than

on

this standard.

than

if darker

of sugar

numbered

renewed

is not

set

a

'is white

samples These

sugar.

in Holland The

of

and

are

time, since the color of the

to

plied sup-

samples should sugar

permanent.

of

chemist a

sample

of this color

will

sugar

a

tropical sugar

of No. or

16, so

as

in with

siigarthat

a

raw

the

factoryshould

to avoid

the

rendment sugar

is the

and

No.

first be

shipment

lighterto certain countries

loss to the factory-owners. The Rendment." 146. of refined

usuallybe darker than

is boiled

molasses

especiallywhen with

of

bottles.

in sealed

time

from

Centrifugal 96** The

up establishment

trade

the sugar be

an

consist

20, which

to

prepared by

are

standards

color

Dutch

The

16

sugar.'

supplied of sugar

consequent

estimated yield will produce. This esti-

279

RENDMENT.

Biate

is in

The

ash

based different

American from

percentage

refining

upon

countries refiners

the of

and

rendment,

five

deduct of

polarization or

for

the

the

of

sugars

times

raw

**

is

and

experience

calculated different

the

origin.

percentage obtain

to

sugar

analysis"

ously vari-

of

the

sugar.

of the

ANALYSIS

FILTER-PRESS

THE

OF

CAKE.

r of

Preparation

147.

press-cakeobtained small

to

it to

With

firm

be

and

Moisture

148.

press-cake, in a

the

water-oven

at

of

means

sample

may

tared

of

reduced

lax^ to

necessary

subsample the

it.

press-cake

readily reduced.

be

-Dry

dish,

5

of

grams

The

the

weight loss of weight

constant

to

100** C.

approximately

be

then

management

be

spatula or

a

soft it may

careful

shallow

sample

104, should

Determination."

a

^The

"

large mortar,

a

and

cane

by

is very

paste in

a

good

will

as

cake

If the

in

directed

fragments and mixed

scissors. rub

Sample.

the

in X

percentage of moisture.

20=

should

sample

The

partly dried

be

at

a

low

temperature

before

to 100" C, otherwise the surfaces of heating the oven be covered with a glazed coatthe fragments of press-cakemay ing

would

which

in all

convenient to have

other

prevent the

two

cake filter-press

to

sample

Wash

the material 6

the

volume

and

small

a

low

a

and

temperature

into

to

100

a

a

Add

smooth

100-cc.

of lead mix

cc,

^Transfer

"

mortar.

it to

rub

subacetate

cc.

to

Determination.

to the

add

heated

one

the

final'temperature.

Sucrose

149.

be

open-dish dryings of sugar-house materials

ovens,

to the

It would

of moisture.

escape

cream

flask with

solution the

25

grams

boilinghot with

of

water

the

pestle. hot water, cool,

(54.3**Brix), complete

contents

of the

flask thoroughly,

and polarize. The polariscopereading is the filter, in the press-cake. percentage of sucrose of the sample, 50 grams convenient It is usuallymore to use of lead while rubbing the material and add the subacetate to

the

a

and

cream

removal

mortar.

A

all into

wash

of the

last

flask with

a

200-cc.

portionsof

the

neck

flask. This facilitates

press-cake from the enlarged above the gradua* the

28a

SUCROSE

is

tion

in

convenient

more

sugar-flask

(Fig.

in

in

object

this

is

using

to

for

correct

by

A

rubbed

to

with

7"

of

water

weight

the

lead

cipitate pre-

matter.

sample

a

of

described,

method

residue

4.6X2+

and

filter-

also

and

0.5

is

9.7,

of

amount

normal

weight.

similar

results

that

average

those

25

the

same

material

experiments described.

to

by

the

was

the

very

of

to

The

sum

other

two

approximately use

instead writer

4.6.

diluted

0.5. in

a

cooled

reading and

as

is

onto

with

a

polarized

was

defecated

washed

filtrate

giving

grams

sample

continued The

of

cent

and

sugar-flask

filtrate

tated precipi-

this

then

was

a

and

per

water

lead,

cooling,

9.6

of

hot

filtrate.

nearly

or

Many to

of

into The

showing

experiments,

with

cream

of

each

portion

after

lime

of

polarized,

washed

filtered.

acid,

in

washing cc.

cc.

was

and

a

200

200

to

acetic

third

The

nearly

to

diluted

correct

on

gave

subaoetate

filter.

cc.

of

saccharates

sucrose.

100

normal

insoluble

the

adding

levulose,

The

the

volume

of

the

by

decompose

to

and

of

material

the

oe.

modified

hot

ordinary

an

of

grams

experiments,

cake,

press

the

that

Parallel

25

instead

analysis

and

Fig.

than

analysis

this

78). The

100

281

DETERMINATION.

the of

have

the

given

ANALYSIS

OF

THE

BAGASSE

CHIPS

the

sample

as

described

mixed

and

quickly reduced The

(DIFFUSION),

Preiiaratton of

1^.

EXHAUSTED

AND

the

Samples."

in 100, it should

be

After

oughly thor-

subsampled. The subsample should small piecesby chopping or shredding.

to

preparation of the sample for the sucrose important. The pieces should be very

Java

securing

rapidly and

be

test is especially

small.

The

require this sample to be fine enough

laboratories

to

^ collaborated in the through a 4-mm" sieve^ De Haan preparation of the Java instructions for bagasse analysis in which the above specification ea to the sample is given. He,

pass

however, has stated

^

is reallylargely due

to incorrect

influence

that the apparent

of fineness

sampling. This implies that the chemist unconsciously selects liie larger pieces rather ' than an Nonis of the sample. 6 nun. i^)ecifie8 as average largest admissible the opinion of the writei^ attempts the diameter

of the.

piece of bagasse. to

reduce

lead to specificationmay the the drying of the sample, especiallywhen Norris'

finer than

is

high.

average

and

4

it to average cent

per

it is evident is

as

may

that

too

high.

even

There

sucrose

Slow

in the

From

then

the

through

errors

content

sucrose

to

ascertain

is often

these

be

sucrose

the

observations

prepared numbers

as

may

compensating error viz.,slightlyimperfect extraction a

rapidly be

1

Int.

"

Ibid., 5.

Sugar

Journ., 1912,

Bui. 32, Haw. "Ibid., 8.

Sugar

result in

may

a

of the

large error

14, 43.

Planters'

Ezpt. Sta., 32. 282

a

that

digestion.

preparation of the sample

i

material

during the preparation of the sample the chopper is covered 2 per cent when sample should

the

offset this error,

tests

numerous

uncovered.

when

possible,and

httle

made

loss of moisture

found

and

Norris

*

the

In

284

ANALYSIS

BAGASSE

OF

AND

EXHAUSTED

CHIPS.

The Athol meat-chopper, size by hand power. No. 405, Fig. 80, is an efficient machine for reducing bagasse. has large capacity and may This machine be oovc^^ during chopping.

by belt

or

indicated

dry

It is also

dried in the condition

mills,to avoid

it is of

has

been

importance

to

tion distribu-

important that the sample

in which

both

upon

As

it is received

from

the

drying during the manipulations.

from

error

Experiments laboratory have

Moisture."

of the lack of uniform

account

on

of the moisture. be

the

preceding paragraph,

in the

large sample

a

of

Determination

151.

manufacturing scale and

a

in the

be heated to high bagasse may without appreciable decomposition. Such temperatures made in drying shredded cane tests were at Preston, Cuba, where the. temperature employed was higher than very much is here suggested for laboratory work. Drying in vacuumthat

temperatures is not dependable.

at low

ovens

shown

recommend

drying samples of

20

or

grams

writers

Many less.

even

From

there point of view of the test of the particular20 grams is no objection to this quantity,but so small a sample cannot accurately represent a material such as bagasse. The methods of drying given in this book are arranged in order of the writer's preference: Method ^This InvolvingDrying in a Current of Heated Air. method requiresa specialoven onthfB principleof that shown the

"

is The Fig. 81. oven provided with a removable and the clamps, E, insure an

in

of the

but water

this does

not

heater

is

If this heater the

the

cover,

D.

rubber-gasket,/^

A

jointbetween air-tight

the

body

clamp may not be necessary A steamif the door is heavy and the jointsare well groimd. of air through a ejector,Ff draws a very strong current The air is heated by heater, the pipe (7,and the basket A. receive a preliminary steam-coil. It may a passing it over quick-lime,followed by filtration, drying by drawing it over oven

and

cylindricalcast-iron vessel, C,

a

air should

appear an

The

cover.

to be

inexpensive and

is uiSed with be

drawn

exhaust

efficient steam

through the

surrounding it,but with live

steam

the coil, The

of air is

specificheat

A

necessary.

heating device.

from

copper

size feed-

small

the

engines,

coil,the

the air should

low, hence

pass

the

steam over

pipes

DBTBRMIKATION

should

be

THE

OF

covered

ajid

a

o! it must

large volume

very

285

HOIBTtTRE.

be

used. A

cylindrical bagasae-baaket

fits in the

be

of the

is used

as

round

tared

banket

holes per

basket

and

the

makes

basket

ueaally sufGraent oS

gasket

A

insure

pipe of

G.

air.

A

battery,

a

a

If it is desired

ejector, F, when an

fur-eock

This

Those

oven

and

used.

leave

or

inches

of loose bagasse

or

deep. 2

the

the

air

are

be,

If the

a

oven

be provided in the

regulating the

will receive basket

to

on

the

provide

in breaking the

use

of any

current

turned

steam

for

This

weight

thermMneter,

it is necessary

elsewhere

for the nriter 12

in

oven,

constructed

The

should

The

if need

air current.

stop-valve

to

cover

be

may

constructed

in diameter

be of the

opening the

in the

1'he

of the

pressure

joint, but

good

may

a

the

is also convenient

valve

625

flange supports

narrow

bagasse and

steam-packing

of

one

about

inch is suitable for this purpose.

H, indicates the temperature forms

The

plate, such

containing

joint vilh the iron castings.

to

should

to be dried.

are

brass

Sheet

brass, A,

baskets

more

samples

is open. a

and

or

sheet

finely perforated brass

is of

square

basket

thin

very

Two

if many

in centrifugals.

of the

top

is indicated.

as

and

provided

bottom

of

oven

of

convenient a

basket

'siw.

8 inohes

will hold

kilograms if lightly packed.

gram 1 kilo-

The

286

ANALYSIS

OF

BAGASSE

drying period is extended basket

of this size may

shown

in

The

few minutes

ft

be used

A by the packing. with the 5-kilogram balance

Fig, 44.

method

of

drying is as follows:

Assuming efficient millkilograms by subsamkilograms of bagasse,

work, reduee, the sample to about 2 pling; fill the tared basket with 2 be necessary. packing it lightlyas may

replacethe

in the oven,

110" C. and

above

be heated

air should

The

air.

and

cover

pr^erably

Insert

sufficient

turn

ejector to produce

into the

steam

CHIi"S.

EXHAUSTED

ANP

a

very

to 130" C.

basket

high-|;":e8sure

strong

conveni^t

to any

the

of

current

temperature

The

air-pipeshould

be well covered.

drying -periodvaries with the temperature of the air and the condition of the bagasse. At 110" C. the period is usually At the close of the drying-period, about ninety minutes. The

which

after

little experiencewith thfe oven

a

may

be

arbitrarily place it in a

by the bail.By and A large earthenware desiccator to cool. a jar will serve as of desiccator. After cooling,ascertain the weight in grams the dry bagasse and divide this number by 20, to arrive at the "the basket

fixed,remove

of

cent

per

the per

dry of

cent

The

contained.

lower

The

in the upper are The capacity each.

per

section

six

and

is

cent

moisture

is 100

dry matter. originallydesigned by the writer

as

oven

The

matter.

contains

illustrated

is less

easily

grams

expensive and

It repairsthan the older model. built in the plantation shops, largely from

accessible for

more

is self-

heating-coils,

drjdng-tubes of 200

bagasse

oven

the

*

be

.

minus

may

old

material. dried be in Drying in Packages* ^The bagasse may with cheese-cloth or mosquito-netting. packages covered Several hours' heating at 110" G. are required to expel the Proceed follows: Weigh about a yard of finemoisture. as mesh including a few pins, and determine mosquito-netting, "

in

moisture

it.

about

kilograms of the bagasse, sampled as described above, in the netting,and pin 'it together and quickly weigh it on a good scale. Dry the package of bagasse to constant weight in the steam the

"""-

"

*

"--

Journ.

"

"

--

Ind.

Wrap

up

-t

' --

and

2

Eng.

--

Chem.,

-

--

June, 1910, 9t No.

"i-_,j,_

6.

_^^^^

DETERMINATION

OF

dr3ing-oven described

farther

the

transferred

package should the

awaiting the

The

this

is smaller

error

weighings

While

than

this introduces

would

moisture

of

is best

calculati""i oi the moisture

the

out directly to the scale with-

through absorption

case

making

In

on.

cooling of the material.

small error,

a

be

be

287

MOISTURE.

THE

otherwise

from

shown

air.

the

ing by the follow-

example:

pins. *

mosquito-netting

of the

weight

Dry

mosquito-netting and

of the

Weight

and

60

pins.

4

package of bagasse

of the

Weight

of the

weight

of

package

in the

bagasse and

"

"

"

netting...

i4

I*

"*"

bagasse

Moisture

2060

Tlie

2000

H-

of

the

in

1 gram

netting

964

grams "

of

cent

is

bagasse.

in the

moisture

large in

so

grams

bagasse used.

weight makes

the

""

4

per

quantity of bagasse

error

bagasse

grams

1096

960

=48.0

100

X

grams

2060

weight of the

=2000=

-60

9C0

t(

56 .

.

Moisture

Dry

grams

this method

an

an

.05 in

only

of

error

that

p"er cent.

for the

desiccation

Manifestly

a

metal

small

netting.

A

fall from

the

be

required

are

could

basket

be

substituted

for

the

quantity of bagasse-dust will sometimes

package, but shown

oven

hours

to

C.

affect the accuracy The

24

usually

110*

at

dryings by this method

the

that

and

complete,

very

shown

has

Experience

in

its

weight is

too

small

to

ciably appre-

of the test. is suitable

Fig. 82

for

in

use

these

tests. in

Drying as

containers

inches

by

1.25

bottom

brass.

and

The

110** C. and

of

"

bagasse.

holding

inches the

Shallow

Trays.

for the

balance

sugar

the

Metal

50

deep.

A

grams

The

tray is of wire

temperature

of

preferably 130" C.

the

metal suitable of

may

size for

be

use

used the

on

bagasse is 4 inches by 8

drying gauze oven

trays

progresses or

faster

if

perforated sheet

should

be

at

least

1 288

ANALYSIS

BAQASSE

AND

drying-otien. The

SUam

Fig.

OP

It

82.

is

drying-oven is

steam

"

CHIPS.

EXHAUSTED

conveniently constructed

most

shown

of

id

2-incb

Two steam manifolds, or planka of well-seasoned lumber. live used with steam to heat the coils,C, of iron pipe are

The

coils, instead

of two

use

pipe is suitable

iron

Half-inch

oven.

for

of one,

making

the

facilitates

coils.

regulating

the

temperature. Holes in the door of the

oven

D.

A

eir

wiirm

inserted in the shelf B. mesh

This

should

protected '

There

shelf

from

each

wire

a

other

the

near

The

screen.

parts should

be

the

usual carpenter's expedients. pipes, globe-valveson each of the inlet and tail-

coil,to regulate the

and

steam

the

dischai^ge

water.

moisture

tests, but DeterminatloD

Method.

"

The

serves

also in

of the

drying glass-ware, etc.

Sucrose.

Single-digestion

"

following is the usual method

the percentage of

capacity and add carbonate.

in the

sucrose

finelydivided bagasse 600

in cc.

a

The

long will

answer,

of

bagasse: Weigh

detfrmining 50 grama

dry, tared flask of about

water

reflux condenser, for which 4 feet

and

wall

be

of this type is a very convenient part of a sug"rnot only be used It may for latxHutory equipment.

153.

sodium

door

of

readily

can

oven

house many

air, and. the moist

hole in the

a

tray B is made

warping by be

of the condensation An

or

admit

thermometer

by boring

oven

be large. The

should to

at

escapes

at A

flask

and

2

should

purpose

a

cc.

of be

a

5%

1000

of cc.

solution of

provided with

small glass tube

about

a

THE

OF

DETERMINATION

289

SUCROSE.

gentleboilingand continue hour. Cool and weigh the flask and the heating during one Drain off a portion of the solution,clarifyit with contents. tube. dry subacetate of lead and polarizeit,using a 400-mm. in the solution is made calculation of the sucrose The by Schmitz's table,as described for use with dry lead,page 500. be clarified with a few drops of Or 100 cc. of the solution may subacetate of lead solution,diluted to 110 cc. and the the made usual by Schmitz's calculation of the per cent sucrose as With these very dilute solutions,the degree table, page 506. need

Brix

of the flask to

the contents

Heat

be considered

not

in the calculations.

of the to terms calculating the sucrose bagasse is illustrated in the followingexample, in which the in the bagasse is assumed to be 45 per cent: fiber or marc method

The

of

of flask +

Weight

"

"

"

bagasse +

620

water

bagasse +water fiber in bagasse thin

=

"

510

'*

50X0.45=

''

22.5

juice

of thin

grams

110

"

"

"

487.5

juice,Home'smethod,

179,usinga 400 2 (account of tube length)=2.2 and the tube =4.4; 4.4 cent corresponding, by Schmitz's table =0.57. sucrose in the bagasse is therefore 487.5 X 0.0067 per cent sucrose

Polarization mm.

page

-r-

per The

X2=5.56. A for

copper

the

convenientlybe

Fig.83, may digester, This

flask.

should

about

be

4

inches

substituted

diameter

by

that may be deep and be provided with a brass cover clamped to it,making a tightjoint. A brass tube attached A brass rod, carrying a a condenser. serves as to the cover 6 inches

small

extend

disk

for

above

mixing

the

tube.

purposes,

The

rod

should should

pass

be

through and moved

up

and

occasionallyeither by hand or mechanically. A Kodak veniently condeveloping-tank, fitted with a condensing-tube, may be used as a digester. should be added to the bagasse after startingthe No water digestion. The boilingshould be very gentle or, preferably, the liquidshould just reach the boiling-point. Rapid boiling, with consequent large return from the condenser,results in down

a

dilution

error.

2d0

ANALTBIB

OF

Repotted JHgttlwn bagaase

with

this

digestion

eight times.

Press

hydraulic

other

boil it durir^ ten

or

with

residue

the

and

press

with

and

water

Uttle

and

temperature

briug

to

water

unite

Clarify the solution

degree

Brix

by Home's

of this very

table

on

calculate page

500.

polariacope reading sucrose

the

If the should

is that of the extract,

peat Re-

spoon.

decantation in

a

Cool

the

in

to

with

divided

Con^dcr

may

tube

by

aid

the

be,

page

179.

be neglected.

600-mm. the

to

volume.

dry-lead method,

a

all

powerful

liquid

easily measurable

an

600-mm, be

iron

Drain

liquid expressed

dilute soluticn

sucrose

minutes.

bagasse

the

finely divided

it, adding, if need

Polarize the solution,preferably using

tube, and

an

the

of the

measure

it to

dish,preferttbt"

of

grams

portions already di'ained off.

ordmary

The

100

CHIPS.

suitable

a

liquid,pressing the bagasse

off the

those

In

"

cover

and

water

BXHAU8TBD

AND

Method.

porcelain caseerole,

a

a

BAQABSE

observationof

Schmita's

has

been

3.

This

the cubic

used per

the cent

centimeters

292

OF

ANALYSIS

BAOASSE

when not in top of the inner vessel,

at the

It should

cover.

not

CHIPS.

EXHAUSTED

AND

use, and

until after the

be removed

and

serve

as

a

completion

the

conclusion of the digestion weighing. and wipe the inner vessel and set digestionperiod, remove be cooled by placing it aside to cool and weigh, or it may the

of

as

in the

Norris

states

calculation

The

it in cold water. made

At

^

of the per

cent

sucrose

is

single-digestion method, page 289. of the vessel that the shape and dimensions

apparently influence the results. The vessel should not be The dimensions too deep. given are those decided upon by Norris after many experiments. of the Fiber Determination 153. (Mare)." The fiber be determined directlyas in the'cane, 110, but preferably may This method was adopted by the followingindirect method. comparative tests in by the author after several thousand The Cuban-American Sugar Co.'s laboratories: The required

data

are

Let

obtained

/Si=the P=the C=the

in the mill control. in the

bagasse; bagasse; per cent sucrose coefficient of purity of the residual juice (see dry

matter

in the

paragraph); cent fiber (marc) in the bagasse,

next a;=per

then

x="Sf-100P/C.

Steuerwald, of the Java of the various at the conclusion

and

methods

of fiber

alcohol-extraction

He

considers

methods

and

an

gation investi-

determination,arrived

that the indii-ect method

reliable results.

most

Experiment Station,in as

above

the claims concludes

gives the

of the .waterthat

the aqueous

give high figures,and the alcoholic extraction, correcting for the separation of saccharetin from the even fiber,gives low figures. ^The residual Residual Juice. 154. Purity of the is considered the juiceremaining in the final bagasse, juice,i.e., chemists to correspond in purity to that of the juice by many extracted by the last mill of the train. The experience of the truth. the writer indicates that this is near However, methods

"

since

the

between

bagasse receives its final and heaviest the juiceflowingfrom the last pair of rolls,

pressure

the last

probably

roll

the

through

them

is

analysis

The

weight

The

is the

usual

to

so

following

F

=

F'

it.

method,

in

fiber

the

fiber

the

weight

of

the

weight

of

thin

X

=

the

press.

the

per

cent

cane;

per

cent

exhausted

ization polar-

chips.

the

chips fresh

is

sponds corre-

estimated

by

considered in

it

and

cane,

be

may

found

is

cane

the

"

100=

the

hydraulic Consider

fiber

the

which

of

fiber

of

weight

This

heavy

well-drained

wei^^t

the

consider

the

i.e., all

Let

with

nearly

very

with

exhausted

in

juice

thin

the

of

the

press Ex-

passing

times

juices.

of

that

be

to

juices.

by

chips

powerful

a

other

for

as

juice

this

of

made

in

chips

the

press

at

pressure,

other

culating cal-

"

several

laboratory-mill

a

in

used

Sucrose.

well-drained

the

from

juice

thin

the

is

for

as

Diffusion-chips,

Exhausted

155.

made

is

analysis

The

fiber.

residual

true

juice

this

of

purity

of

coefficient

The

juice.

the

approximates

nearly

more

293

SUCROSE.

DIFFUSION-CHIPS,

EXHAUSTED

the

a

stant, con-

bagasse:

chips;

cane;

juice

in

chips,

the

then and

F'(a;+F')=100F of

Both

sampled, in

this

the

and

fresh

hence

calculatioQ.

juice

thin

the

direct

per

exhausted fiber

x

=

100

the

100F/r-F',

weight

cane.

chips detenninations

may

be

may

accurately be

used

OF

ANALYSIS

"

o! Waste

Analysis

156.

^The

polarizationof

requires

least

at

reasonable

attain

from

waters

waste

Diffusion

Water,

The

accuracy.

Prooess.

diffusion-battery

the

observation-^ube

50O-iiim.

a

WASTES.

FACTORY

in

order

to

after iOtration

waters

the use usually clear enough to polarize without As few plantershave polariscopeslong enough f op a mtist tube, a Ghezmcal method generallybe used. Concentrate the s"mple to 5 per cent of its volulne.

are

of

lead.

SOO-^nm.

.

the

by

sucrose

of

5

cc.

hydrochloric acid

of

means

acid. to

75

Nearly hydrate.

89).

in the

tion propor-

of the concentrated

cc.

the

neutralize

Invert

acid,

Determine

sample (see inversion^ with

after

the

late Calcuglucose formed. the glucose and multiply the per cent by .95; the result will be the per cent sucrose plus the small tity quanof glucose naturally present in the waste water. This sodium

quantity of glucose is be

may

The waste

small

too

to be

taken

neglected* Use Meissl and Weiu's of

prese?ice

is

water

an

aicpnsiderable amotint evidence

of

gross

of, and

account

table,l"age of sucrose

neglect

in

the

oa

189. the of

paft

the

batterymen. 157. Analysis of

current

of

from

Foam

compressed air,or

a

Sirups,

etc."

A

littleether

rapidly evaporated, liquid. Remove the

the foam to a quickly reduce ether by evaporation over warm water, at a safe distance from fire,and proceed with the analysis by the methods

will

described,beginning 125. 158. Analysis of the water

for

evaporated steam

the

Boiler

steam-boilers

from

condensed

the

juice and

in the

the

coils and

important

source

tubes of water

^The

feed-

largely derived from sirup. ^The water from

that

calandria

multiple effect,the calandrias and

is

Feed-Water.

and

of the

first vessel

coils of the

of the various

"

heaters

supply for the boilers.

of

the the

vacuum-pans forms a very

Sugar 294

may

ANALYSIS

OF

these

enter

the

BOILER

THE

through entrainment

waters

juice and

sirup and in the heating""urfaces. from

Sugar

the

causes

water

to

295

PEED-WATER.

with

the

vapors

through defects that develop foam

in the

boilers and

may

lead to accidents.

Further, though sugar may not be present in sufficient quantity to endanger the boilers through foaming, it is decomposed by tine heat into prodoets that are very detarimental

the

to

and

tubes

shells of

the

boilers,causing

pitting and overheating. The sugar is supposed to be first hydrolized,after which the dextrose and levulose decompose. The dextrose produces levulins,formic and acetic acids,and and formic acids and insoluble humic levulose,humic Both the acids and the insoluble humic compounds. pounds comHumic are injuriousto the boiler-plates^. compounds the

only when

form

for its action

the water

the humie

absorb

water

thin

Ammonia

retards

or

soda*. Except

forming humic compounds, injurethe plates.

hlgh-^essure boilers and'

compounds

with

the

monia am-

feed-

longer float,but deposit in non-conducting layers.^

which

threads

the hottest

at

into

ammonia

in

to

af^ear

introduced

Fats

form

levulose

on

does not

contains

the chemical

no

action whi(;h is most

vigorous

parts of the boiler.

position Sugar itself does not attack the boiler metal, but itsdecomproducts do, both chemiisallyand physically. The action has been explained. Some chemical of the decomposithe heating surfaces with oonse* ticm products deposit upon quent overheating and damage to t^ plates. The platesmay also be attacked by the acidityin the water derived from sulphited Juiftes.This "may b^^ prevented by the

addition

of soda

the

acidity of the juices.

Jt is evident

water

preferablyby reducing

or

thorough control of the feed-wat^r is The moment the best ^feguard against sugar. sugar appears .

the water

^

Osier

1912,

be

be turned' to the

thoroughly blown

should

below

as

a

this should

in the water should

that

to the

be used

at very

and in tracing the

.-Ungar.

14, 472.

Zeit.

down.

the boilers

The

"-naphthol test frequent intervals in testing

sources

Zuckerind,

and

sewer

1912,

of sugar

43,

397;

in it.

Int.

The

Sugar

odor

Jou^n.,

296

of the

the water

pronounced when

is very

steam

WASTES*

FACTORY

OF

ANALYSIS

contaiiis

sugar.

Qtuditativeand Approximate Quantitative Tests for Traces detected

quantity also

^The

"

sucrose

estimated

as

alcoholic solution of

cent

test-tube,then by means in 10 of the tube, run In the of

in the

circulatingwater qualitativelyby the o-naphthol method,

in Water,

Sugar

of

presence

demarkation

drops

5

of

may

be

and

its

20

a

pa-

a-naphth"d to 2 cc. of the water in a of a pipette,reaching to the bottom of concentrated sulphuric acid. cc.

sucrose

of the

Add

follows:

of

violet

a

Uquids and

two

the

at

appears

zone

line

gradually spreads.

of 0.1 per cent of sucrose, the color reaction In the presence is obscured by the darkening of the solution; with 0.01 ceut

per

color

the

si^crose

with

darknned of very wine; the entipe solution is colored. is that

O.OOr per cent sucrose, aoid used The in this test

be

strictlychemically and the a-naphthol should be of very good quality. solution of the reagent should be freshlyprepared from

pure

The time

and

to time

This 1

Ulac

is

test

the

be colored.

in the

"

When

test, and

is charred

sugar

-

solution

the

in 10,000,000 parts of water

sucrose

is shown

color

not

extr^nely deUcate.

part of

sucrose,

should

must

with

0.2

by the acid.^

a

A

tains con-

paleof

cent

per

I

and

similar

described was original method by Molisch.* Also the following: Thymol instead of rx-naphtholin the test yields a deep-red coloration,which on dilution with water gives at first a fine carmine, then a carmine flocculent precipitate.

possibly the

159.

Feed-water.* in

^This

"

for

Alarm

Automatic

alarm

is

Sugar based

in

the

BoUer

the

upon

change

It is comdensity of the water in the presence of sugar. posed of two communicating tubes (communicating vessels) within

one

tube

and

the

other.

The

flows through the

water

is stagnant

outer

at

a

in the

level.

constant

float a change of level in the inner tube causes close an electrical circuit and ring a bell. Since and

^

Rapp

*

Monatsch.

Besemf

Chem.,

elder, Deutsche 6, 198;

Zuckerind.,

1892,

in Jour.

Chem.

Abstract

923. I

Avertiseur

Lavan,

Ed.

Gallois, Paris.

inner

to

A

rise and

the

water

538. Soo.

Abs., 50.

COBALTOUS

is

the

of

NITRATE

corrected.

automatically

evident

increased

in

sp.

in

will of

the

placed

high,

the

float

1

free

be

should

possible

as

the

near

mm.

may

instrument

as

is

meters

instrument

the

location

density

1.5

lift

The

be

the

are

contact.

should

another

tubes,

gr.

sensibility the

Cobaltous

160.

1.001

the

bell

both

297

SUCROSE.

FOR

columns

convenient

a

A and

of

adjusting

vibrations.

pump

The

that

by

placed

be

solution

a

is

It

in

temperature

same

.therefore

TEST

of

feed-water

laboratory.

Nitrate

Test

Sucrose.^

for

^To "

about

15

which

is

are

sugars

soon

be

of

a

by

one,

and

distinguished.

such

as

of

subacetate

"

50

this

If

gum-arabic lead

Agricultural

dextrose

before

Analysis.

the

be

dextrin,

or

applying

H.

W.

the

Wiley.

two

hydrate.

When

9

the

with

lit,

ties, impuri-

alcohol

test.

Vol.

p.

the

dextrose

parts

with

two

is

sucrose

mixed

treat

color

turquoise-blue

by in

sucrose

sucrose

a

green.

produced

part

the

amethyst-violet

gives

light

a

tion solu-

cent

per

sodium

of

an

coloration 1

5

a

mixing

solution

treatment

into

of

cc.

thoroughly

cent

per

Pure

the

5

After

passes

mixed

predominant can

cc.

permanent.

which

color

2

gives

sucrose

add

nitrate.

add

solutions,

solution

sugar

cobaltous

of

"Pure

of

cc.

189.

or

ANALYSIS

MOLASSES

OF

CATTLE-FOOD

(MOLASCUIT).^

of tlie Moisture*

Determination

161.

of the food in

for

hours; cool in

10

and

the

note

the total los;sas

off.

This

weightof

the

ical supplies,form moisture

weigh.. before..

as

of

weight, driven

water

weight multiplied by 20 is of moisture in the sample. lead bottle-caps, used by dealers

The

granu)

boiUng water,

desiccator

a

5

drying 1 hour and weigh there has been only a slightchange

Repeat If

of

flat dish, at the temperature

a

Dry

"

the

centage per-

in chena-

conyenient dishes

very

determinations.

They

are

for

pensive inex-

very

8

sizes.

may

After

use

they

2

be

to

are

of

grams

of the

Etiier

Extract."

different

of many

be obtained

Determination

162. erate

and

thrown

away.

tlie Ash.

material

^Incin*

"

described

as

in

131. 163.

food, dried

the

of

161, The

with

extraction

Extract

described

as

D

is

flask

shown

connected

by

modification in

a

reflux

Fig.

cork

a

containing ether. with

The

tube 1

S

is sealed

Partly based

upon

into

the

methods

lower of

graph para-

a

Soxh-

85.

The

tube

a

small

tared

outer

tube

and

tube

A

closing the A

wire. small

Official Association

is .connected

the

from

part of the

in

of

with

condenser

percolator is prevented tube Z) by a spiralC of copper or

"

conveniently made

percolator,using Knorr^s let's apparatus

in

alcohol-free ether.

anhydrous

is most

to 3 grams

2

of

syphon-

percolator A^cultural

Chemists

298

300

Sucrose

166.

with

of

portion successive

filtrate

The

analysis

for

is

the

of

portions is

cooled

preliminary

in

tests

boiling

diluted

and

the

10 water

to

a

a

on

suitable

example,!

filter-paper.

volume, will

work

glucose

smafl

a

for

grams

187.

page

extracting

by

cattle-food,

in

given

prepared

glucose!

and

sucrose

methods

chemical

the

by

solution

weighed

500

indicate

ec

the

dilution.

proper

Notes

167.

and

^The "

The

The

Glucose.

and

determined

are

CATTLE-FOOD.

MOLASSES

OF

ANALYSIS

the

the

control

in

excellent

preparation.

on

tests

sugar of

the condition

Analyste."The

Cattle-food

are

usually

maiiufacture. for

required The

the

moisture the

by material

analysis,

without

factory is

usually further

in

DEFINITIONS WORK

AND

Normal

168.

Juice. assumed

to

These

normal be

the

Undiluted undiluted

or

juice

expressions are

USED

now

SUGAR

IN

APPLICATIONS.

THEIR

Juice.

The

"

EXPRESSIONS

OF

Absolute

Julee.

juice

originally

was

actually exists in the cane. applied to the juice extracted by

as

it

saturation of the bagasse. dry-milling, i.e.,milling without '^ The expression undiluted juice" is perhaps preferable to ''normal The

juice,"but long usage is known

cane

to

has established

contain

water

the latter.

that is free of sugar

If a piece of cane (lOB). This is termed "colloidal water." the rolls of a mill a part of this water be passed between In view of the exudes and drips from the end of the stalk. difficult to define the juice of this wBitet it becomes presence it exists in the cane, in the light of factory requirements. as the whole or normal For calculations based upon juiceof the it may

cane,

"

in

the

This the

be

well to consider

^juicesolids dissolved This

cane.

would

assume

solids be

may

be

this the

water-soluble

in all the

termed

that all the cells may

the

contained

water

"absolute

be broken

distributed in their liquid content.

stituents con-

juice."

down The

and cells

ruptured in milling,therefore the juiceextracted in dry milling can juice. only approximate the "absolute" This the inferential fact has an important bearing upon are

never

methods

all

of

calculating the weight of the

cane,

saturation-

juice content, etc. The customary use of "normal juice" jBS explained above is that employed in this book. The analysisof the normal juiceis calculated from the density and first-mill juice,and the of the crusher or mixed-crusher water,

mixed

the mixed

diluted

culated juice (109). A factor is calfrom the aensity of the crusher-juiceand that of the juicesobtained in dry-miUing. This factor is applied

purity of

or

crusher-juicedensity to ascertain that of the normal juice Crusher-juice Brix, 20^; mixed juice. Example: to

the

301

302

EXPRESSIONS

Brix, 19.7;

USED

factor

ratio

or

WORK.

SUGAR

IN

19.7 4-20 =0.985.

=

also page

See

323.

to indicate

used

are

it is finallymixed

as

Diluted

Juice.

Mixed

169.

and

the

Juice.

juice extracted

Megasse.

Bagasse.

sions expres-

all the

by

mills

to the defecation-staUon.

sent

juice is usually diluted witli the saturation 170.

These

"

This

"

This

water.

is the

expressing the juice from the is used in th^ English colonies. The Residual Juice. bagasse

left aft^

residue

woody The

cane.r

word

' '

'*

megasse 171. a

as

sponge

that absorbs and

retains

be

may

"

r^arded juice. The

part of the

a

ual" residjuiceso retained,the residue of that in the cane, is the juice. The true residual juicecan only be approximated and in the analysisonly the coefficient of purity of an assumed ^'

juice is determined.

residual

of fiber

the percentage In

cane.

train

or

number

the

purity

juice from

the true

as

the

in

culating cal-

bagasse and

the last nijill of the

the last roll of that mill is considered

or

is used

in the

marc

practice the juiceflowing from

coefficient of uses

This

to have

the

residual juice. The

same

writer

of the last mill in this discharge-roli

test.

Fiber

17;5.

of the

matter

Marc.

or

The

cane.

This

"

is

fiber

true

or

the

water-insoluble

cellulose is not

mined deter-

in the factory control.

Sirup.---The sirup is the concentrated juice of the

173. cane

from

^'meladura"

which

of the

''sirup'' has an it is applied where

has

sugar

no

been

extracted.

This

is the

factories. The word Spanish-Ammcan in sugar refineries opposite meaning solutions

to

frpm which

ha^

sugar

been

removed. 174.

Massecuite.

"

The

massecuite

sirup or molasses in which or

the material

has

the sugar

crystallize. Massecuites are numbers indicating their purity or 175.

sugar

that

are

has been

trated concen-

lized crystal-

point where designated by names or a

the number

of crops

of

to be removed. .

Molasses.-rWhen

the centrifugalmachine the mother liquor. This and is designated by names

the

been concentrated to

it will

crystalsof

is

a

massecuite

is ^un

in

a

crystals are separated from termed liquid is now ''molasses,"

sugar

and

numbers

correspondingwith

CIBCULATING

the massecuites. residue

from

'^

The

which

no

303

WATER.

final '^

more

be

can

sugar

is the liquid

molasses

true

or

removed, either

on

factory equipment or for commercial reasons. This is termed barrel-sirup in the refineries. ^This is the water used 176. in CIrculatiiig: Water. in the evaporation of the juice and condensing the vapors sirup. After leaving the condensers, this water, together with that derived from the. vapors, is usuallypassed over a cooling-tower to reduce its temperature, and it is returned to the condenser, thus circulatingthrough this apparatus. This water is often termed "cooling-towerwater." of

aocoimt

"

"

"

Sweet-water.

177.

of the

calandrias

^The

"

evaporator

condensed vapors often contained sugar,

in

the

carried

by entrainment, with the older types of apparatus. called "sweetThe water resulting from these vapors was though with efficient water,''and still receives this name, In refinerypracticeany very apparatus it contains no sugar. into

it

solution is termed

dilute sugar

Entrainment.

178.

from

vapors **

"sweet-water."

^When

"

h carried off with

sugar

the evaporators and

the

this is called

vacuum-pans,

entrainment." Coefficient

179.

of

Purity." The

usuallyappliedis the percentage

coefficient of

of apparent

solids (Brix) of the material.

purity as

in the

sucrose

parent ap-

coefficient is calculated

This

by dividingthe per cent sucrose, as ascertained by direct plying by the degree Brix of the substance and multipolarization, The calculated in this number the quotient by 100. coefficient of purity but only the apis not the true parent way of is calculated T he true coefficient purity coefficient. the

in

matter

determined

sucrose

as

method

are

term

from

'*

apparent

polarization. It is an

the

purity"

solid

of

and

the

Clergetor double"polarization industry is

sugar to

degree Brix

is well known

the number and that

approximate number, but

it is of great value

always be

by

in the

coefficient of

the

percentage

used.

general usage

The

the

by actuallydrying the material

ascertained

as

that

except

manner,

same

so

used.

in sugar

the

to

when

apply

calculated

sucrose

by direct

this coefficient for

manufacture

comparative and

the

so

lated calcu-

purposes

will doubtless

Frequently approximate data of the purity

304

USED

EXPBESSIONS

WORK.

SUGAR

IN

pf a product are required for immediate use, and as the factoiy wait for a tedious of determination superintendent cannot tedious double solids and an even polarization,he uses more the

coefficient, bearing in mind

apparent

allowances

Since

analyses be always conducted under be given the that due weight may other

the

On

special

in

used

at

omitted,^as is pften the

coefficient.

of two ''

word

should

true"

facture manu-

factories.

more

or

renderingwhat

case,

be

nevet

wotild

otherwise

useless.

^^ta almost

valuable

be

conditions,

different stages of the

the work

using this coefficient the

In

the

of purUy is only coefficient and in making comparisons

products

comparing

in

or

similar

very

that

true

researches

various

the

among

the

hand,

shortcomings.

it is adrisable

made,

be

must

its

expressions ''quotientof purity," ''degree of purity," often simply "the of purity," and quotient," "exponent The

the

and

With

"exponent"

using crystallizationin motion,

and

molasses

refening to this coefficient. of sugar-house work, "boiling in"

methods

modem

in

used

are

frequently required

coefficient is very

and

the

apparent

is of very

great

value.

Coefficient, Glucose

Glucos^:

180*

Ratio.

Glucose

Per - "

.

glucose

cent "

"

=r

-,

Per

is calculated

^This number

"

"

cent

X 100

follows:

as

"

,

"glucose

-.

Suerose,

100

per

": coefficient. ,

sucrose '

"

"

"

*

coefficient is useful

This

material

the

destroyed;

and

no

in

has

glucose

the

of

has been

sucrose

glucose

no

increase

an

detecting inversion

Provided

in the manufacture.

from

in

been

sucrose

separated

removed

coefficient

or

indicates

inversion. It is of both sugars *

181.

possiblebut hardly probable that by and

sucrose

the

might remain

quantity of

unit

per

sucrose

and

samfe

Coefficient.

Saline

relations

glucose the

"

saline

have

cent

of ash.

sucrose "

-r=r

Per

cent

z

ash

,. "

"saune

m

the

two

occurred.

coefficient is the

Calculoiion: Per

destruction

between

yet inversion

^The

the

t

,

coefficient.

Apparent

182.

the

noraial

183.

Actual

(Diffusion

Dilution

apparent dilution is the

305

DILtJnON.

APPARENT

that has been

of water

amount

The

Process)."

added

to that of the juice to increase its volume certain juice-contentin the diffusion-juice.This assumes a

to

cane.

Dilution.

milling and diffusion work

in

added

to

the

diluted

the

normal

of dilution.

water

of the

terms

in

179

to

actual

of

that tion, evapora-

reniove

the

preferablyreduced

to

juice,to

cane.

The

"

and

apparent from

derived

coefficients

all

the

Coefflcientis.

on

regard

is

number

density to

the

of the normal

This

weight of

Notes

184.

its

it represents

terms

both

is the percentage of water

and

juice to reduce

juice. Hence

in percentage

expression is used

^This

"

paragraph

coefficients

true

the

in

remarks

apply

to

"of sucrose,

percentage

degree Brix, or the solids by drying. According to usage, otherwise stated, the apparent coefficients are except where the

meant.

185" Available calculation

the that

Sugar.

of available

factory should

a

be

in the

or

sugar

able

to

given analysis. Manifestlythere control the

formulae

Several

"

are

in

use

for

the sugar it is assjimed lobtain with juicesof a

are

several conditions

that

able proportionof sugar that may be considered availof the machinery, viz. : the efficiency mill-juice,

intendent. quality of the juice,and the skill of the factory superof the In considering the juice,the quality of its impurities,as well as its richness,should be nature

the

into

taken

account.

A

grown

cane

on

certain

soils may

melassigenicsubstances than one of the same and equal apparent richness purity from another soil,and consequently the proportion of actually available sugar formula would indicate whereas a would be quite different,

take

the

more

up

canes

to be

Available

equal.

sugar-numbers

but

rough apprb^nmations ency except factoryequipment and efficitaken into consideration. The yield or recovery of are varies with the coefficient of purity of the juiceand the sugar for available sugar losses in manufacture, hence a formula when

must

The

the elements

take these elements

are

of the

into account.

practicalapplication of

available

sugar

calculations^

306

EXPRESSIONS

USED

except in estimatingreturn the present work

of

period or with that of SOU

and

organization. In this stock-taking, how

in

paring com-

factory with that of some ous previfactorysimilarlylocated as regards a

of value

are

it is desirable

event

in the

operated under

establishments

several

of

investment,is

new

calculations

Such

climate.

a

from

WORK.

SUGAR

IN

central

a

to know

trol con-

out (1) with-

nearly a factory is approaching its much efficiency; (2) how previously demonstrated sugar whether the factory is becoming is in process to determine requires either

congested and

of the process,

modification

much

(3) how

accounting

reasons

reduce

rate

the

closer

or

a grinding-rate,

supervisionof the

sonnel; per-

for commercial is in process or it is more (4) whether profitable to

sugar

and

grinding or

of

reduced

a

sacrifice somewhat

in

juice

extraction. Available is

cane

purchased

on

a

become

available

for

upon

sugar

factories.

The

industry

factory and

are

from

sugar

evidently

were

possibly that of these of

those

the

of

beet-

branches cane-sugar

fullyin the calculation

apply very

will not

production of

unlike

very

sugar

in both

conditions

when

necessary

analysis.

refiningexperience and

based

the

also

basis of its

earlier formulae

The

of

estimates

sugar

of the

cane.

following formula by Winter and Carp was published experience in Java, by Prinsen-Geerligs^ and is based upon which represents very favorable tropicalconditions: The

X

=

available

^=per

sucrose

cent

sucrose

cent

per

in the

cane;

juice in

terms

of the

weight of

the cane; C

="

coefficient of

the

purity of a;=/SX

To

calculate the available the value

juice.

(-f )

sucroee

"

to terms

of the available

by the polarizationof the sugar and multiply the quotient by 100. formula of The of Wint^-Carp-Geerligs has been found used great value in the writer's tropicalexperience. When sugar,

divide

^

of

International

x

Sugar

Journal, 6, 439.

308

USED

EXPRESSIONS

It should

remembered

be

liable to fluctuations

by the

than

of estimate

errors

"run"

that

date,"

"to

of two

WORK.

SUGAR

IN

as

figures are more they may be affected should

It

runs.

be

stated

operated beyond its normal capacity, factory was n umber froni thus necessitatingsUght changes in its efficiency that this

time s'

to

time. the

as

gar

is used

run

in

the

recovered

or

of

example

a

Also

previous

Betentlon

is the percentage of the retained

estimate

calculation.

for the

Sucrose

186.

the

the

of

available

efficiencynumber, for the previous

date"

"to

number

average

affects

This

in the

This

number

in the extracted

sucrose

in the commercial

the

juice that is ing In the follow-

sugar.

is the

balance, 92.32

sucrose

run

is used.

crop

Recovery."

or

first

retention

number: Sucrose

in the extracted

Sucrose

in the sugar

the extracted

juice,per cent

per

in the extracted Sucrose

.

in

sucrose

92 per

cent

32

6.58

press-cakeper in the extracted juice in the undetermined in the extracted

.

sucrose

juice.

in the

Sucrose

.

juice

in the molasses

Sucrose

100

cent.

cent

sucrose

.44 p^r

cent

crose su-

juice

100

66

Number. Efficiency Boiling-House Many factories use how retical to show efficiencynumbers nearly a theoThis number is usually yield of sugar is obtained. 187.

the

"

relation

percentage

recovery

available

number sugar

between

(186) and formula.

A

the

the

actual

number

retention

based

upon

or aa

part of the Winter-Carp-Geerligs

formula, 100(1.4"40/0), is used by the author in calculating Cuban- American the EfficiencyNumber of The Sugar Co.'s factories. This calculation is best illustrated by an example : Let the coefficient of purityof the raw juicebe 86.0 and actual retention number be 92.32, as in the previous paragraph, then 100(1.4-40/86) =93.49; 92.32-5-93.49X100=98.7, the number. A table is given on page 514 from which efficiency the

value

of

inspection.

100(1.4" 40/Purity)

may

be

ascertained

by

EFFICIENCY

BOILING-HOUSE

actually

available, in

the

based.

the

factory This

on

is

number

efficiency

The

as

it

takes

particular whose

number

of into

factory work

may

the

exceed

309

NUMBER.

in

value

the

account

as

calculating

with

compared

available 100

losses

in

sugar some

cases.

sugar

in

facture manu-

those fotmula

in

is

GHEMIOAL

CONTROL

SUGARrHOUSE

OF

Introductory." The chemical

188.

WORK.

control of the factory

is intended

along lines of

primarily to guide the manufacture best practice and to assist in detecting and

of sugar. The chemist

in the

reducing losses

factory corresponds with the auditor in

the

accounting department. He charges the superintendent with the sucrose material entering the factory in the raw and

credits

him

and the

control

that

leaving it in the products, byproducts, It is his duty to trace the travel of

losses.

and

sucrose

The

with

locate losses. the

of

milling considers

the

from

cane

its

delivery to the crusher to the delivery of the juice to the boiling-house and the bagasse to the fires. It is quite as important to ascertain the loss in the bagasse as to report the

extraction

engineer should reduction

locatingthe The

much

to

sucrose

consider

the

engineer. The

the

proportion of sugar that lost. The effort should as always be the of losses. It requires the assistance of the chemist

extracted

in

juice and

of not

so

of these losses.

causes

crystallizationof the

attention.

should

sugar

receive

constant

The

should purity coefficients of the massecuites be maintained at certain numbers, that the pan-work may and and that systematically efficiently no sary unnecesprogress work be thrown the crystallizers.This facilitates upon the

reservation

large part of the crystallizercapacity for the low-purity massecuites. The be must crystallizers controlled the best conditions to meet of equipment and manufacture. and

The it upon content

the

is often

sold

on

a

basis of its test,

control of the massecuites

becomes

of

importance.

quality a

a

Molasses

in this event

additional

sugar

of

of

the

sugar

basis of the most must

from

be

must

controlled

to

profitableanalysis. The

kept within

deterioration

be

certain

limits

to

maintain moisture

protect the

in storage. 310

311

INTRODUCTORY.

chemist is also the statistician of the factory. He

The

reports the quantity and

quality of the

materials,the

raw

and of analysis of the materials in process of manufacture the products and by-products. The chemist tistics staprepares that

have

of the manufacture Research Uie

and

or

with

is often

processes

both

necessitates

and

control

economy

the business of the establishment.

in connection

work

equipment

the

bearing upon

a

technical

and

the

improvements

called for and

chemical

in

this often

trainingon

the part

of the chemist.

laboratory should

The

all the

for part of the traiiiing-school chemist

methods, problems and

His

facture. the

a

superintendents. The

future with

be

control of the work

becomes

acquiunted

difficulties of the

should

mani"

familiarize him

with

details of the processes. The chemist's tunately training unforlacks the opportunity for practice in directing and This

controlling labor. the

leave

acquire A

a

that

samples

their

before

he

the

must

be

must must

be

highest feasible

be

must

integrity

methods

of

him

to

come.

must superintendent. He good .working knowledge of pan-boiling.

lesson

that

school

must

also

learned

early in factory control is representative of the materials and

be

unquestionable. Apparatus

adapted

to the work

is

accuracy

and

can

required,as

in hand. in the

Where

and the

testingof the

products, no detail should be omitted lead to dependable results. labor spared that may or The This following is an outline of the factory control. be greatly extended numbers by introducing ^Hrue" may materials

raw

instead appear

The from

the

of apparent for sucrose, etc., but in routine control; necessary

weight

of

this number

the and

this does not

usually

is

reported to the chemist and the weight and analysis of the raw

cane

juice extracted he calculates the the weight of the engineer and

superintendent. He must later the products, by-products and

mill-control sucrose

aecount

losses.

numbers

chargeable for this The

to

sucrose

mill

for the in

control

the analysisof the bagasse, and largely upon this analysis. in some cases, entirelyupon The juice is the starting-pcnntin the control of the raw Its weight and analysisare also elementsof manufacture.

depoids

very

312

the mill control.

WORK.

SUGAR-HOUSE

OF

CONTROL

CHEMICAL

in the

extracted weight of the sucrose juice plus that remaining in the bagasse is the baas determination of the percentage and weight of sucrose in the

The

The

and

caaie

analysis of the sirup

"meladura"

of the

of the

for the calculation

concentrated

or

the

of

ing entertion. extrac-

sucrose

juice,the

cane-

Spanish-American factories,is

the

trol con-

purificationof the juice and its evaporation, and results is a guide in the sugar-^boiUng. To obtain satisfactory in pan-boiling and to bring this work to as nearly a scientific and basis as is possible, the analysis of the massecuites molasses Massecuites is necessary are now usually boiled of the

.

Careful specifiedpuritiesby the injectionof molasses. control of this work is essential to a systeiraticgrading of to

the materials

the most

for

considering the

profitableextraction

tests factory. Control also often are required in the conduct of the crystallizers. The controlled both as products, sugar and molasses, are a

check

limitations

of the sugar,

and

manufacture

the

upon

the

of

to

meet

market

ditions. con-

cake is usually the only by-product whose filter-press be ascertained. Its analysis is usually hmited weight may of the sucrose, to the determination though occasionally The

controllingthe efficiency of the pressing and the quantityof water used in '^sweetening off,"or in reducing the cake for refiltration. the

A

solids

loss

of

determined

be

must

sucrose

temperatures

of

the

through

occur

may

multiple-effectsand

for

entrainment

of

knowledge

A

vacuum-pans.

in the

condensing and

the

condenser-waters

is

required in estimating this loss (313). In the

opinion of the author, many

losses in

apparently

manufacture

not

through inaccuracies

so

the processes

are

of

of the so-called mechanical actual inherent

the the

in

are

certain

of

analysis.

Except in very large factories,which force of chemists, a complete chemical The

losses, but

chemist

must

judge

can

from

afford

a

sufficient

contlrol is not

ticable. prac-

the

equipment of without decreasing

be omitted factory what work may tions efficiencyof the sugar-house. He must under all condihe detei^nine when properly, to some degree, may

WEIGHTS

AND

sacrifice accuracy for the sake of figuresfor immediate use. It is

just

control

arranged

be

in

the accounts

Measures.

be

it is

may Cane

of

pretense

measure

to

the

of the

bagasse and

mill

It is the

the control

the

in Cuba.

The

There

makers

the

to

to

leading scales

ton is

This

on

w^ght

custom a

factories

the

to

in

making

that

do

even

a

boiling-house,and

in

mill

this

control.

entirely upon the

the

In

a

analysis

Spanish pound in weighing reported in arrobas

are

{tondada)

contains

confusion the

on

in Havana

2000

the

of

pounds

part of scale-

Spanish pound, though

properly graduated.

are

gave

the

A

decree

of

equivalence

a as

100 kilograms, therefore avoirdupoispounds. Scale-beams

=46.0096

in Cuba

central

i^ould

use

some

=

It is the

with

equivalence of

pounds

Spanish

cane

reduced

weights, however,

Cane

weights

101 .4338 Spanish pounds graduated in Spanish pounds

the

weights and

juices.

Spanish Captain General 100

be

those

of the

depends

These

(libras) Sp.

few

are

control.

general custom

as

There

especiallyamong

control

pounds, Sp.

the

not

dispensed

be

event

25

all

applies especiallyiii Spanish unusual to find English and Spanish

chemical

a

may

cane

or

Weiglits

to

remark

cane,

essentia

not

are

system

same

Weights."

weigh their

not.

regard

in

be adopted ^ould weights and measures accuratelyas possible. A checking-system should the conditions of the factory and in so to meet in the calculations be possibleeliminate errors

devised

190.

MEASURES.

of

system

as

be

departments

indescriminately.

used

applied as far

AND

of the

This

system. America, where

same

be

of the various

It is quite essential that

"

should

measures

The

ical large factory, that the chemthe laboratory records well

Considerations

General

189.

units

promptly obtaining approximate

accimtte.

WEIGHTS

and

a

cctaiplete and

that

as

full and

important,

as

313

MEASURES.

and

scale

be used

use

the word in most

"libra." factories

inmiediately before

in the control.

to

reweigh

grinding it.

314

It

the

CONTROL

CHEMICAL

SUGAR-HOUSE

OF

beyond

through conditions that the weight of the

occur

may

chemist

WORK.

the be

must

cane

of

control

estimated

Small the factories,and even by an inferential method. in large piles, of Louisiana, often store the cane large ones ities liquidatingthese as often as is practicable. In certain localthe

is flumed

cane

call

special conditions should

methods

or

floated to the mills in water. for

and

statistical purposes

the

of

constituent

in

in

not

Inferential methods

factory.

inferential method.

an

used

only be

estimating the

the

serious

Such for

cane

control

of

require a knowledge of

that

.cane

These

be

may

traced

the

some

through the

The following millingprocess, e.g., the fiber,solids,or sucrose. example, from the records of a factory, illustrates aji inferential method:

appliedto the analysisof the give approximately the percentage of sucrose

Assume

juicewill

This

cane.

varies with

factor

and

content

crusher

factor which

a

the

variety of

the

cane,

It is smalls

milling conditions.

the

in the

with

fiber

light

heavy crushing. The factor approximates 0.85. with factors varying frozn a heavy crushing. Deerr ^ found

than

minimum

of 0.81

According

0.825. from

to

0.83

maximum

a

to

Pellet

0.84 and

to

writer has determined

the factor in

*

be

may

factors

and

of 0.848

as

low

as

low

as

as

Egypt

requiredof

Polarization Tons

0.80

in

very

extracted

sucrose

juice

in the mixed

Bagasse

18

45

.

juice. .305.7 11.3

cane

cent

per

cane

=

11. 3X100-5-48.

48.9 9=

Sucrose

in the

Sucrose

in the cane, per cent 18.45X0.80= in the bagasse per cent cane =23.11

bagasse, per

cent =

23.11 4.5 14.76

1.04

X0.045=

M^

I *

Int.

Sugar

Int. Sugar

1911, 13, 15. Journ., 1912, 14, 587.

Journ.,

The

large duty

.

in the

Sucrose

usually

0.80

i

of the crusher

of

Cuba, the low

(directtest) Fiber in the bagasse (directtest) Fiber

is

the crusher:

assumed

Factor

average

0.82 to 0.80.

being probably the result of the

numbers

an

316

CHEMICAL

CONTROL

a

free overflow

A

3-inch

''T"

The

is

;

service

the measured

and

should

conditions. volume

interference by

be

calibrated

Corrections

for temperature, with

foam.

with

be

must

water

applied

milk of lime added

to

and

the

for air juice. The allowance experimentally. It varies with milling

determined

conditions.

pumping

WORK.

suitable size.

a

air entrained

shouldbe

SUGAR-HOUSE

juice,without

measuring-tanks

under

for

for the

OF

A

tank

should

be

filled to

the

,

overflow

with

hours

few

juice and

its temperature

the temperature

be

noted.

After

a

and

shrinkage of the juice should be noted. A factor should then be figured from these data^ for change due to making allowance It is temperature. advisable to add formaldehyde to the juice to insure its preservation the period of res t as long as is pracand to make ticable. ihe juice moderately Occa"onally factories warm its way reduces the error due to the liming-tanks. This on .

of air.

entrainment

to

of the

The

method

juicefrom its volume factories

Many

defecators.

are

Such

given

compelled

is

of

should

which

tjbevessel is to be filled. of lime

to

measurement

block

the milk

wood

is

use

be

and

arranged

of

calculatingthe weight

on

page

347. the

measure

unsatisfactory.A

very to

juice in the

indicate the point

Correction

must

for temperature.

be made

to

for

It is customary

the heating surface is covered, juice the moment the reaching the "cracking" temperature about the moment defecator is full. This expels the air and gases which carry a part of the precipitated impuritiesto jihesurface with them. This, scum adds to the difficultyof making an accurate heat

to

the

The

rreasurement.

calculations

are

made

given

as

on

page

347. ii is tank

quite

is often

a

usual practice in Louisiana, whsre used

for

the

defecation

a'.ngle to clarification,

and

a

time in skinmiings.to remain in the troughs some with them; this order tQ separate the clear juice entrained into the defecator back and clear juice is finallydrawn of its volume. The account no being taken recladified, Yolvune of such juice should be determined, and average.

allow

the

calculatingthe net learn that.it is only by

deducted soon

that

he"

in

can

succeed

under

volume.

The

chemist

will

.

extreme

these

care

conditions

and

vigilance

in obtaining

MEASUREMENT

i'easonably accurate the

OP

THE

and

measurements

of

317

JUICE.

samples.

tion addi-

In

indicated,there is another due to the necessity of depending upon the workmen to keep of the number of defecators of juice. the count Automatic and counters be recording tank^auges may used in controlling the measuring-tanks. The recording check the a nd as a serves filling emptying of the upon gauge to

sources

error

tanks.

large tanks are used as in these processes it is well provide a printed sheet for each liming-tank,on which

When to

the

workman

and

when

should

he finishes

record

is correct, and

account

of the volume

of the

data

the

filled with

of tanks

number

juiceshould

time

when

he

begins filling

and the volume filling a tank

these

With

used.

lime

the

note

correction

of the milk

to

of lime.

of

ascertain

can

juice,whether

also the

also be

chemist

of milk

the

the

workman's

be

applied

The

on

temperatiu'e

occasionallynoted.

of the Juice. ^The juice may ing readily be strained through a perforated brass plate,containof the linkholes to the square 324 round inch,by n^ eans trash -elevators,now belt strainers and so generally used. AiUomatic

Measurement

"

thorough straining facilitates the measurement juice,though it will not usually admit of the use of This

automatic

The cold

juice,as it flows from of

sources

error

for such One meand

semi-automatic

or

of of

indicated measurement

thi^most a

apparatus such in Fig. 86. This

as

of

measurement

the

eliminates mai^y mills,, o^ the in the preening paragraph. Apparatus of the juiceis but httle used. "

of tanks

that

meters.

the

reliable methods

combination

of the

described

and

of measurement

automatic

an

farther

and

on

is

by recording illustrated

requirestwo tanks with an overflow from to the other, and very large dischargerpipes and one automatic registers, Ik" discharge- and preferably two be changed e^^her by h^nd or automatically. inlet valves may When changed automaticaUy the valves are operated by of electrical floats or by mechanism put in action by,means method

.

devices. a.

Measurement process cell. A

^The diffusion of the,juice in diffusionwork. of the juice from Qach requires the measurement

water-gauge

"

should

be

attached

to

the

measuring-

318

CHEMICAL

tank.

A

This

measurement.

exact

by

of

means

been

have

devised

method

register The

workmen

The

below,

take

pride

one

in

a

by

direct

ftll calculations

of

sugaf-house

of

locating

the

volume

errors

and

but

of in

the

amount

It

of

consists

essentially of A

means

of

a

free

float vrire

in or

of

errors.

erf juice is of

ia the

losses.

juice

the rate a

the chain

undue

only

of fuel.

baas

An

is of

not

illustrated

juice drawn, and

clockwork. oy

the cost

mcrease

convenient.

moat

record-sheet

preventing

Horsin-D6on,

of

the

weighing,

Irregularitiesof dilution sugar,

of

automatic

weight of the juice derived

or

its volume,

little juice.

the

together mth

is

The

great importance.

very

the

preventing

to

too

or

registration of tlie amount

automatic

of

sa.

suggested above,

described

view

a

much

too

Pta.

The

with

urement meas-

methods

raeasurenient

accurate

drawing

Several

float.

espedally

the

than

reliable

more

ordinary the

more

from

batteryman

is

an

for

but diffusion-juice, the

gauge-tube facilitates noting the

float in the

colored

WOBK.

SUGAH-HODSE

OP

CONTROL

cspedal and

of

value

losses

automatic

lilg.86,

with

a

drum,

ol

ratus appa-

registers the and

all delays.

recording cylmder revolved meaSuring-tank

in

tion. irregular dilu-

occasion

drawing

neariy edge knowl-

accurate

The

in

of

from

is which

by

connected revolves

WEIGHT

pinion, which

is attached

turn

THE

or

to

small

a

arm,

When

the

juice'enters the tank

drum,

and

by

a

line

of the

reason

the

on

parts, corresponding

12

each

part is subdivided

should

also be

may

attached

be

corrected

for

lifts,revolves

pinion the penciltraces The

hours

is divided

paper

of two

watches;^

The cylinder spaces. It is obvious that this

mill-work, in which

in

the

"

it

case

suitable measuring-tank.

a

its volume

juice from

be

to

Weight of the Juice.

The

and

hours.

used

pendL

a

float

the

to

carries

the

5-minute

into

twelve

every

once

instrument

the

rack

which

paper-coveredcylinder.

into

revolves

319

SIRUP.

is a falls; on the shaft of the dnun in revolving engages a rack; this latter in

float rises

the

when

OF

In

"

and

expansion

calculating the weight of should density, the volume

correspond with conditions of the graduation of the hydrometer. In using the Brix spindles,which are graduated to give the density of the solution at 17)^ C. as compared with water at this t^npera* ture, the volimie

weight

The

of

of the cubic

a

juice should be corrected foot of water

17J**C, is 62.2795

gallon,of whibh

there

These

may

numbers

juice under

the

lbs.,and

If

per

are

United

States

cubic

conditions.

hydrometers

ture, tempera-

foot,is 8.3255 lbs. in calculatingthe weight of the

be used

above

the

of

171" C.

to

the normal

at

that

7.4805

are

facilitate these calculations the

to

table

A

(page 495). graduated

is

the

to

given

to

temperature

adopted by the International Chemical Congress, The the volume to 4" C. of the juice should be corrected

standard

weight of

cubic foot of water

a

methods

The

of the

and

Measurement

193.

used

sirup is not

at 4"

C. is 62.3565 of

Weight

lbs.

the

Sirup.

juice apply with sirup. The usually required,except in taking for

of the stock of the material

sirup in his method

in process.

Deerr

uses

the

"

weight account

weight

calculatingthe available sugar.' in view of imIt is the present tendency of the factories, provements that have been made in the defecation,to hold the pan the sirup only long enough to meet requirements. of

of

" '

"

-

^The ftre *

iniervals between

termed

"

the

hours

6

to

12

a.m.,

watches."

Bui. 41. Hawaiian

Sugar Planters'

Expt. Sta.

12

to

6

p.u.,

'

"

etc.,

320

CHEMICAL

This

makes

OF

CONTROL

SUGAR-HOUSE

routine

accurate

WORK.

difficult

measurement

if

feasible. be

sirup miist

The

occasionallymeasured for the

in process

of the sugar

taking

in

account

this purpose the tanks should be gauged iEtndthe volume per inch of depth In these measurements it is more convenient be tabulated. the "inches

to note

and

out"

For

reports.

run

figurethe sirup in the tank

by

difference.

with

the

factories. direct be

weighing

observed

involved

Weight

of the

accuratelymeasure

Massecuites.

weigh a massecuite methods of manufacture prevailing in modem is discharged into the massecuite When cars,

is difficult to

"It

and

Measurement

194.

may

in

be

resorted

taring the

or

to, but

empty

cars.

special care The

must

labor

extra

the

in

weighing, and the difficultyin securing in most satisfactorylaborers, usually prevent this work factories. It is also

impracticable to accuratelymeasure it is discharged directly into the

when

mixers

weight The

or

can

The

centrifugal

Under these conditions the crystallizers. only be calculated approximately. (See page 345.)

in

the

mixer

and

especially in

should be made crystallizers immediately on massecuite,on account of its increase in volume or

cuite masse-

into

measurements

further

the

the

striking the after

stirring

crystallization.

measurement

only required

or

at the end

weight of the of

"

a

run"

or

is

massecuite

usually

period for calculating

In very quantity of sugar in process of manufacture. in these when measurements, large factories the errors of carefullymade, are so small as compared with the amount be neglected. in process that they may material

the

A

sample of

the

massecuites

should

be

drawn, when

ing, strik-

calculations analyses for use in making the necessary of and for the guidance of the sugar-maker in the conduct the pan-work. chemist should from time to 106. -Sugar-weights.-^The for

time^xheck per

the

package

may

scales

dry white

are

sugar,

weighing of the sugar, since a small error Automatic appreciably affect his calculations. coming i.e.,

into

extensive

granulated

sugar.

use

An

in

weighing

empty

ba^

321-

SUGAR-WEIGHTS.

forms

does

and

packages,

scales

with

away

for

allowance

other

class of tare.

reliable

weights. The workmen at the scales usually fill the packages to "down" weight, and where sugar is packed very fast this to a large quantity in the course surplus weight may amount the and add of to the manufacturing season, apparent

These

mechanical

give

using this

when counterpoise,

part of the

a

losses.

Dependable These

use

the

into

''dribble''

in

This

hour.

the nature

from

and

successive

method

is

very

"Libra"

be

Molasses.

scales

occludes

^The

urement meas-

ing by difficulties arisis very

Molasses

the containers,making uncertain.

tank

a

"

itself.

slowly from

Further,

considerable quantitiesof air. the

question of

definition

a

This of

the

gallon of final molasses. that

has

been

reduced

reboilingis readilymeasured

on

horizontal air occluded

page

in the 498

with

when

factory control. for the measurement

cylindricaltanks varies with

the

water

in the tanks.

weighed in tank-cars

importance

given

the

accompanied

in

of air raises

Molasses

its

and

of the material

measurement

commercial

is

drains

molasses

occlusion

should

type of these scales

bags of 325 lbs. of the of weighing reduces

of the

of the molasses

to

adjust the

to

80

Richardson's

loss.''

Measurement

195a.

heavy

than

sug^.

to regulate the flow of

quantity. One more

raw

in Cuba.

use

viscous

for

weighing-hopper and

accurately weigh per

made

now

are

arrangement

the

''undetermined are

scales

last small

or

sugar

raw

automatic

mechanical

a

sugar

will

very

preparatory Final molasses

possible,on A

account

table"

"wantage

of the molasses

(tank-cars). The

container,the method

of

amount

of

in of

filling period measuring. In an experiment by the writer,a molasses weighed less than 11 lbs. per U. S. gallon, measured immediately after filling and the air-free weight of the same tank-car molasses a 12 lbs. This indicates the importance of experimental was data as a basis of calculation of the weight of the molasses in meeting local conditions. A float measurement, using a float,is the most satisfactoryfor molasses stored in copper very large tanks.

it and

the

that

elapsesbetween

and filling

322

CONTROL

CHEMICAL

OF

MILL

Mill

SUGAR-HOUSE

WORK.

EXTRACTION.

quantity of juice or sugar removed from the cane by the mills,the mill extraction,is usuallyexpressed in two ways, viz.,(1) The weight percentage the cane of the mixed juice calculated to terms of the on density of the normal juice. This expression is gradauUy being superseded by the second, which has become quite in analytical and reliable through improvements milling extracted methods. in the juice (2) The weight of sucrose in the cane. This number of the weight of sucrose per cent 196.

its

Extraction.

The

"

only to the fact that it directly indicates the sucrose extraction,but also because it is less influenced by the variations in the composition of the cane. the direct analysis This number was formerly based upon ewes

of the

increasinguse

cane

or

a

upon

not

derived

number

sucrose

assumption that the juiceas it exists in the composition. (1) Extraction Juice. the

Divide

"

Weight Terms

in

the

weight of the

weight of and

cane

in the incorrect

cane

is of uniform

of the Cane

diluted

or

mixed

and

Normal

juice (169) by

point off for percentage,

to

tain ascer-

dilute extraction ; calculate the dilution per from the dilute (1H)7) and subtract this number

the per cent cent

cane

extraction

number.

juiceper

normal

cent

(2) Extraction in the Cane

and

The

in

remainder

is

the

extraction

of

cane.

PercentageTerms

the Extracted

Juice.

of the Weights of Sucrose Calculate

"

the

weights of

in the diluted

juice and in the bagasse. The weight of the bagasse is ascertained by subtracting the weight of the diluted juice from the sum of the weights of the cane and sucrose

saturation-water. extracted the

cane.

in the weights of sucrose in juice and the bagasse is the weight of sucrose The weight of sucrose in the extracted juicedivided

by that in the extraction

cane

number

the extracted

calculations

and

sum

the

in terms

of the

quotient multipliedby 100 is the of the

sucrose

in the

cane

and

in

juice.

(3) Extraction water

The

are

in

without Saturation. Dry Milling^i.e.,

similar to those of (1) and

of dilution need

"

(2) except that

The no

be considered.

methods Example illustrating

of

calculatingthe extraction:

324

CHiaMCAL

times

used

SUGAR-HOUSE

OP

CONTROL

supplying information

in

WORK.

adjusting

for

the

mills: Juice extracted

(per cent fiber in bagasse cent fiber in the cane)-t- per cent fiber in the bagasse "per is subject to error This method XIOO. arising from the difficulty experienced in sampling the bagasse as it passes Saturation.

198.

quantity of

An

weight of the to the

open

same

or

by

only

accurate

is sometimes

estimation of the water

^The

"

bagasse can

certaintyby weighing

inferential method

an

Imbibition.

used in saturatingthe

with

measurement.

the

=

Maceration.

water

determined

by

cane

mill to miU.

from

be

cent

per

similar to that used

in

made

estimating

Inferential m^^thods for the water

cane.

are

objectionsas those for the weight of the

cane.

The the

on

should

water

calculated

cane

to

over

and

in Java

it should

or

be

measured

and

culated cal-

percentage should be in terms

cane.

dilution in terms

The

The

actuallyweighed and its percentage

weight. The

weight of the

of the

be

of the normal

the Hawaiian

percentage of water

juiceis used largely

Islands to indicate the saturation. on

the

weight of the

cane

is also used

in Hawaii. Saturation the

per cent

cane

=

weight of the

waters-

weight of

XIOO.

cane

Dilution

juice (Brix of normal juice" Brix of diluted juice) -s-Brix of diluted juiceXIOO. There confusion is much sugar-chemists in the among nicthod of stating the amount ,of saturation-water used. The author suggests the adoption of the expression *'Per calculated from the density for the water cent dilution as of the juices,since this represents the water, in terms of the total juice, that must actuallybe evaporated on account per

cent

normal

=

"

of the

use

of saturation.

from *'Per cent

For

the

saturation-water,

its weight and that of the cane,

saturation"

house reports, in

or

''maceration"

the

as

culated cal-

expression Sugar-

is suggested.

the quantity of water used,should indicating employ both the expressions''Percent dilution" and. "Per cent

L

saturation."

control of the

The

of moderate

analysis of

The

work,

in its stead

or

the

pan

If

cut

strike is to

and

to

latter to

the

massecuite

be

drawn

of the desired

purity.

boiled,the purity of ihe above

be

of

that

a

juice,and that of the

the

of

daily routine

in the

made

as

quantity

produce

into

accuracy.

analysisof

the

indicate the

molasses

a

sirup

the

"

requires crystallizers

and

vacuum-pans

rapid analyticalwork

Crystallizers.

and

of Vacuum-pans

Control

109.

SUGAR-BOILING.

THE

OF

CONTROL

325

SUGAR-BOILING.

THE

OF

CONTROL

molasses

the

be

to

cuite masse-

boiled-in,supply

quired quantity of each of these reof a certain purity. These to produce a massecuite cient made calculations are by the followingformula, with suffi-

for

data

the

calculatingthe

for the purpose: accuracy Let 100=total weight of massecuite

purity of the sirup,or, in the

F="

that

of

case

left in the

massecuite

of the

strike;

in the

strike,

cut

a

pan;

boiled-in; p"puiity molasses to M*= purity of the required massecuite; a: percentage by weight of that part of the strike of molasses; to be formed be

"=

100

percent age of the strike

*-x=

from

or

to

be derived

from

sirup

previous boiling;

a

(P-M)

100 "*" ^"^

i"

r

"

V

proportionsof the materials used in making

The of

"

mixture

certain

a

also be quickly calculated by the purity may It is not feasible in pan-work method, page 347.

diagram to base

the calculations

actual

on

weights. The

approximate

densities of the massecuite to be boiled in

A

a

for example, and footing, should,however, be considered.

sample of the mixed

massecuite

lasses mo-

brought to the laboratory immediately the strike is dropped. A portion of this should be dissolved in water

Brix,'and

15" A

second and

its apparent portion should be the

should

the

to form

be

a

solution

of about

purity should be determined. fugal purged in a laboratory centri-

purity of the molasses

be

determined

as

above. If

dry lead defecation is used

in this

work, the labor

of

326

CHEMICAL

WORK.

SUGAR-HOUSE

OP

CONTROL

the apparent coefficient of purity may calculating 526. table, by the use of Home's page

be avoided

FiQ. 87.

The

puritydata

molassed samples be should to- the promptly sent superintendent and the pan-boiler. All mixed strikes,especiaUy those

of the massecuites and

purity, should

lowest

the

of

be

in this way. The relation the between purity of the

controlled

and

massecuite from

it in

the molaisses

purged

the

diately laboratory,immeafter boiling,is a valuable guide in boiling low-purity mixed strikes.

Convenient

are centrifugals in Fig. 87, and shown a filtering Thi" filt^* is indevice in Fig. 88. expensive

and

efficient. It is

very

funnel,'sparable at the ing. ground joint,A, to facilitate clean-

a

copper

The

filteringsurface is of oentrifugallining-sieve having about Pjq

braces.

625

round

holes

The

sieve

must

gg

TJie funnel

is used

in connection

per

be

square

inch.

supported by with a vaeuum-

327

INVERSION.

filtering flask with

the

or

yields

good

indicates

the

Inversion.

200*

the

from

sion, and

which

varies

little if any

is

in

limed

neutrality

to

changes

aUy

Inversion

the

inversion to

the

of

The

phenol.

some

adds

weaker

organic acids

of the

inverting with

inorganic salts and latter feebly, exercise an

salts

Many

alone

The

in

the

of

of

equal parts

The

ulose.

the

defecation,

levulose

and

and

the

dark

products. of the

whether

indicate

"

of the

In cane-sugar in

brevity

the

action

on

sucrose.

invert-sugar,* is

two

viz.

sugars,

these

is often

more

color

has

the

products

has

usually

in this book.

place and

other

called

the

56.

the The

composit de-

position decom-

no

glucose

wiU or

lev-

alkaline

to

been

examination,

invert-sugar are

in the

of the ratio of the

taken

in

heat

juice is due

there

and

decomposed.'

noticeable the

of

and

posed com-

in page

given

lime

in part

is very

dextrose

:

are

sugars

by the

upon

inversion

Juice and

all.

organic acids, though

of

juices,etc. under

this expression is used

great rapidity

inversion,

Provided

manufacture,

or

air.

glucose,a comparison

sucrose

gradu-

water-solution, but

of this sugar

decomposition defecation

acted

are

raw-

juice is

in

properties of

sugars

In

greater

a

scarcely at

invertive

sucrose

of

presence

product of

These

will invert

the

by all acids, to

mineral

inver-

to

condition

alkaline

sucrose

is caused

sugar

delays, there

since

sucrose,

of

and

rapidly

of serious

event

neutrality in the storage-tanks.

degree, the

Heat

due

sucrose

to

less

the

loss of

a

white

the acidity of the juice.

with

factories,except

sugar

of

manufacture

is often

there

cane,

the

In

"

control-tesJls, will

the

and

pans

these

sugar-boilersare obtaining the material are capable of yielding.

whether

indicate

results

best

low-purity massecuite

a

with

work

following the

usually

When

poor.

the

will indica^^^e whether

immediate purging, it high-purity molasses, on boiling. A few days' experience with the poor

a

pans,

factory.

of control

or

is made

Connection

plate.

the

of

this method is

pap-boiling

bell-glassand system

vacuum

often

Very

a

to

usually

not.

reducing

gittCose, and

The

stances subfor

828

CONTROL

CHEMICAL

difference

between

inversion

in

except

From

the

above

in

the

general

a

materials

raw

detected,

however,

and

be

will

loss of

that

detected

It

glucose usually be

and

can

balance

often

not

sucrose

estimated

and

sucrose

products.

losses

as

of

measure

a

"

quantities of

and

percentages

the

always

cannot

not

way.

renoiarks,it is evident

through inversion from

glucose ratios is

the

WORK.

SUGAR-HOUSE

OF

one

another. In

of inversion,

using the followingformulae,for the calculation the

above

inverted

Sucrose

should

considerations in

the

be

evaporation

kept in view: etc.

"

The

inversion,

^

in

except

diffusion-battery,may

the

formula

following extended Louisiana Let

Experiment

Dr.

calculated

William

by

Stubbs

Station: unit

of

juice;

6=

glucose per

unit

of

juice;

c=*

sucrose

per

unit

of

sirup

or

massecuite, etc.;

rf^

glucose per

unit

of

sirup

or

massecuite, etb.;

of

juice (nounds);

sucrose

=

^=the

s

total

total

=

gf=

the

of the

per

a

Let

of

be

weight

removed

sucrose

(pounds); total glucose removed (pounds) ;

a;i= total inversion; a;2=lossin concentration

in the

sugars

and

by

losses

in the

sugars

and

by

losses

of the

sirup

juice to

or

1st

^

massecuite; afj" loss in concentration

of the

juice to massecuite.

_^^E(ad-ch) -\-cg-ds] ^^^

""''

100c

(2) When concentration reduces

neither of

sucrose

+ 95d

nor

glucose is removed,

jiiiceto sirup or

1st

95^(arf-c") "2

= '

100c

+ 95d

in the

massecuite, the formula '

to

as

329

INVERSION.

(3) When the

and

there is

formula

in the sugars,

glucose removed

no

reduces

^"0,

to

9^E(ad-ch)-d8] ^'"^ 100c + 95d

following generalformulae

The

Clements,

B.

formula

U.S.N.,

modifications

are

of

by Lieut. Dr.

A.

Stubbs'

:

'

"

"

"

"

(1)

for inversion

inverted

af=sucrose

cent

per

in the original

sucrose

juice; "S=

sucrose

i7=

in

removed

sucrose

in the

rj"per

in

in sugars

by

and

glucose in the juice-f- per the juiceX 100; cent

cent

losses per

cent

the originaljuice;

cent

r2=per

per

originaljuice;

glucose removed sucrose

by losses

and

sugars

glucose in

etc., -5-per cent

the

cent

massecuite

in

sucro"e

or

molasses,

in ditto X 100.

sucrose

^lO0(r^-r,^g)-r,S 10000

i"""" =

105.263.

95

(2) Multipljdngthe above equation by a, the per in the originalsolution,we obtain x in terms sucrose the weight of the juice;

cent

of

rz-Vr+g-rJS x=^a-

10000 95

(3) Calculation re

=

inversion

/^i*=percent in

^,=per

per

cent

sucrose

in terms

of the

glucose:

juice; in

the

juice-5- per

cent

glucose

ditto; cent

4-

of inversion

per

sucrose

cent

in

the

sirup

or

massecuite, etc.,

glucose in ditto;

in the removed "S3=sucrose glucose in the juice;

sugars,

etc., per

unit

of

330

"7ji=glucoaeremoved

WORK.

SUGAR-HOUSE

OF

CONTROL

CHEMICAL

in the

of

unit

etc., per

sugars,

glucose in the juice; 6"glucose

juice.

cent

per

Xf^b

100^

100 1.05263. 95 901.

the

for

Formulae

Calculation

the

of

in

Inversion

Diffusion-battery.^ in the

diflfusion-juice

pe"

cent

sucrose

per

cent

glucose in the diffusion-juice

per

cent

sucrose

in the

normal

juice

per

cent

glucose

in the

normal

juice

per

cent

glucose in the diffusion juice;

'

"

6= x=b

"

=inversion

~7~"

1+

in

the

'

battery

cent

per

Fjj '

"

95

diffusion-juice. (2)

cent

a=per per r

=

in the

sucrose

in the

diffusion-juice

sucrose

in the

diffusion-juice

glucose

in the

normal

sucrose

7"7 m

glucose

cent

^

X

'

'

per

cent

per

cent

per

cent

-^

r2=-

x=a

diffusion-juice;

"

!"^=

100

'

'

juice

p^-T-XlOO; the

in version

normal

juice

in

battery

the

per

"

cent

Jiffusion-juice. (3) [p" (100" e)P].9j"xe=in version

diffusion-juice. p=per glucose juice; P""per cent *" Fonnulas

(1) and

(2)

are

cent

in

baaed

the

upon

in

the

glucose normal Dr.

battery in

juice Stubbs*

-r-

cent per-

diffusion

100;

formula.

e

=

332

CHEMICAL

CONTROL

OF

SUGAR-HOUSE

apparatus, conveniently arranged

of

the

at

If the

sample

with

ends

cups

at

systematicallythrough

go

factory drawing samples measuring the quantity of material

juice,.etc., and

the the

various

should

begin with

the

manufacture.

of

stages

juice and

the

all material

include

must

ments measure-

midnight, for example, the '^^ant,and the laboratory helper, provided and a measuring-rule, should at that time

ass.

an

noting the

for

stations.

factory day

chemist,

WORK.

This with

end

in process,

at

stock-taking

the the

even

of

and

sugar, in

sugar

the

convenient the to measure centrifugals. It is usually more depth of the empty space in the tanks, rather than that of small measuring-cup for samthe liquor. By using a very pling,! cupful) for example, may be drawn from a. quarter one of a tank of sirup,two cupfuls from half of a tank; and so on, thus forming a composite sample that will represent the

If the

accuracy.

each

from

drawn

estimated

of

and

in

material

be

with

the

of

the

sirup in

ascertained

from

value.

sugar

beginning

and

in the pans. until the

the

of

vessels

of

time

to time

as

the a

quantity

is in

be

may

The

use.

measured

may

when

be calibrated The

season.

be

density

should

evaporator

be

guide in calculating the

.

with

Thus

the sugar

molasses

be used

they reach and

quantity

constant

a

apparatus

the

By prcfarrangement sirup (meladura) and the stock

the

or

of

degree

sizes,the

apparatus

multiple effect tanks

at

the

fair

a

accordingly. multiple effects should

the

considered

when

liquidated into water

sirup with

of different

are

juice in

run, the

the

be varied

may

to

run

tanks must

(volume

The

from

of

composition

average

to

these the

may

be omitted

as

such

complete strikes of massecuite massecuites

or crystallizers

molasses

boiler,certain tanks of

be

need if

not

be

from

then

measured

immediately purged,

If separately considered. this arrangement is not feasible, the sugar boilers should,at the depth of sirup and molasses the whistle signal,note in the tanks and -indicate the approximate depth of -massecuite in the pan by chalk marks. The condition of the massecuite should be noted or, preferably, proof-stick samples should be drawn for anedysis. The quantity of sugars in thecentrifsugar

may

BUN

333

REPOBTS.

ugals,hoppers and bins should be noted,ftlsothe last serial package number. Stock-taking in if the above

a

When

the

be followed.

scheme

accurate

as

largefactory need require but the stock taken

were

as

report is called for

run

stock-taking

to include

be

known

factory will be shut down day later for cleaning or other reason.

a

that

are

tically prac-

a

certain

date,

should facilitated^

work

may

results

during a shut-down.

the

or

of

The

utes min-

few

a

the

it be

day in advance

a

In this event

the

ground before or after the date is either carried as stock and figured to sugar or its product is deducted the case as require. may data and samples and the Having secured the necessary be made analysis of the latter,the calculations may as cane

follows: Juice

and

"

ahead

of manufacture

estimated

be The

from

available sugar

with

the

Since

Sirup.

juicehas

all the processes sugar value should

raw

it,its commercial the previous experience of the factory. of

method

given.on

page

305 in connection

number be used. If there is no record efficiency may of the previous experience of the factory, the yield may be based calculations by the commercial formula, upon sugar the probable or an estimated 342, taking into consideration page an

loss in

especially to figures are

the first run

more

These

manufacture.

of the

accurate, and

remarks

apply

factory,after which there is

further

more

the

run

experience in

the

factory to guide one. A slightlyhigher yield may be expected from the sirup than raw of its having been purified. This juice on account is also true of the clarified juice. The table,page 515, is a convenient

guide in making these estimates.

Massecuites boiled

without be

may

and

Sugars. "

the

calculat"ed

addition as

in the

^If the of cases

massecuite

has

molasses, its sugar of

the

juice and

been value

sirup.

If, however, molasses has been boiled-in or mixed with the in crystallizers, the following fcmnuia should be massecuite used: Let

a?=per

cent

of commercial

obtained B

from

(sugar-value)to be the massecuite; sugar

""degree Brix of the massecuite;

334

CHEMICAL

Let

CONTROL

P"

of the massecuite; polarization

p=

polarizationof the commercial

S

fiolidsper unit of the commercial

w

WORK.

SUGAR-HOUSE

OF

sugar; sugar;

ssooefficientof purity of the final molasses.

M

lOOP-BM Then

x

= .

p-SM V

This

formttla

gives

Brix and

true polarization,

calculated

It will be

With

results differ but

that

noted

in these

calculation

If,however,

is

the

true

low-purity massecuites, the actual yield

little from

If but

simply

gra-de of

one

to know

it

as

of values

is

simplifies

is made,

sugar

grade is made,

one

final molasses

the

is advisable

substitution

a

than

more

purity of

This

estimates.

calculations.

the

the

centrifugals.

at the

used

when

used.

purity are

polarization,etc.

apparent

only

For the purposes it is usuallysufficiently the to use accurate

of the estimates

the

results

accurate

the

in the formula.

e.g., 96"^ugar

and

in what

2ds, it is necessary proportions these sugars and made, allotingits proportion to the 96" test sugar are

reducing the remainder In reporting estimates in addition and

second

sugar

for the

period or run, it is customary general statistics of the manufacture

the

to

of the

terms

to

the

analyticaldata,

per

cent

report the

to

yield of

sugar

follows:

as

1st sugar tyj

Total

Total

The

tt

It

It

tl

t(

"

*'

"

"

''

"

since

in

in the

sucrose

juice.

ii

It

tl

tt

tt

tt

tt

*'

*'

"

"

tt

tt

tt

tt

tl

"(

occasionallyreported as follows: of sucrose in the juice.

is also per

cent

It

it

tt

tt

"

"

"

"

order

figuresmust polarization.

very

a

to

statement

be

be

the

The

of

H

is not

This

cent

per

H

Ist sugar

Total

retained

sucrose

it

sugar

nj

cane.

tt

1st sugar, t\J

of the

tt

^"

**

f*

"

*'

''

""

satisfactorystatement comparable with those

reduced

to

terms

of sugars

of of

the other

of the

yield, runs same

'

,

giving the

sucrose

retained in the

conuner-

^ LOSSES

OP

SUGAR

IN

THE

335

MANUFACTtTRE.

in the juioe"6ho\vBat a cial sugar per ceht of the sucrose glance, in comparisons, the relative quality of the woric.

Final

is in very generaluse. In msaiy factories that are

of statement

form

This

molassea,

"

favorable

located at

markets, the final molasses

a

distance

from

to

this only oheok the chemist has upon Where the molasses is his analytical work. is which into lai^getanks, from shipments are made

waste

material

pumped from

of the

time, data

to

composition

run

the

and

time

are

often

may

be

total volume

obt^ned.

and

average

It is often diflBcultto

accurately distributingthis product the various runs, or periods. among The average composition is best ascertained from analyses of samples of each shipment, but in addition to such anal"iGies of the molasses as frequent control-tests should be made the weight of the it is puniped from the factory. Where molasses is ascertained by weighing it in tank-cars, these should them, as owing to cars always be tared before filling molasses workmen of the the the viscosity frequently fail the tanks. to entirelyempty of In the Manufaeture. Losses ^The 203. Sugar information

secure

for

"

usual

of loss

cake, and bagasse,filter-press in the evaporation. through decomposition and entrainment Other are by inversion, fermentation,and possiblesources sources

are

so-called mechanical

the

in the

or

undetermined

losses.

bagasse. ^The loss in the bagasse is calculated from estimated weight of the material and its analysis.

The the

The

"

weight of the bagasse is between

often

estimated

as

the

ference dif-

the

and that of the weight of the cane normal juice. This does not usually give a correct result when saturation is practiced,since the bagasse may leave the

third mill heavier than

it would

be otherwise.

In

this

if the

be known, the weight of the saturation-water bagasse is the weight of the cane + weight of saturationwater" weight of the mixed diluted juice. It may that the weight of the saturation-water is occur case

not

known.

used. B

In

Fiber

bagasse

per

this event

per cent

cent cane.

cane

an

inferential method

be

fiber per cent bagasse uncertain quantity in this

XlOO-^ The

mu^t

calculation is the percentage of fiber in the

cane.

336

FUter-pressCake,

BUQAB-HOUSE

OF

CONTROL

CHEMICAL

^The loss of

"

WORK.

is calculated

sucrose

from

analysisand weight of the press-cake. The from weight of the press-cake is usually estimated of several filterthe actual average -weight of the contents this is not When a practicable, the cake from presses. of the press is weighed from time frame or single chamber the

time

to

obtain

to

an

weight and

average

this

niimber

is

of cakes in the press, to obtain multiplied by the number lbs. the total weight. The cake weighs*approximately 60-62 per

ft.

cu.

is

There

loss of

a

This

cloth.

filt^

It will vary to 0.6 lb.

or

with

the

unknown

filtercloth.

per

more

Inversion.

usually included

the

by

methods. quantity varies with the filter-press from almost nothing with double filter-pressing

This

losses.

is

juice absorbed

in the

sucrose

Inversion

"

estimated

be

may

by the formulse

glucosehas been destroyed. It may also be estimated by reducing the analyses to a dry basis. For example: A sirup has a coefficient of purity of 86, that on

327, provided no

page

is 86 per

of its content

cent

massecuite

evaporation to indicates

that

0.5 per

cent

This

inverted.

or

is sucrose; falls to 84.5.

of solid matter

after

the

This

purity

of its solid matter

has

been

the solid matter

assumes

to

stroyed debe

a

constant.

is

Glucose

usuallydestroyed when

therefore materials balance

be obtained

can as

actual

well

as

a

sucrose

to

some

in the

extent

facture, manu-

calculated

weights of the it is preferable to figurea glucose balance to obtain light on the or

losses. used in Changes in the saline coefficient are sometimes tracing losses either by inversion or mechanically. Zimmer^ based upon the persistenceof certain mann suggests a method

page 349.) the ash and beaker in the

and

throughout the manufacture. {Se^ the the determines He sucrose by Clerget method

soluble

of the

salts

sulphated ash. He transfers the the lime,etc.,with ammonium precipitates as

presence

of

ammonia,

then

washes

out

and determines sulphates left in the precipitate

"^Int.Sugar

Journ., 1914, 16, 383.

ash

the

their

to

a

oxalate soluble

quantity

TEST

by- difference.

BOOKS

AND

calculations

The

337

RECORDS.

illustrated by

are

of

one

examples: Mill-juioe* Sucrose, 10.5 per cent; soluble sulphates in the ash, 0.31 per cent; 0.31 : 10.5 1 :x and x"33.87, the ratio for juice. Sirup: Sucrose, 46.3 per cent; soluble sulphate in the ash, 1.38 per cent; 1.38 :46.3"1 : y and y 33.55, the ratio for sirup. The change in the ratio from juice to sirup is 33.87" 33.55=0.32, corresponding to 0.32 per Zimmermann's

=

s=

unit

sulphates. Then

of loss

33.87

:

0.32

100

"

:x"0.94,

per

in the

juice. This is evidently a very exaggerated example. The soluble sulphates are much higher than the usual total ash and the cent

on

sucrose

loss is excessive. this class of

This

is

method

to call attention

quoted

to

investigations.

ErUraininent.

^The loss

"

by entrainment

be estimated

may

This loss is estimated from the by Norris' table,page 434. and its analysis of the water flowing from the condenser weight as calculated from the temperature changes and the instructions evaporated. Detailed arc quantity of water

printed with

the table. LABOBATORY

Test

204. a

Books

set of books

and

FACTORT

AND

and forms

RECORDS.

Records. without

It is difficult to

"

plan

knowing something of the

needs

of the owners, the force of chemists available for con^ trol and whether this control is to be partialor fairlycomplete. The

reports include:

usual

slip for the Manager, Superintendent and Engineer, giving preliminary data of the mill work and control analyses of the juices,the output of and

sugar

the fuel

(1)

consumption;

A

this should

be

supplemented the analysis of the

by frequent reports to the Engineer on (2) The preliminary report should bagasse. what include the

termed

be

may

data

statistics.

This

losses.

methods

(3) Run

of all data

including

a

The

''operatingreport,''which

covering the entire line of chemical

manufacture.

r^sum6

an

be followed

sucrose

data

should

mill and

reports at stated

collected balance

shot^idbe

of manufacture

include

and

both and

for the a

full

should

control

and

ing manufactur-

intervals,giving a run

statement

enough

supply the

by

owners

to

and

date, of yield and to

indicate a

the

permanent

338

CHEMICAL

record

CONTROL

of methods.

OF

SUQAR-HOUSE

Working and

lost time

should

also be

portion of the factory's capacity is being utilized. in (4) Laboratory records: (a) Used the (b) Extraction analytical work, figures, etc (c) Records of pan-work, (d) Unit^book, used in recording the m quantities of materials, products and by"^roduots and

reported to

indicate

WORK.

what

calculatingweighted Printed

routine

forms

averages.

should

be

laboratorywork.

supplied for

the

entries

in

the

large space should be provided in these forms for the figuringwith a view to tracing errors. The of printed fonns also promotes use systematic work. A

loose-leaf binder

should or

in

be used

is convenient

each

specialbooks

It is advisable

A

day. and

All

never

for these

figuringshould be

on

and

forms on

a

sheet

the sheets

of paper. forms for calculatingand

scraps

have

printed recording mill data, operating and lost time and fuel consumption. A special blank should be posted at the mills fen* reporting the delays and their causes. These figures should

be

to

tabulated

from

time

to

time

for the

use

of the

Manager and the Chief Engineer. The daily laboratory reports, for a fairlycomplete control, should include: (1) Analyses of the diluted,normal culated) (caland residual juices. (2) Fiber and socroee in the cane. (3) Analysis of the sirup. The Brix is for the control of the evaporation and the purity coefiicient for that of the defecation. and molasses (4) Analyses of the massecuites and the work to control the injection of molasses oi the and polarization of the sugars ciystallizers.(5) Moisture The moisture has a bearing on and occasionallyash tests. of the sugar; the polarizationmust the storage qualities meet market requirements; the ash is an additional check upon the of the juice. (6) Analysis of the final m"^as8es purification General

to

meet

ma[rket

lizers and to

control

conditions

and

to

control

centrifugals. (7) Analysis the

loss of sugar.

the pans, crystalof the filter-press cake

(8) Analyses of the

bagasse

frequent intervals, indudmg moisture, fiber,and sucrose (9) Frequ^it examination tests, for mill control. of the the for feed-water for sugar, protection of the boilers. (10)

at

Entrainment

tests in the condenser

water, to protect against carelessness in the evaporationand in the pan-boiling.

CALCULATIONS.*

SUGAR-HOUSE

Introductory.

205. the

chemist

to be

All materials

"

dealt

with

and

by the

composed of sucrose non-sucrose, latter including water, dextrose,levulose,organic non-sugars, are

(ash). Certain of these (marc, etc.) and inorganic matter substances persist throughout the manufacture, others through but one or two stages of it. A knowledge of the proportions in the originalmaterial,prodof these substances ucts by-products, is the

and

basis

algebraicequations,with which

construction

of

yields,quantities,capacities,

calculated.

be

etc., may

for the

the purposes of the usual calculations,in addition to the proportions in which the various constituents are present, For

certain

relations

required, such

often

the

between

constituents

themselves

are

saline coefficient, purity coefficient,

as

constituent of a simple when the original material practicallyunchanged through passes the processes, e. (/.,the fiber in dry milling.

problems

The

etc.

are

very

illustrates the principlesinvolved following formula The water used in in many of the sugar-house calculations.^ dilutes the extracted saturating the bagasse in milling cane The

juice; the of

means

based

equation

an

this dilution

of

percentage

upon

(Brix) of the extracted normal the diluted juice: m Let

100

"

6== B"

100"

a;

=

x

=

the

is fact

ascertained that

the

(undiluted) juice are

by solids

present

weight of diluted juice; degree Brix of diluted juice; degree Brix of normal juice; weight of dilution-water in diluted juice; the weight of normal juice, the

then 100

6=B(100-a;) *

The

mark

and

"

/

a;

"

=

100-100fe/B

is used

to

indicate

=

100(B-6)/B.

division.

340

FOBHTTLA/

DBT-MILLINO

341

is the usual dilution formula and is used because it is

This

the diluted

juicethat

is

weighed

measured.

or

The

value of

multiplied by the percentage of dilute juiceextracted from the cane gives the dilution in terms of the weight of the cane.

X

In

similar way, calculations may the dry matter of the cane,

a

of the

of

constituent Since

of the

numbers

press-cake,the ash

or

a

them

upon

ascertained

analysis

are

calculasugar-house tions approximations, but are usually

for the purposes

sufficientlyaccurate

in sugar

of the results of

absolute,many

based

the fiber

upon

it,etc.

many

not

are

be based

of the

manufacturing These considerations apply especially contnd. to massecuites in whose molasses and be analysis absolute results cannot expected. full work

The

deducing

of

the formulflQ is

followingparagraphs, with

the

in the construction

necessitated

of formulae

to

that

not

are

given

that

or

are

by specialconditions. Fonnula*"

Dry-milling

206.

view

a

usuallygiven in the beginiier assisting

The

fiber

or

is the

marc

constant: Let

weight of the bagasse from

F=the

percentage of the

s

2=

a;

cane;

B "the

F'

(1)

weight of the

the

100=

=

percentage of

in the bagasse;

marc

(2) F'S-IOOF;

100-B;

X

=

100

-

of J3

in

lOOF/F'

(/S07) is noticeable.

whence

B"100F/F';

(1)

100(F'

=

similarityof this formula

dilution

cane; in the cane;

marc

percentage of juiceextracted;

substituting the value

The

100

and

This

F)ir.

-

that

should

be

calculating

for

e2q)ectedsince

(Brix) is diluted and in the other the constant (marc) is concentrated, i.e.,its percentage relation increases. to the bagasse as compared with cane

in the

one

307.

the constant

Dilution

FormulaB."

of the mill- juice in terms

The

formula

of the diluted

been

given in the Introductory (205)

and

the

followingdilution number

or

To

for the dilution mixed

reduce

juices has this number

.

to

percentage

terms

of

342

SUGAI^-HOITSS

of

it vl necessary to multiply the values ively. by the percentages of diluted and normal juice,respectThe dilution per cent normal or undiluted juice is

weight of the

the X

CALCULATIONS.

calculated Let

100 B

X

weight of normal

the

=

6

follows:

as

"

=

=

cane,

juice;

the Brix of the normal

juice; the Brix of the diluted juice; percentage of dilution in

the

of the normal

terms

juice, then

the solids

of the diluted

(Brix) of the normal

juice,6(100+ar) This

weight

100+aj=*the

100

=

B and

is used

niunber

in

juice,and

juiceare =*

x

certain

100

countries

all

in the diluted

found

B/6-

100

sinc^

100(5-6)

=

indicate

to

/6. the

that has been used^ though quantity of macerr.tion-water th"%t has passed in fact it only indicates the part of the water into the juice. Concentratloii and Formulae." 208. Braporation formulae

These

in the

derived

100

Let

6

same

then

100!"

The

those

for dilution

and

are

weight of the juice,etc.;

the

=

the Brix

of the

Brix

juice;

of the concentrate;

percentage, by weight, of

=

the

=

(100-x)B,

(5ee(311.) is derived

evaporation by voliune

of

percentage

evaporated;

water

whence

100(5 -6)/B.

x=

to

way:

=

B^the X

similar

are

as

follows: Let

100 h

B X

then

=

the volume

of the

of the

juice,etc.;

"

the Brix

"

the Brix of the concentrate

=

the percentage,

g

specificgravity; of G

by volume, of

specificgravity;

water

evaporated;

100^6, and

GB(lOO-x) x=^lQO"gh/GBf =

juice of

the

volume

of

water

evaporated.

(See 312.) 200*

Commercial has

a

wide

Sugar

Formulae."

(A)

This

application in the sugar-house control

mula forand

required in crystallisers, capacities

estimation of the

the

in

313

FORMULA.

6U0AB

COMMERCIAL

etc. :

x=the

Let

percentage

yield

commercial

of

of

sugar

polarizationand S per cent dry matter; 100=: the weight of the primary material (massecuite, molasses,etc.)of P polarisationand B per cent p

.

dry M=

purity of the residual molasses; in the molasses; the weight of sucrose

coefficient of

P"px/

100

B"Sx/

100

then

(Brix);

matter

=

the

=

weight of dry

(Brix) in the

matter

mdasses.

Since

the

coefficient of of

percentage

sucrose

purity of

in its

dry

a

matter

sugar we

material

is the

haye

B-Sx/lOO' clearingof fractions,transposing and reducing, lOOP-BM X-

p-tiSM/100' yield of

the sugar

of

100"

commercial

sugar.

as polarisation/

refinery work, the formula

reduces

^"*

If the is

product is refined

customarily assumed

in

to

'

100-M

(B) This

yield

of

formula

sugar

percentages in Let

X

=

from terms

is

applicable in the calculation

massecuites,.molasses, etc.,and of the primary material.

the percentage of commercial eoefiicient and

sugar

of P'

of the

gives

purity

dry matter; the weight of primary material, P its coefficient 100 of purity and B its degree Brix; Af sthe coefficient of. purity of the residual molasses. s:

6 per cent

of

344

calculations.

0nQAR*HonsE

BP/IQO

Then

6x/100

^

the

weight of

=

the

weight of dry

material;

in the

suorose

in the sugar;

matter

I

"

P'bx

_P'

1006a?

X-t:^

^^

the

=

,^^^^,

sucrose

^,

the sugar;

m

10000

100

100X100

.

.

,^ of^ wei^t

weight of solids in the mohisses;

B"bx/lQO^the P'hx

BP

weight of

the

=

in the molasses.

sucrose

10000

100

precedingsugar formula, an equation the coefficient of purity of the residual molasses As

in the

clearing of fractions,transposing and

x^lOO

X"

in the

It is derived

dry

and

let the other in the

x

the

=

matter

dry

matter

take a

above sugar

fonnul"

way,

but

letters have

the

ceding. pre-

is based

upon

cane

The

of

same

meaning

"

=

P 100--

of the

-M "

dry

",

matter

the

per-

in the

apphed in the calculation of the or

''

the

(B),

juice,but

the losses in manufacture

estimate^

in terms

sugar

(Brix)of the residual molasses;

in terms

be

may

the

from

into account

correct

same

whence

centage of anhydrous sugar primary material.

yield of

applications as

previous formula

P'a;-M(100-a;)-lOOP,

The

same

(Brix) ,in the 4"rimary material,

the

as

"

have

we

b

percentage 3deld of anhydrous

Let x^the

100

reducing,

materials:

moisture-free

Then

the

has

formula

upon

is formed:

.

P'-M

(C) This

based

it is necessary to in order to make

available sugar'' formulse (185)

CRYSTALLIZEB

since they take the losses suitable for sueh estimates,

more

are

into

345

CAPACITY.

formulse

These

consideration.

find their chief

uses

in

the yield of sugar in process in massecuites,etc. calculatinfi; The commercial ^10. CrystalliKer Capacity. sugar in used the in f ormulie be estimating required capacity may and molassescertain machinery, notably pans, crystallizers "

tanks, using

solids and

true

in accurate

sucrose

to estimate

work.

quantity of crystalluEer massecuite of 94*^ Brix and 60" purity that would be produced clarified juice of 20" Brix, 18 per cent sucrose and 90** from sis purity, the sugar that has been extracted having an analyof 96" polarization and 99 per cent dry matter: Using it be

Let

formula

required

(A), 1309,

the

have

we

100X18-20X60 ,^"^

X

16.39

=

=

96-99X60/100 sugar

80

solids) matter

13.11

contains

juice

The

The

cane.

therefore

matter,

-V-

ceot

per

sugar

on

16

"

12.98

then

cane,

12.98

=

="

16.39 X. 80

contained

sugar

X.99

juice. Let the juicebe 99

dry

dry

cent

dry

cent

per

cent

per

per

13. 11

=

sugar.

(Brix

matter

3.02, the percentage

of

dry

going into the crystallizer massecuite; 3.02

cane

massecuite

the

.94 =3.21,

of the

20 X. 80*= 16

and

cane

on

weight

weight of the

of the

cent

per

the

of

cent

per

cent

per

Massecuite

cane.

of

lbs. per cubic foot, therefore 3.21 cubic feet massecuite 100 lbs. cane, or -^ 94.4 =0.034 per Massecuite swells considerably, cubic foot per ton of cane. 0.68 Brix

94"

owing

certain

diluted

of volume

0.68+25

from of 25 per

should time so

we

of its crystallization

the

to

of be

94.4

weighs

time

(see page

98) and

time

page

(see

the decomposition

it should An

95).

is safe allowance

cubic

and

for

also

increase

alteration,or

Further, the massecuite the crystallizer about four days, the ii;L

=0.85

remain

have

to cent

per

cent

de:"ending then

salts

sugar

upon

the

0.85X4

feet.

size and =

3.4

type

cubic

of the

feet per

crystallizer, ton

of

cane

is 1850

tons daily milling capacity. If the milling capacity the crystallizer capacity should be 3.4X1850=6290 of cane will depend upon size of the crystallizers The feet. cubic

the

size

of

the

vacuum-pans

and

under

the

usual

con-

346

SUGARHttOUSB

CALCULATIONS.

of 12 feet in diameter

ditions with' pans

striking1000

cubic

1250 cubic feet,would be approximately 1000-1-25 per cent of crystallizers 5 -f, the requirednumber feet; 62904-1250 Allowance to actuallyhold the massecuite. aJso be must mJade for one and to receive massecuite empty crystallizer to be dischargingto the centrifugals, or in all 7 cr"'stalone lizers of about 1250 cubic feet gross capacityeach. This estimate is based upon juice of exceptionallyhigh purity. In actual practicethe estimates should be upon the juiceof the lowest purity that is hable to prevail over extended periodat any time of the manufacturing season. an The lower the initial purity,the largerwill be the quantity massecuite. In actual estimates the true of crystallizer soUds and purityshould be used to avoid errors. Mixed of Massecuites. 211. lasses MoProportion and Sirup. These massecuites should be boiled that desired in the moto a definite purity,depending upon lasses =

=

"

obtained

be

to

from

them.

This

formula

that the densities of

sirupand molasses are the is sufficiently accurate for practical purposes: {A) Let

100

=

P= p=

M

=

x

100"

=

"=

assumes

same.

This

weight of massecuite in the strike; purityof the sirup; purityof the molasses to be boiled4n; purityof the requiredmassecuite; perc^itage by weight of the strike to be formed of molasses; percentage by weight of the strike to be derived from sirup, total

100{P-M) then

aj

=

P-P This is the

formula

purityof

may a

be

appliedwith less accuracy

footingor nucleus

upon

which

a

when

P

strike is to

completed with inolasses. be made with greater facility (B) This calculation may ^ method for mixtures,illustrated in the diaby Cobenze's

be

"

Vta

L

A.

Cobenie,

Nottrand's

der prakt. Photografio., 9th Compendium Annual, 1913, p. 563.

Chemical

ed., p. 379;

j

348

SUGAB-HOUSB

CALCULATIONS.

of measurement;

reduce

the

degree Brix of the juiceto that at the temperature of measurement by means table of corrections,page of Gerlach's 489. Apply the Brix corresponding to this reduced specificgravity number perature at the temto the weight of the cubic foot or gallon of water temperature

of measurement.

Example: 15** Brix

at

Required the wdght of 17.5717.5* C. measured

Degree Brix

of the

Hydrometer

correction

cubic

a

foot

of

at 28** C.

juiceat U.S'' C (page 489)

juice of

15.0'' 15** Brix at

for

28*C

7

corresponding specificgravity at (Sp. Gr."1.05831)

Degree Brix and 28** C

Referring to the table

14

3**

449, a cubic foot of water measured at 28" C. weighs 62.1289 lbs,,therefore 62.1289 X 1.05831 =65.75 lbs.,the weight of juice required. The is well within the limits of accuracy of this simple method error of

at

tank

preferable that all measurements made is be practicable,the temperaat, as nearly as ture of graduation of the hydrometers, thus keeping all errors

minimum.

a

*

Calculations the

used

in

Ash

assumed

and

mineral

to remain

comparison

whether

Based

the

upon

Sucrose,

etc.

Relation These

"

tween bemethods

ascertainingwhether sugar or other matters are in a boiling decomposed and removed ])rocess, for

destroyed or example. The a

page

It is

measurements.

214,

are

on

of

constituents

unchanged the

has

saline been

cf

the

during the

coefficients

materials

process,

are

therefore

(181) should

show

destroyed,and

similarlywhether have been other constituents method A of decomposed. this class must be used with great caution,since very slight lead inaccuracy of analysis or loss of mineral matter may to

an

sucrose

conclusion.

erroneous

should be used

in

The

true

or

Clerget number

comparisons. numbers are Example (allsucrose by the Clerget method) : A clarified juice containiog 15 per cent sucrose, 0.3 per cent ash and

sucrose

50 saline coefficient

was

evaporated

to

sirupcontain-

r RELATION

BETWEEN

50.7

ing

cent

per

coefficient

of

in

less

what

finding

is of

the

and

in

This

sucrose.

juice

is

decrease

coefficient

original

coefficient

the

the

0.29,

saline

a

saline of

sucrose

cent

per

the

the

of

decomposition

of

terms

percentage

coefficient,

saline

indicates

ash

cent

per

349

SUCROSE.

AND

reduction

The

"0.29,

by

ASH

1.02

sucrose,

49.71.

50"40.71

by

THE

in

in

50,

culated calthe

this

case

0.68.

has

method

This

in

manufacture limited

the

C.

sulphates

soluble salts

which

addition ashless

filter

matter

is

an

removed

of

pnd

ash The

sulphates.

I

Xnt.

Sugar

with

The

difference

16,

is

residue

calculations

J.,

is

are

(1014),

made

383^

also

the

storage the

only

since

through

the

with

the

tran^erred and

ash

to

the

an

soluble

water.

The

residue

between

the

original

hot

the

the

of

usual

as

what some-

method,

persist

ash

The

is

utilize

this

ashed

is

washing

this

in

formed

are

in

to

filtering-crucible

alundum

by

ash

cane-sugar

part

a

and

proposes

acid.

weighed.

and

dri(^

weight

or

of

surface

material

sulphuric

of

deposition

sulphated

and

application

*

they

The

manufacture.

is

the

beet-

its

but

evaporating

of

from

the

Zimmermann

A.

H.

in

used

losses, of

fact

the

on

tanks.

the

estimating

by

constituents

been

long

weight as

this

of

the

p.

336.

before.

work

soluble

EVAPORATING

AND

O^

DISCUSSION

JUICE

HEATING.

METHODS

METHODS.

CALCX7LATION.

OF

BY

H.

W.

Prop.

General

Conslderattons."

low

used

the

At

"

based

Dean

pressures

Regnault's

on

Department

op

New

University,

Tulanb

Technology, 215.

Creighton,

P.

Orleans,

-^tyipora^n

in sugar

house

should

377

page

assume

given

of

water

on

the

pressure

will be

pressure

the

by

below

217a.

Variation

Purity.

The

"

with

A

^^^

jj

217b.

A,

portion of

corresponding In liquid mass.

portion of

sugar

inaccuracies of

mass

a

as

sugar

due

to

the

the

portion considered.

surface

the

of the

entire

of

depth

the

mass

portion

of

with

Temperature

boiling-point of

the

in

is indicated is

as

Density

in Gerlach's in the

sugar

table, page

and tions solu454.

following table:

Brix

60

Fahrenheit

5.4

Centigrade

3.0

boiling point of

The

a

the

to

density,its viscosity and

surface. of the on

It is usual

liquid'ssurface.

variation

density

Degree / Degree \ Degree

Table

as

any

serious

to

a

its

that

general, the variation

In

leads

pressure

the

considered

which

at

entire

boiling of upon

absolute

increased

of the

depend

will

such

Solutions."

will boil is that

of

solution

or

tables

Sugar

temperature

assumption

temperature

This

of

surface

the

this

solutions the

the

on

pressure

tables

used.

that

mass

of Water.

calories,

Only

use.

Point

Boiling

216. to

for

be

.

formula

605.4 -fO.305 T

inaccurate

too

are

La.

the

work

H=1091.7+0.305(r-32)B.t.u., U^

op

solutions

sugar

is also

enced influ-

by their purity. 218.

Elftect have

increase

the

of

gums,

Viscosity. mucilages

viscosity of

the 350

In

"

and

the

raw

other

fluid.

juice

we

compounds As

anything

times some-

which which

EFFECT

the

Impedes

tends

surface to

easy

of the

escape

produce

to

that

see

the

from

bubble

steam

heating it is

local rise of temperature,

a

sirups will have

gummy

boiling than

of

351

VISCOSITY.

OP

puce

higher temperature

a

difference

The

solutions.

sugar

is uncertain.

the

At

with

Vaiiatioii

219.

low in

pressures

used

pressure

produce

tmder

than

far

which

at

For

of 2

will change the pressure inch.

head

a

pounds

at

141.8*

145.8"

F.

solution, without

difference

this

there

is

temperature

as

of water.

We

case

and

between is

values

boils at 125.5**

.03

solution whose mean

F.; imder

of vacuum, have

we

it boils

a

ture tempera-

heating

the heated

to

temperature, to

"*"

we

20.3*"

similar

a

lost

liquid that

see

in

F., difference

condition

in

the

degreesin temperature

Sugar

a

solution

sugar

equation of to those

30 .86

Solutions."

40 .79

may

be

its specificheat

70 .58

.65

of tlie

Liquid."

specificheat

is

To

raise TF

C, from

temperature, tt,requires

TrC("j-"i) B.t.u.

a

hence

readilyfound:

60

50 .72

relation

straight line and

a

below

and

The

80 51

.

Heat

square

to

of

of

20

....

Specific heat.

per

their effect.

the

Degree Brix of 10 solUitioii

a

pounds

shall call these

density of

the

intermediate

tu to

3.4

compared

Specific Heat

expressed by

2I^1"

to

loss of 145.8"125

a

later will discuss

21d0.

square

the

from

upon

in

(50.6*') inch, corresponding

'produce boilingin the sugar considering at all the effects of viscosity.

depends case

is 26 inches?

vacuum

per

water

required

transfer of heat

As

What

of 2 feet of solid (no

per square inch, or 23.8 inches Add for density 4* F. and F.

3.4

ferences dif-

portion of sirup of

pounds

vacuum

26 inches vacuum,

At

of

"^

inches

26

to

ferences dif-

sirup of specificgravity 1.236

of 2 feet of

head

small

example:

small

bubbles) sirup in the third effect if the A

work

larger temperature

a

50.6'' Brix will boil if it is under

Surface."

the

house

in sugar

high pressures.

be the temperature

wiU

Below

Depth

pounds of

mean

"

90 .44

a

.37

sugar

temperature,

362

EVAPORATING

Thus,

raise 10

to

HEATING.

pounds of sirup at 60" Brix from

leO**

temperature,

JUICE

AND

F.,

to

116 B.t.u. require 10X.58(180-160) and Sohitioifts 22^. Heat To Sugar

would

mean

180**

temperature,

mean

a

a

F.,

=

Water.

The

"

temperature

the

imder

water

of

Evaporate

risingfrom

as

that

When

the

same

pressure.

same

the surface

reaches

the

will be

solution

sugar

of the vapor

from

boiling

pure

superheated bubble

boiling sirup it loses all

a

boiling

a

excess

heat

temperature in vaporizing its watfery envelope. To raise Wi pounds of juice from a mean temperature, ii, temperature, fe,and evaporate Wt pounds of water a mean

and

to

temperatiure, tst corresponding to the .presaire at the surface, requires WiC(ti-ti)-^WiLiy where Lt is the latent at

a

heat In is

correspondingto

of water

h is greater than

where

cases

negative and

fe,the

quantity WiC(ti"ti)

be subtracted.

must

Condensate."

223.

h-

In

condensing

in evaporators

steam

that the condensate is work, it is usual to assume to anoth^ removed at the boiling point. If taken place of will give to self-evaporation and it will tend less pressure in sugar

pound

if W

another

to

is condensed

of steam

units in its

thermal

equal

vessel

where

is

steam

of normal

maceration used

water,

is

tanks

and

a

it is usual

removal

evaporated

into

the

give

Thus,

up

condensate

condensing W(ti-U) Heated.

at

WLi is led

a

lower

B.t.u. "

The

(mud

amount

amount

or

the

of water

oachaza).

In careful

experiments, weight of the purified juice to

from

that of the

dilution

as

juice,taking

raw

indicated

by

the

sities. den-

juice varies with the milling and the manufacture; methods also, with the equipment total weight of liquid to be heated of the factory. The The

or

dilution

concentrated

of

weight.

by evaporation in the various

of water

heated

consideration

if the

defecator-bottoms

calculate the or

its

increased

be

cake. with the filter-press to

loss in temperature

by the of lime, wash-waters, and

must

milk

diluting the

in

There

be

juice

cane

up

to be

Liquid

of

Amount

the

at "i, it will

vessel, and

own

temperature; fe,it will there give 224.

to

multiplied by

condensate

the

in

units

of thermal

number

a

up

usually

the

ranges

from

about

90

to

110

per

HEAT

353

LOSSES.

The mean weight of the cane. evaporation in the multiple effect in tropicalfactories approximates 78 per cent by weight. is not only lost from Heat Losses. Heat 225. the heating vessel itself by radiation but is lost from the pipes conveying heated liquid. Steam condenses in steam-pipes idle. The loss of heat is not negligible when when the even conducted. heating or evaporatingis carelessly Transfer Coefficient of Heat 226. (K)."The unit of heat transfer,called the SpecificThermal Conductivity,is of ihe

cent

"

of

number

the

the steam for each

thermal

units

transferred

hour

per

from

Uirough the heating surface to the sugar solution tween degree difference of temperature, Fahrenheit,bethe

and

the steam

solution for each

foot of

square

heating surface. for heat

formulas

The

involve this unit which

transfer have

may

are

simple, but they all value

any

between

1500

B.t.u. per hour. Experience and judgment requiredto select a proper value. Some of the variables and

B.t.u. are

50

effectingthe value of this imit are: (1) The velocityof the steam past the heatingsurface; of the sugar solution past the heating surface ; (2) The velocity (3) The presence of air or other incondensible gases; (4) T^e character and thickness of the depositson either both sides of the heatingsurfaces; or position (5) The surface pressure and the depth, densityand comof the sugar solution being boiled. transfer of heat is the transfer of vibration

The

deadening which rate

should On

no

and lowered

be swept aside to allow the the

sugar

solution

must

be

moved is

heating surface,as steam is

results in less.

have strudc the Rurf ace

bubbles

steam

the vibration

longer any

doubt

as

or

a

poor

to

the

cules mole-

their vibration cules. mole-

new

heating surface,

swept heat

thing any-

Steam

impact of

side of the

and

away

from

conductor.

existence

and

the

There

enormous

importance of surface films of gases, where the heating fluid is a gas, or of a vapor having air-containing films,as in to

effects,which

ance magnify incalculablythe resistthe transfer of heat through the metal plate. Smith

condensers

or

hJ

354

EVAPORATING

found of

that at 90"

1/20

cent, and

of air

reduced

heat

3/20 in.

the reduced

mercury

transmission

in the tube

water

to the

Ps

represents the

of

the

partial

HEATING.

JUICE

F. the presence

in. mercury

that heat

says

AND

partial steam and

steam

with

the

and

power

25

per

Orrok

cent.

(p^) where ,

and See

pressures.

the

Pt

sum

'^Vacuum

In the steam belt shown in Fig. 93, any Pumps," 246. in the heating steam is positivelyforced to the outlet incondensible

High

air

for

gases.

velocity then

ciurent

heating surface.

the

*

Telocity of the

with

pressure

air

pressure

a

transniission

it 50 per

varies

6/10

producing

cross-section

of

the

as

high

secure

steam

decrease

path should

To

is desirable

current

rapidly as

at

both

on

of

sides

velodty the right angles to its steam

the volume

of the

steam

is decreased

by condensation. is increased culation by securing a positive fluid cirEconomy in a predetermined path. In the ordinary standard is

juice. The

juice circulation

transfer

definite

path of either the

effect there

no

of heat

is

spout into the

high, with

is erratic.

In

tendency

a

but

to

steam

or

the

spots the

some

the

cause

juice

the

largest part of the heating surface is not used efficiently.In the steam heating there are in which the incondensible large volumes space to

gases

accumulate

Eddy

currents

steam

and

space,

lower

the

efficiencyby bkmketing is eddying with cyclonic the heating surfaces. As the steam are constantly changing position. velocity, these volumes indicate inefficiency.

When

exhaust

steam

liable to

contain

much

of this oil and

of

is used

for

heating

oil from

the

engines. The

scale,arising from

the

purposes,

lime

used

it is

presence

in the

defecation,impede the transfer of heat. As the metal

used

to

is generallyeither copper

separate the heated

and heating fluids

quite thin,the coefficient of heat transfer is not affected appreciably by its thickness. of the Juice and 227, Evaporation Crystallization of the Sugar. Sugar juicesare evaporated to the saturation distinct stages. The or crystallization first point in two or

brass and

"

1

"Proportioning

tions of the American

of

Surface

Condensers,"

Society of Mechanical

G. A. Orrok, TransaoEngineers, 1917.

356

AND

EVAPORATING

of

cyde

juice of about

feet of

unit

of 10

to

serieB of vesaels called

a

cubic

a

Bnx

12.5"

If

therein feet.

is

will be

multiple effect,it cubic

involves

daily.

times

several

repeated

operations

the second

while

Operation is practically continuous a.

HEATING.

JUICE

sent

orated evap-

about

lo

is about

stage

In the

feet of

cubic

into

drawn and

a

vacuiun

which

will

be

sugar

and

half

from

pan

about

to

of tnasseeuite

foot

Besides

about

half

molasses.

evaporating the

sirup

water

point,

in the pan

Fia.Ol.

the

enlargement

of

the

governs

design is

dependent

thick viscous

a

Multiple

228.

usually consists

usually even

four

six

increases are

whN"

the heat other

the

with

concerned. the

of

necessary

side.

used.

of steam

evaporate

Necessarily

pan

charging dis-

the

are

so

far

simple side

water

from

t"mperature

three

as

efficiency fuel coste

steam

of

a

tube

the juice and

or

five and

Europe

operated,

one

on

multiple effect

in Cuba

in

vessels in

vessels

These

to

while

Properly of

the

vessels;

ordinarily;

number

condensing

Louisiana

In

three

or

vacuum

quickly.

mass

two

been

have

This

efficiently handling and

upon

Effects."

used

are

size.

the multiple effect,while

of

design

more

the crystak

boiling to grain. Efficiencyof evaporation

is called

operation

sugar

subsequent

commercial

to

the

include

graining or forming the crystals and

it

bring

to

the saturation

I operations

two

sirup will be

evaporated

1 cubic

ond sec-

of

unit

our

in the

to

preparatory

operation.

next

to

tiple the mul-

is stored

eEfect and

tanks,

its

Brin.

53"

from

It b pumped

2

thickened

This

juice is called simp and density

a

heaters affords on

pressure

the of

the

steam

juice

the heating side

on

heated

or

side.

The

357

CONDENSATE.

OF

DISPOSAL

higher than

are

those the

arising from

vapor

the

on

boiling

juice in the first efifector vessel passes through a pipe to the steam space of the second effect,Fig. 91, and will evaporate juice if the

the

from

water

maintained

pressure

this

on

the two fall of temperature between proper The vapor sides of the heating surface. arisingin each effect

juice allows

a

last which

the

is sent

to

that

followingone, except

in the

evaporativeduty

does

from

condenser.

a

belt (A) could be of the form shown Fig. 90 the steam surrounds In this tyx)e the steam in Fig. 92. in section The the small tubes. juice boils up through the tubes and In

either

descends

in

down-take

tubes

through adjacent the

and several largertubes used

omitted

the

Note

in

followingconditions

through the large

large down- take

The

center.

or

down-takes

as

inay as

be

desired.

Fig. 90:

IV

Effect. differences

Temperature

40"

PresBurea:, -16.2 -24.7

side Steam side Juioe Differences Densities, Briz:

8.6

effects effect)!

Entering In

data

These

""

470

obtained

were

capacity

older

especiallyin the contain

sugar

moving

steam

carried

sugar

the

foaming.

Figs. 90 American

to

93

In

are

necessarily.

and

from

indicate

may

the other

in the be used

effects,

is liable

evaporators,

in the

to

rapidly

is rarely preceding effect. There well-proportionedand well-operated

If the

used

were

not

condensate

by entrainment

over

the

from

multiple effects.

1

The

of

do

economy

condensate

types

in modem

entrainment

start

maximum

or

The

boiler feed water.

of

and

^

belt of the first effect is free of sugar

steam as

test

on

Condensate."

of

Disposal

229.

in.

12**

maximum

either

in. in.

condensates

containing

even

traces

boilers,these would ultimately modem the confactory, in which

in the the

from

a

paper

Society of Mechanical

by

E.

W.

Engineers.

Kerr 1916.

in

Transactions

of

358

EVAPOEATINQ

contain

8

boilere, in (mud

AND

no

cachaza)

or

the

and

HEATINQ.

this water

sugar,

saturating

JUICE

ia used

in

feeding the

bagasse, in diluting tank-bottomB

in wfkshing the

various

Gondensat" effect

tanks.

from be

may

the

third

the

fourth

the second

passed

and

the total into

by

condensate

from

each

to

or

belt of the

termed.

of

Incondeosible

"

bteught into the

are

multiple effect [in the and

juice

or

under

to

fast

they

as

of the and

pose juice decom-

should

be

the gases

with

calandria In

positive are

forced

steam

The

not

the

air

cools

the

air has a

air to escape.

traps

and

will

stem

and

sink

steam, so

for

will

is t"ken below

but

the

valve

to

that

the

neither escape

fact

steam.

in attemptii^

oloaes

air

of the the

pose. pur-

with

let the

exit

pressure

in connection pass,

that

eaolt

the

using high

let water

Advantage

escaped, the

valve

valves

air relief valve

steam.

readily

pans

the

connect

air pump

or

vacuum

by

steam

The

steam.

nor

heats

of the

case

traps.

but

condenser,

the

so

to move

to

by the pipes which

the air ia removed

steam,

air

the

removed

The

heating.

continuously are

ammonia

of the beating steam

path

they

as

nitrogenous

form

the

during

pressures less un-

Certain

bodies

off

accumulate,

removed enter.

steam

given

are

the reduced

and t"nd

where

the

Disposal

Gases.

a

pump

calandria, as

is often

330.

gaaea

of

separately

heating section effect

then

means

It is usual

the

into

effect and

be removed pump.

The

that After

follow, allowed

359

TCBEB.

Jnlce

231.

the juice height, as

when

the

tube

lite

sirup

sheet,

kept

is

controlled

valves

may

height

gaged by the

tube

height.

the juice over

cany

indicate

not

same

the

exterior

the

juice level,

in all effects

by hand-

pumped

amount

from

of thin juice drawn

amount

the first.

into

Different

232. are

bubbles

auhMuatically, the

or

last liffectbeing

the

the

at

by the glass gage

oae-fourth

this does

but

vertical

is secured

capacity

greateet

to

the effect the s'^eam

the

ordinary standard

indicated

effect, is one-third

Inside

the

effect. Fig. 92, the

multiple

to

In

Height."

diSet^ot

many

few

The

most

of difierrat

couunon

large

fault

is

juice

capacity,

too

so

mains juice re-

the

long in

too

effect.

Home

lack

types

styles of multiide efiects made

There

elements.

same

the

Effects."

Multiple

of the

modifications

that

of

Types

in

the

poaitiveness of the of

circulation steam

juice

or

the in

or

withdrawal

the

cS

incondenuble

the gaaes.

The

beating is made

face sur-

of

up

straight tubes

usu-

^^

^

ally either vertical

Usually the

horizontal.

or

the

juice through

type

the

juice is sprayed

of the

tube

are

and more

contains

Tabes.

333.

about 40

to

permit air

To

steam.

"

ft inch 54

a

the

tubes

the closed

upper

vertical standard

thick, 1} inches

inches

intensely

to escape

In

inclined

over

horione

taining con-

end

pin hole.

a

In

the

passes through the vertical ones.

and

Eontal tubes well-known

steam

long.

small

The

number

or

effect the

2 inches

longer these of them

tubes

in diameter

tubes

is heated

and the

the more

360

AND

EVAPORATING

JUICE

HEATING.

they spout juicehigh up in the rapidly moving efficient the heating surface, the The more more

wiU

certain steam.

the

will be

uniform

will be the

the smaller

juice and

entire

top sheet

and

temperature difference between

sides.

steam

the

boilingover Intense

localized

heating

the

should

be

avoided. tuTjes in horizontal

The

about

and

diameter

12

unit

a

as

Longer tubes

of

are

These

eight, which

in

tubes

be

may

moved re-

(Fig.91). of Eff eets

Relations

234.

long.

inch

1

or

in the middle.

in nests

generallyarranged

are

f inch

are

feet

14

or

supported

unless

liable to sway

effects

effects will operate when

to

they

Each

Other."

Multiple operating efficiently.

not

are

arisingin one effect must be condensed in the belt foUowing, and conditions will change so that next steam this will occur. Suppose that the third effect suddenly All the steam

its heating surface

had

the

transmit

covered

of heat

amoimt

with

and temperature pressure transmitted heat the was rise till steam

in

belt

the

in

increased the |)ressure

its steam

Ihe

formerly,as calandria

or

the

on

of

belt

not

would

effect.

rise in

the

the

condense

to

second

the

could

before, so

sufficient

from

over

less than

this would\be pressure

coming

now

It

it transmitted

steam

the

scale.

the

third

But steam

effect

juiceside of the second

all

has

effect.

capacity of each effect depends upon the capacity of the effect preceding it and on the one following. Beal and Apparent 235. Temperature Oifferences. The

The

"

difference

going

vapor

apparent as

double

the a

first effect

of

four

and from

temperature.

the

parts.

paragraph, These

the

are

the

there

tabulated below

standard

for

temperature

in

in

steam of

into a

vessel.

one

two

the

In

parts, in

quadruple

enumerated

causes

are

the

the last effect is the total For a single effect,such

pan, this total range occurs effect this range is divided

For

in

temperature

triple effect into three parts and

into

of

the

to the condenser

range

vacuimi

a

the

of

calandria

between

in

effect a

ceding pre-

of temperature. lost-degrees a

tnple and

type, for usual

quadruple effect

conditions

under

three

heads.

(1) The

boiling temperature

loss is due

to

the

fact that

TEMPERATUBE

we

dealing with

are

tiUed

static head

(2) The

and

third

Obtain

assumed

loss

to

the

the

enter

and

the

125.4"

can

scale

expected

of

ranges

apparent

or

the

166.8** Fiom

The

the

199.8** F.

second

be

is the

is

range

-29.8**

triple

a

conditions affecting, as

heating surfaces.

vessel

the vapor

apparent

considered

26** have

is

steam

divided, for

with

belt.

apparent steam so

range

been

for instance In

the

table

assumed. of the

sum

obtained

Tha

assumed

is the

in the steam

A

TRIPLE

first steam

temperature 199.8**

in the second can

gives

vessel.

readDy find the

the temperatures.

IN

27.4**

temperature,

Subtracting SS"* F. from

correspondingto DISTRIBUTION

in

temperature

F., the temperature of the vapor tables (page 377) we the steam

pressures

of the

its

the assiuned

F., from

the

sity den-

expected lost degrees of temperature. the temperature of the vapor rising in the first

vessel, subtract

in

in. each

in it and

obtain

on

22**,24** and

range

real range

belt.

oil

been

The

is 227.2** -125.4"

now

coefficients that have

heat

F.

F. and

The

F.

real range

real range

the

to

in the Vessels

first vessel at 227.2^

effect,into three parts in accordance

To

depth

(218).

5.4*'-|-9' +15.4** =29.8''

are

This

72** F.

the

dis-

below, the total loss degrees

table

the last vessel at

leave

the

with

to the

(assumed) due

to he Carried

the Pressures

227.2** -125.4'' =

in the loss due

viscosityof the solution

temperature

to

loss takes

includes

Multiple Effectr^ln of

than

boilingliquid(216), (219).

(3) The To

solution rather

sugar

a

(217) ;

water

of the

361

DIFFERENCES.

EFFECT.

362

EVAPORATING

AND

DISTRIBUTION

In

"Steam

IN

A

in

Economy

HEATING

JUICE

EFFECT.

QUADRUPLE

the

Sugar Factory/' Abraham, translated by Bayle, the following table is given, illustrating losses in temperature LOSS

IN

in evaporators of beet sugar DIFFERENCE

TEMPERATURE,

factories:

IN

DEGREES

FAHRENHEIT.

System.

Evaporation

Single effect.

.

Double

.

.

effect Triple effect effect. Quadruple Quintuple effect. .

.

.

....

gives

Hausbrand^

temperature

in the

equal

The

him

area.

are

as

greater differences

even

effects when

the

ratios of the

in the

fall of

heating surfaces

fall of temperature

are

of

given by

follows:

In the double

effect

1

1 58 .

1 tripleeffect In the quadruple effect. .1 In the

Applying

ratios

these

apparent temperature

in

1 .44

3.44

105

1

1 48

.

the

differences O

preceding as

2

.

175 .

would

cases

follows:

1JI

o

1?

op*

op.

"

In

the

In the The

tripleeffect quadruple

1

of

"Evaporating,

brand, Eng.

.

17.3

24.9

59

17.7

19.5

26

.

temperatures Condensing

Ed., 113.

2

38.4

.

of the difference between

discussion

differences

effect.

has and

give

been Cooling

real and

introduced Apparatus,"

apparent

largelyto E.

Ha\is-

364

did

EVAPORATING

build

not

bring the

to

m^ and

pressure

evaporation enormously increased.

HEATING.

if

liad been enough steam supplied to 18 pounds per square lute, inch, abso-

up

the

rate

In

foot

square

per

this test the

would

been

of temperature

being 7.6" F.

by Prof. Kerr should be consulted

originalpapers

drawing conclusions

have

total range

53.8" F., that in the first effect

was

The

JUICE

AND

before

to the relative

of the tors efficiency evaporaincluded in his tests. The results of his tests are given in the tables at the end of this chapter, to serve as examples. ^In properlyoperated clean effects Heat Balance. 237. it is close enough to say that 1 pound weight of steam per as

"

unit of time

will evaporate

approximately 3 pounds of water from 4 pounds of juice in a tripleeffect and that it will evaporate 4 pounds of water from 5 pounds of juice in a quadruple effect in the us

the

assume

steam

of

unit

same

temperatures

on

To page

show 361

this, let

for

a

triple

density of the entering juice is 12 Brix, the temperature being 180" F.

effect and

Heat

also that

time.

the

Distribution

in

Effect.

Triple

a

Heat.

First Effect. 1 lb.

steam,

per

Heat

5 lbs. pressure

0

Latent

=960.7

Juice,lb. B.t.u.

000

4 .

sq. in.

requiredto raise

4 lb.

juiceat 180" F. to 199.8" F.,specific heat =0.9, 72 (199.8-180) X4X0.91 =

=

.

Total

.

.

heat liberated heat

Latent

888.7

at 199.8" =977.7

B.t.u.

Evaporation No.

1 =888.7-^977.7=

Juice transferred

to No.

Second liberated

Vapor from

as

No.

1 effect

=

Effect.

888.7

27.4

juice:

(199.8-166.8)3.091X0.85= Total

^"x=i5-5".

condensate:

(227.2-199.8) Xl heat from

*"

3.091

follows:

Sensible heat from

Sensible

.909

2 effect

BS^tooHeat

.

heat liberated

86.7 1002.8

INCBEASING

EVAPORATIVE

transferred to No. 2 effect

Juice

heat

Intent

at 166.8

No.

Evaporation

2

1002.8 ^998

15,5_2J086

.

Vapor

heat

Sensible

^ _^^o "r"-^3.

. ""

Third No.

2.086 "

Brix'"3.09r from

1.005

=

3 effect

transferred to No.

Juice

3.091

,

998

=

=

Effect.

2 effect

from

1002.8

condensate:

(199.8-166.8)(0.909+1.005)

63.2

=

from

the

juice: (166.8 -125.4) (2.086)(0.75) heat

Sensible

366

EFFICIENCY.

64.7

=

'

heat

Total

liberated

.

heat at 125" F.

Latent

.

.

.

1130.7

1021

=

1130.7

Evaporation

'^

in No.

3

.

No.

3, gg^

Increasing

238.

it is

0.979

0 979

23

Sirup from

1 107

=

=

=

g^*

Evaporative

always advisable

on

^"

"*"

the

=

^^'

ally Efficiency." Theoreticscore

of steam

to heat

economy

to

low-temperature low-pressuresteam to heat those of high temperature. high-temperature steam at different temperatures, By using a series of heaters taking steam use

solutions in

a

series of

can

be

solutions and

raised

in the

steam

the last effect is wasted, yet

be

used

its

owi

the vapor

high temperatures

operations.

Thus, all the heat from

to

a

going to the condenser portion of that heat could

ten degrees of juices to within some In other heaters, steam taken from temperature. pipes of the third,second, or first effect could raise to

raise cold

juiceto highertemperatures. The practicalobjectionsto the scheme are the increased complexity of the apparatus, its initial cost and upkeep.

the

the

followingassumptions: of heat units in 1 pound weight of steam (1) The number at all pressures (practically). is the same (2) If X pounds of water are evaporated from a multiple of pounds of exhaust steam effect,then the number required number if of vessels the is the in be effect. will x/Uy n taken from the boilers and If h pounds of steam are (3) Let

us

make

366

used or

EVAPORATING

in any

JCHCING.

HEAT

AND

singleeffect heater, such

the defectator,

used will be

steam

"

the

as

vacuum

pan

h^.

n

Suppose that the

being sent from the last effect to the condenser were of high enough grade,it is evident that we could save 100 per cent of h pounds of steam by diverting h pounds of this steam from the condenser. Every pound of steam sent to the double effect should evaporate 2 pounds of water, but if 1 pound of vapor is from the vapor removed pipe leadingto the second effect, then the evaporation has been reduced 50 per cent, as only has been evaporated. By removing h 1 pound of water pounds from the vapor pip)eof the firsteffect we must send steam

h

X

to the first effect

^ +"

Every pound of

h

pounds of steam, thus saving ^ pounds.

steam

sent

3 pounds of water. GAIN

IN

PER

to

taking off

By

CENT

tripleeffect should

a

pound EFFECTS.

ROBBING

BY

a

orate evap-

of vapor

-

lose the

evaporation of 2 pounds of water in the followingeffects and so the gain is 33 J per If the vapor taken from the vapor cent. were pipe of the the

from

second

first effect

effect

gain 663

we

evaporate

we

2

out

of 3

pounds

of water

or

per cent.

General

to abstract h Equations." If we are pounds of steam from only the first of n vessels and must nish evaporate x pounds of water in those vessels, we must fur239.

the firstvessel with

(

(a) This

expressionmay We

may

-j +hi pounds of

steam.

be considered to consist of two

imagine

a

weight

of steam

( \n

normally in

n

vessels and

so

evaporate

-] to n

n( \n

tors. facact

/

^j =x"h n

/

IN

SAVING

pounds

^i

essary

The

of water.

factor,hi, evaporated the

other

neo-

the firsteffect and this vapor

from

of water

pounds

367

CENT.

PER

perform the auxiliaryheating. t^ken from only the second If ^2 pounds of steam are

is sent

to

vessels,the

n

of steam

amount

that must

be sent

of

to the first

vessel will be

("-^)+A,.

(6)

before,we

As

I

"

"

to

imagine

may

act

the steam

normally and

supply

representedby its value

times

n

additional evaporation, or (x"2ht) pounds. The will evaporate /is pounds from each pounds of steam in

h^ of

effects,giving z for the total evaporation and hg for auxiliaryheating. be drawn In general let hi,hi,At, hn pounds of steam nth effect,then the total the first, from second, third, will be, on consumption of steam rearranging expressions (a) and (6)above two

.

.

.

.

rnx-T'H'rni-r*

"

.

.

.-[-An

.

.

n

n

Savliig in

Cent."

Per

"

The

saving A, may also be expressed as a percentage of x, so that the consumption of and the saving may be expressed in terms of x. steam the conThus, if hi-T-x^px, hi-i-x^pz hn-^x^pm sumption of steam expressed as a percentage of that required 240.

.

for direct

"

and

the

a

.

multipleeffect evaporationwould +Pi-f-pa

.

.

.

be

Pn

,

percentage saving would be (pi4-2p2+3p8

In

.

quadruple effect

the second

the

effect of O.lOx and

.

.

npn)-^n.

.

first effect is robbed the third of

(.15X.254-.10X.50+.05X.75)x

=

of 0.15x,

0.05z,the saving is

12.6%. j?|a; or

(238.)

(.16+2X.10+3X.05)-*-4"12.6%.

or

In

and

a

quadrupleeffect if,in

third effects

are

robbed

one

of

second instance,the first,

equal

amounts

of steam,

368

EVAPORATING

AND

JUICE

HEATING.

and, in another instance,the second effect is alone robbed of the same is the same quantity of steam, the efficiency in both cases theoretically: .25+.50+.75_ "

~'^'^

3 the reduction

however, Practically,

in

complexity of piping

robbing of the second effect preferable. the When 241. or Pauly Heaters Pre-evaporators." ficient supply of exhaust steam from the various engines is not sufthere is a choice between admitting live steam direct makes

the

the boilers into the steam

from

using this live

belt of the first effect

heater

and

taken

not

of

or

sending the resulting belt. If P pounds of steam into the steam sent to are vapor to the first the preheater,it will deliver P pounds of steam effect, and

in

steam

be

must

care

a

multiple effect

twice.

The

pounds

of steam, and

x-P.. ,

,

must

proper

this steam

count

evaporate x"P

now

requireeither

this will

(^1+2^2+3^3+.

,

,

to

.

nhn)

.

n

n

pounds of steam, n

according as the effects are robbed or not. If the effects are robbed, then the firsteffect (n+l)P.,

X

,.

(/ii-f2/i2+3/i3+...n/in)1

,

,

-|-/ii+/i2-r "

.

.

+P,

hn n

n

n

receive

must

simplicityS^-f P pounds of exhaust steam, llE being the quantity enclosed by the brackets. which

shall call for

we

If the

effects

-PJ pounds

(

robbed, the first effect will receive

not

are

of exhaust

and

steam,

P

from

pounds

(x"P\

the

preheater or

total of (

various

I

of boiler and

total amount

The the

a

use

Ha^ Hi,, He

effects

are

robbed

.

"

of hu

"

exhaust and

auxiliary machines

former

pounds.

the

Hg pounds

hz, hz

.

.

.

hn

steam

supply

to

the

effects when of

and

steam

pounds

the

of steam

will be

+ f/a + H6+

2^+P ^ I "

n

Z7

1

17

|-/2a~r"6"r

.

.

u'

. "

"

"

.

Ho-{lh+h,-\^

hn)^ (Ai4-2/t2+3/i3 4...

.

.

.

nhn)

'

"^

"

n

n

HEATIiNG

Steam

242.

Consumption

manufacture

In the

of

369

SURFACES.

cane

In

Cane

a

Honse.

factories do

most

sugar

Sug^ar

not

use

do

they rob the effects,though the large use and the high cost of fuel is leading to of maceration water the rapid introduction of preheaters and preevaporators. preheaters nor

The

is also used

preevaporator

increase

to

the

eva|X)rative

capacity of the factory. In beet sugar factories preevajx)rator8 generally used and the effects are robbed of vapor. are In the following example the weight of steam used for is expressed as a percentage of the weight of purpose any the cane ference that there is no difground. It is further assumed in the and

steam a

in that

from

water

that

vacuum

a

of

pound of high-pressure

a

pound of low-pressuresteam; that in condensing will evaporate a pound of steam the juice; that a preheater may be used and using low-pressuresteam for heating is pan

of

pound

quantity of heat in a

feasible. In

house

a

is 78

provided with of the

cent

per

quadruple effect,the

a

weight

cane

supplied the firsteffect is therefore

steam vacuum

use

pans

22 per cent

and

78/4

the

oration evap-

exliaust The

cent.

per

for

heating 16 per cent steam used is then, for, preheater,no robbing of effects,

weight of steam (1) Straightevaporation,no

is used.

and

The

7Q

-^+16+2257.5%. =

(2) If

preheater receiving10

a

per

cent

is

steam

used,

55%. "^^^^^+16+22 =

(3) If the

preheaterreceiving 10

a

cent

per

first effect is robbed vacuum

pan,

of 10 per cent steam the second effect is robbed

juiceheating and for heating purposes, for

the fourth

4

same

are

to

for

a

and

sure low-pres-

of 10 per of 6 per effect is robbed

cent cent

4

If the effects are the

is used

steam

robbed

not

heating surface. be robbed

to the next

as

diminishes

the

it is usual to

This mass

cannot

of steam

greatly. Thus,

give each vessel

be done sent

if the effects

from

one

effect

370

EVAPORATINQ

The

exhaust

78

AND

steam

JUICE

HEATING.

to the firsteffect

sent

S^"

=

5X10_^^^^^^_^^_ )^,, ^^^ (10X1+10X2+6X4^

4

4

IB,..

19.5

10% Steam from

I"

-29.6%"

10.0-

re-

Eeater

10%

T,

n-i".5%"

19.5%"

in"

IV-L3.6%

fl.5%"

I

i

i

29.5%

10%

19.5%

9.5%

9.5%

Evaporation 78%

factory is prosperous, it is usual to increase its in the sizes of effects, capacity. If changes are to be made it is well to consider robbing," lettingthe old effects follow first effect,enlarged to provide the necessary extra a new Where

a

'*

heating surface. 343, Heating 378,

is struck

one

By referringto Table

by the wide

disparityin temperature

different

in the

allowed

Surfaces."

effects in different

B,

page

fall

houses,and

also

conductivity by the disparityin the coefficients of thermal in the different effects in houses of the same capacity. that

It is evident are

with

the

that water we

can

the

water

in each

conditions

effect will evaporate

we

6.5 to

the

effects

operated vessel, will be are

do not

conditions, for example,

average

per

when

incrustation,and

these economic

quadruple

a

obtained

fall of temperature

proper

different when Under

results

free of oil and

and

new

the

obtain. may

7.5

assume

pounds

square foot of heating surface per hour and hence the heating surface obtain by dividing necessary

evaporated

be

to

in each

effect per

hour

by 6.5

to 7 5. -

\

Thus,

of water

if

a

quadrupleeffect is to evaporate

per

hour, the

heating surface

100,000 -5- (6.5X4) =4000 If the effects surface cane

of

of any

ground

sq.

100,000 pounds

of each

effect will be

ft.,approximately.

robbed

of vapor, the area of the heating effect is found by multiplying the weight of are

per

hour

by the product of the percentage

of

evaporation in that effect and the latent heat of the steam and fall of temdividing by the product of the apparent perature in that

effect and

its assumed

coefiScient of

heat

372

EVAPORATING

AND

fall of temperature

in them

JUICE

and

HEATING,

in the

those

creased de-

first two

by increasingcorrespondinglythe fall of temperature in them. Find

Example:

juice heater for capacity; at

equal

taken

of the

that

of

183.5^

F.y assumed

lOO"*

Aspume'the

the

F., the

of the

weight of the

to lose 1000

effect

juice is

entering the heater

of heat

difference

a

daily grinding weight of the

pipes of the second

vapor

transfer

between

B.t.u. per

specificheat of the juice is 0.9. the

of cane,

cent

per

coefficient

steam

tons

heating "vurface of

its temperature

degree Fahrenheit

per

6

the

and

cane

to

from

temperature

a

of

area

factory of 1000

a

steam

be

to

cane

the

The

is 250

the

B.t.u. sides.

two

pound and

is

the

that

rise in temperature

in

juice B.t.u.

1000X2000X0.06X1000

^o

^^ wo

p *"

1000X2000X0.9 The

of

difference

mean

between

temperature

juice and

sides of the heater

steam

too

loo.o

=

Allowing

10

-

I

"

rt

)

=50.2"

for radiation

cent

per

heating surface

/100+100+66.6

c

other

and

,,1000X2000X0.9X6G.6_^^o

-

.,

^"^

^'

250X24X50.2

originaljuice temperature be

must

ten

or

losses,the

will be

1.1 X

The

F.

plus its rise in temperature

degrees below

more

"*

the

assumed

steam

tem-

perature. Pan.

Vacuum

244.

A

"

vacuum

pan

is

a

single effect,

evaporating from 12 to 15 per cent of the quantity of water, requiredto be evaporated by the multiple effect. Economy of time To

rather

boil

and

than

drop

of steam

economy

strike

a

is

sought in its design.

quickly is desired.

To

boil

required properly clarified sirup, good quickly there are and air and coils free of condensate sirup circulation,steam the heating steam as great difference in temperature between and

the

massecuite

quickly the heating the massecuite.

as

is

surfaces

practicable. To must

not

impede

drop the

a

strike

free fall of

373

CONDENSER.

Boiler

passing a reducing valve, is

steam,

vertical manifold the

Inside

pan.

4-inch

helical

In

feet.

of

the

nozzles

divide

be

entering

into

manifolds

two

a

2

4

or

longer than

not

having similar

on

site oppo-

and

nozzles

40

tubes.

so

contain

must

the

In

and

thin

it is covered

unless

steam

first part

is rather

pan

or

preferably may

nozzles

to

culation arranged as to give the best cirthe quickest drop possible.

massecuite. in

there

be

must

and tube

these

tubes

pans

8 branches

or

pan

diameter

a

tubes

No

the

copper

large

sides These

having

6

admitted

of

the

with

operation the

diminishes

mass

till it

in volume

grain. After that period dui*ingthe building increases in density and of grain the mass amount to up when the pan is full. Owing to lost degrees maximum a of massecuite,highin temperature in boiling deep masses inch, is usually used. steam, 45 pounds per square pressiu^ is

to form

ready

Sugar is often boiled ivith exhaust tube at high velocity,as enters a of

the

when

process,

the

unbalanced

When

steam.

it does

in the

sirup is thin, and results that

pressure

this steam first part

condenses, sets

siderable con-

excessive

up

vibration, unless the tube is restrained by collars fastened soft coils must to rigiduprights. The not rub against their produce pin holes in the tube. 0.55 boiler horsepower designing the pan, about

collars and In

pounds

450

of steam

be

must

allowed

per

of

ton

or

cane

per

from

the

day. Condenser.

245.

last effect the

of and

vacuum

or

the

As

incondensible

that

so

the

condenser

placed

condenser

pump

vacuum

is

a

is

may

either

on

by

in the

air

inal orig-

heating process provided to remove

maintained.

preferredtype height above a

that

the

be

be

below

accompanied

dissolved

during must

steam

is reduced

steam

gases, formed

juices or sirup,or through leakage, an air them

the pressure

pan

atmosphere.

other

condensing the

By

"

The

or

metric baro-

plantations. It is

a

the

when

ground so that it discharge by gravity against the atmospheric pressure the bottom of its discharge pipe is submerged in an

open

tank

may

In enters

the

at

filled with modern

the

water.

type

condenser

the vapor at

pipe from

the side

near

the

the effect bottom

or

and

pan a?

374

EVAPORATING

the suction

AND

pipe of the air

JUICE

HEATING.

is attached

pump

at

the

top,

the

path of the gases is toward the top. The injectionwater the top of the condenser enters and is broken into near up their way

on

water a

thin

or

sprays

sheets the

which

through

the vapors

condenser.

counter-current

discharge pipe usually supports

should

pass

air pump

and opening. As the vapor in opposite directions,it ia sometimes called to

move

The

must

be about

feet

34

high.

To

the

condenser.

find the minimum

It

height

the absolute feet,divide the difference between pressure and the minimum absolute of the atmosphere to pressure in pounds per be carried in the condenser inch, by square in

the

and

weight of

a

in feet necessary

of water

of efflux of the Fins

Example. from a

cubic

pounds per discharge pipe of

a

carrying

condenser

the

feet of

60

weighing

high height velocity

this add the

the

assumed

atmosphere

at

inchithe minimum

on

the

bottom from

water

cone

whirling

discharge foot, are

water to

per

be

second,

discharged

foot cross-section from 0.5 square of 2 pounds, absolute,into pressure

a

of

pressure

a

placed

level.

the normal

If 5 cubic

"

be

prevent the

to

proper

risingabove

so

1 foot

discharge water.

of the condenser

and

To

produce

to

projectionsshould

or

discharge water

in cross-section.

inch

1 square

of the

column

14.7

height will be found (14.7-2)

pounds as

-^^=30.5

per

square

follows:

ft.;

ion

V^=2gh;

/.

^1

=

^^^ 1.56

=30.5 height

Minimum

=

ft.;

=32.06

+1.56

ft.

Cast iron is porous and Pump. air be tight with will leak through it,although it may regard should be raised and the sirup. A vacuum or to steam 346.

Vacuum

"

entire surfaces of effects and and

then

The

length

should

be

heated

gently

pores.

paraffincor other paint which will Joints of all descriptions may leak air.

of time

a

painted with

close these

pans

a

vessel

will hold

a

vacuum

indicates its

VACUUM

air

tightness. Air leakage of air that must

amomit

The

office of the

oondensible off

oome

as

but if the

this

than

be

can

to

or

air and

pump

The

pumping

reduced

to

by more incoming injectionwater To do this bring the vapor, Fahrenheit. opening of the air

suction

small

than

avoidable, un-

amount

10^

that 15*

or

just as it is

ing enter-

into contact

with

pump^

of the

having the temperature

surfaces

vapor

exceeding

not

in-

is

vapor

very

of the

the

the

other

air and

some

a

temperature

a

times

more

unavoidably.

vapor.

that

so

air is cooled

two

is to

air pump

mixture

a

be

may

be handled

rather

gases

375

PUMP.

incoming injection

water.

The

in the

pressure the but

parts

and

vapor

from

in all

same

different parts of

differ considerably. If

of the

the

the

take

we

tables

the

find

the perature tem-

sponding corre-

shall find this pressure less than that The difference of these existingin the condenser. we

pressure

actuaUy

nearly the

the

of

temperatures

may

mass

vapor

is

condenser

due is the pressure to the incondensible gases. pressures the less the amount of steam in lower we cool the vapor The

given

any

the

and

mass

greater the

of air

amount

the

as

The constant. total pressure remains proportion of vapor of air present is in proportion to the pressures and they This

exert. Thus as

suppose shown by the shows

that

the

table

From

law

is Dalton's

gauge

the we

in pressure and that mm.,

102

was

of the

temix?rature see

gases.

absolute

the

that

of mixed

that

the

is 92.3

temperature

mm.,

pressure

that

condenser

a

eter thermom50"

was

vapors

C.

correspondingto

P

this

a

92 3

'^^

is, 'p"~r^'

^^^

=9.7 mm. At the top of the condenser pressure is 102"92.3 meet cooHng surfaces at 15" C. and acquire let this vapor By the table we see that the temperature of say 20" C. a steam

is

pressure

in the condenser

17.5 mm., the is 102 mm., now

and, since the total air pressure

is 102

pressure "

17.5

="

84 5 84.5

Each

mm.

=8.6

times

as

stroke

much

air

of the air as

it would

pump

have

would

remove

removed

under

""

"

the

previous conditions. The

work

of the air pumps

can

be

enormously reduced by

r 376

EVAPORATING

HEATING.

JUICE

AND

(1) Reducing air leakage; (2) Using

the

(3),Reducing air pump

to

with

kilo.

per

vibsolute

clarification,and

in

for boiler

is used

the

that

pans

condenser in

this

and

pressure

of

the

air

displacement

pump

One

kilo

at

the

the

all the

C.

per

or

vacuum

air

into

carried

in

of

at

{273"+15")=288" and Find

cent.

first effect

air

of the water

be

C,

the

assumed

air

that

As

heated

will

volume

by

the

pheric atmos-

absolute, is the

the

volume

15)=21

kilos

efficiency of

air

minute:

per

requires 600-t-(43

steam

pipe

latter of

amount

that

is 80

pump

The

mm.;

temperature is 20"

in effects

carries

perature tem-

760

mm.;

from

assume

water

the

of the volume

cent

is 102

condensate

leakage.

to

barometer

C; suction

will

Assume

injection water. 5 per

the

as

air

(roughly) C;

sirup is small,it having been

injection

equal

case

is 15"

43"

sent

are

injection water

air pump

feed, we

except

steam

calorics

in the condenser

of air in the

the amount

of

600

water

orifice to

at

the

to

volume.

lose

and

of

discbarge

pressure

of vapor

going

vapors

kilograms

hour

per

Temperature of

clearance

no

1000

Suppose

condenser

the

to

necessary;

minimum.

a

"

of the

temperature

(4) Using pumps

Example.

than

injectionwater

more

no

"

injection

water.

Each 760

mm.

kilo and

of

288" 0.46

this becomes

contains

injection water absolute.

C, liter

At

84.5

0.05

liter

mm.

and

C.

760X0.05^84.5 ^^

Displacement

293"

at

by applying equations

PiVi^PiVi Ti

Ti

air

288

of air pump

volume

293 per

(21X1000X0.46)2X100

^__ =^^2

minute

*"

is

,.

^'^^'

60X80 The gases

effect of increased

passing

into

leakage

the condenser

higher temperature is readily calculated. or

of

PROPERTIES

247.

TABLE

A,"

DIFFERENT

OF

PROPERTIES VACUA

SATURATED

OF AND

377

STEAM.

SATURATED PRESSURES.

STEAM

AT

EVAPORATING

AND

JUICE

HEATINQ.

BVAFORATINO

AND

JUICE

BEATING.

"'.lit sals

sliSsSSSSIS!

S-BmSSRSSSSSSTiSSSsSE

z

I

1

I

c4(pe4oSr"C4oSS9oR^^O^O^S^

SRSSm2S"SSSS2""8KS22

1

3

ssstsss"sasssss

SUMMARY

OF

STEAM

CON8UMPTION

TESTS,

381

PURCHASE

OF

General

250* to the

at

of

"flat"

a

and

content

syston

ON

BASIS

A

Conslderatioiis.

lactones

sucrose

A

CANE

the

purchase

price,i.

test would

on

the

cane

as

would

cane

prcducdon

sugar

not

of his fidds

with

a

decrease

in costs

a

grower

and

ddiver

based

regard

to

a

the

upon

either

be

is not

the

will

purchase that

oi

operated without simple cme. degree Brix ocmtent

sucrose

fences purity. This method oooservalive price for the cane,

very

The

to the marufacturer.

of

coefficient

the

possible after cutting. Prompt ddivoy result in increased ddivery weight and

sranetimes

are

juice, without

pay

the grower.

care

excitingthe distrust ci the fanner Sales

considered.

not

undoubtedly increase

and

better

take

re^rds

quality, as

e., its

iNToblem of devising a system only equitable, but that may

The be

to

soon

as

the

of

forced

be

susually sold

is

purity of the juice,is

profitsof both the manufacturer would

Cane

"

ANALYSIS.

ITS

OF

the

of

the

or

the

factory

offset the

to

to

low

This purity of the juice in the early part of the season. method has probably been used en account of the fairiygood idea of

density (Banm^) real

The in the

hdd

by

cane

difficultyin devising

sampling of the

cane

itself.

a

in

fanners

system Somali

of

generaL purchase lies

samites from

cart

a

usually of very littlevalue in indicatingthe analysis and of the cane the juice for testing is eepeciallyso when The only method of sampling eaqxressedbyalaboratoiymilL that has given practicalresults is that ol the juice drawn from or

car

factory mills and

the This in

are

is inchided

method

'comparing Given

a

canes

in the

from

daily routine

the

various

fidds

of the is

an

cane,

step is the estimation Thk but

migjht be based the

of

oi many

a

railway particalar

of its sogiar upon

cane.

factories

and

representativesample of the joieefrom

lot of cane;, the next to the manufactarar. eonteat

representing the entire load

the

value

sucrose

diffieuhyof delcnnining

ol^ieelion. Tlie

method

sdeeied

must

this be

AS

SUGAR

better than

BASIS

A

OF

383

PURCHASE.

CANE

manufacturer

rough approximation in order to protect the and be fair to the farmer. Obviously, to be

equitable,the

method

a

of the available

be based

must

and

consideration

a

upon

of

cient figuringthis number, the coeffiof purity of the juiceand the efficiency of the factory The method described in the following paramust enter. graph, is in fact though apparently complicated, quitesimple. Cane Purchase. of Basis Available Sugar as a S51. ^A specialchemist and assistants are requiredfor these tests. sugar,

in

"

Reduction two

Factors.

reduction

chemist

should

first determine

factors,in cooperation with the chemist

factory, as follows: of the

^The

"

juicefrom

(1) Factor the

crusher

juice of all the mills.

for

of the

similar

(2) Factor

Brix

reducing the degree

that

to

of the

mixed

preceding

the

to

normal

crusher-juiceto that of the normal juice. The first factor has long been used and is regularly determined at intervals by the factory chemist (168). To det"*mine these factors,operate the millingplant for a short period without saturation-water; sample and separately analyze the juice from the crusher and the mixed juice from the entire plant. Calculate the ratio or factors, of the crusher-juice (1) Brix of the normal mixed juice-4-Brix for

reducing the per

and

(2),Sucrose crusher-juice.

per

Sampling." The and

the chemist

advised

is

to prepare

it is advisable The or

chemist

cent

notes

the

number

continuously and

in normal

juice-f- sucrose

of the cart

or

of

car

cent

per

cane

is noted

and is given a ticket bearing this number is to be samfor sampling. If cart cane pled, to group

the

crusher

juiceto

sucrose

cent

wash

he

a

the

if need

allows

of loads under

number

positionof

elevator,using markers

reaches

of the

a

cane

on

be, and

the conductor after the

definite interval

the rolls and

test.

one

cane

for the

pressed ex-

then

preferably samples brief intervals during

automatically or at The sample is sent to the laboratory the passage of the cane. with the ticket correspondingto it. Sample follows sample in this way.

Analysis, On receipt of the samples by the laboratory, A the samples and tickets are arranged in regular order. numbered cylinder is filled to overflowing with the strained juice and the remainder of the sample b held in reserve "

384

CANE.

OF

PURCHASE

pending the completionof the test. arranged in convenient inserted.

are

After

standing ten further

a

be

example, and after minutes the hydrometers

of ten, for

groups,

the latest to arrive has been

should cylinders

The

of five minutes

interval

The degree Brix and temperatures are to be noted. corrected Brix should observed be and Brix, temperature entered on a duplicate of the load ticket. These operations should be conducted allowing a definite systematically, very period for each. the

The

by Home's dry lead should The 234. laboratory equipment page considerable number of 200 cc. (approximate) test

sucrose

method, include

a

should

cylinders like C of Fig. etched

mark

on

it to

be

made

Each

39.

indicate

should

of these

have

approximately the

a

100

cc.

should be provided point. A spoon having a conical bowl of 1 gram It should hold about for measuring the dry lead. measurement. lead, struck Arrange a group of these cylinders,corresponding to those used for the density determination, and filleach to the mark the with juice. Add of lead to the juice,cover a measure **

"

cylinder with the palm of the hand and mix its contents by vigorousshaking. Filter, polarizeand calculate the sucrose Enter this test on the ticket. by Schmitz's table,page 468. Available sponding Sugar. Multiply the degree Brix by the corre"

reduction

factor

and

the

per

cent

by its

sucrose

gives the degree Brix and the per cent sucrose of the normal in terms the coefficient of juice. Calculate calculated by the method purity. The available sugar is new (;ivenon page 305, and this in turn to a basis of the factory normal by applying the efficiencyand juice extractionnumbers. The following example indicates the steps in the factor.

This

"

calculation:

Example: Factor

for

reducing the degree Brix

Factor

for

reducing the

per

cent

0.978 0.965

sucrose.

...

Degree Brix of the crusher-juice Per cent Assumed

18

in

crusher-juice mill extraction,normal juice. number the of efficiency factory

sucrose

....

Average

0 .

....

15

7 .

78.0 98

"

-

SUGAR

AI3

Brix

D^ree

BASIS

A

OF

calculated

of

mal nor-

juice Per

cent

=18.0

juice

Coefficient

juice.

extracted normal

find

we

gives

accordingly: 96"

be

the

11.29, from

method

given

results

the

the

basis

a

the

yield

of tory fac-

figure

yield

percentage

of

cane.

be

may on

on

sucrose

Since

reduce

must

we

expected this

of

sugar-house

actual

98

the

cane

11.52.

=

515

page

corresponding into

cent

per

cane

on

sugar

multiplied sugar

=

=11.82%

table

the

96**

11.82X97.43 is

may

reliability

The

of

11.52X0.98 that

sugar

yield

number

efficiency

of

number

efficiency,

factory

100

This

.78

X

of

number

yield

the

15.15

.1760=86.08

15.15

section

second

the

extracted

-

mills

=

the

97.43, purity.

X0.965

15.15-s-

=

the

by

to

86.1

to

:

juice

Referring

=17.60

lated calcu-

purity

normal

in

15.7

=

of

Sucrose

X0.978

calculated

sucrose

normal

385

PURCHABB.

CANE

judged

from

the

307.

page

.

method

This of

may

prices be

based

expected

enables

upon to

the

actual

the

give

manufacturer

in

his

yield

factory.

to

of

sugar

arrange

that

a

the

scale

cane

ANALYSIS

LIMESTONE,

OF

LIMESTONE.

OF

of

Preparation

252.

AND

ACID.

SULPHUROUS

ANALYSIS

SULPHUR

LIME,

the

Fragments should of pieces of the stone

Sample.

"

large number and reduced to a uniform si^e,then mixed and sub-sampled small to sample should be reduced by quartering. The iron mortar fine powder in an a on or a grindingvery or plate, plate. Particles of metallic iron, from the mortar be

chipped from

should

a

removed

by stirringthe powder with a magnet. Sift the powder through an SQ-mesh oughly sieve,and mix it thorby siftingor otherwise. of Moisture. Determination 2SS. Dry 2 grams of the powdered stone to constant weight in a tared flat dish be

"

should be heated to 110** C. watch-glass. The oven loss of weight divided by 2 and multiplied by 100 is

a

or

The

the percentage of moisture. of

Determination

Sand,

Clay, and Organic 1 grani of the Matter. limestone in a Treat powdered of hydrochloric acid, beaker, with a few cubic centimeters being cautious, in adding the acid, to prevent the projection 254.

"

of

particlesof with

beaker Collect

the

a

residue

100

is the

Place

is the

the

the

glass. Cover

liquida

few

the

minutes

quantitative filter,wash it reserve

filter and

the

filtrate (A) for

residue

to

constant

The

The

residue

weight

percentage of sand

silica and

and

water,

the

weight of the residue multipliedby percentage of sand, clay, and organic matter.

the filter and

incinerate.

heat

tared

a

Dry

110" C.

at

on

hot

treatment.

weight

from

watch-glass and

thoroughly with further

material

the

alumina.

The

in

a

tared

of this residue

platinum crucible and (A) multipliedby 100

and, clay, i.e.,silica and difference between

combined

this percentage 386

388

ANALYSIS

Treat

graph. Incinerate

LIMESTONE,

residue

the

before, wash

as

OF

it

on

the filter and

heat

weigh,

and

in the

preceding paragraph.

soluble

from

that

filtrates A, concentrate of pure

excess

boil it until collect while

the

alumina

B,

and

them

to

of

Iron

the

convenient

described

as

percentage of

the

obtain

the

centage persilicates.

Alumina.

bine Com-

"

preceding operations volume. Add a slight

the solution

it is still hot,

while

be detected, only a slight odor of ammonia can small filter, a precipitate on filteringrapidly is hot.

If there

is considerable dissolve

to

and

iron

predpitate

the

reprecipitate it with directed above, unitingthe filtrates (D). Partly

as

used,

are

and

incinerate

filters,and filters

ashless

and

from

hydrochloric acid

dilute

dry both

silica

in insoluble

as

to

filtrate (C).

bright redness,

to

silica,to

present, it is advisable

ammonia

of

Subtract

sand

a

the

residue

total

C

ammonia

solution

the

with

the

Determination

257.

the

acid

hydrochloric

reserve

percentage

silica present

of

and

the

of

dilute

filter and

a

calculate

with

ETC.

correction

no

silica.

for

advised

as

need

be

made

oxides

of

iron

If for

them. residue

The

ICO

mixed

and

percentage.

usually

not

alumina

the

obtain

to

is

It

the

(FcgOg, AljOg). Multiply the weight of the residue

alumina

by

of

consists

separately.

determine

to

necessary

the

axid

iron

If

required, however, proceed as of the with follows: Treat limestone 1 gram powdered concentrated hydrochloric acid, most conveniently in a with platinum dish. Evaporate to strict dryness, moisten again

hydrochloric acid, and for

described'

dilute

with the

filter

hydrochloric acid, with with

hot

water

alumina.

Wash

above,

sulphuric ticid,and

dryness. The

Wash in

cautious

iron

with

a

the

the is

and

the

water-bath,

Treat

heat, and treat

the

as

residue

the

filter;wash filtrate

with

precipitatethe iron and the precipitate into a small dish, dissolve

described

as

on

silica determination.

the

ammonia, it in

dry

now

use

evaporate

residue of most

standardized

to

the

into

an

the

solution

Erlenmeyer

nearly to fiask,being

water.

conveniently determined

tion by titra-

solution

of

of permanganate

sium. potas-

DETERMINATION

Add the

small

a

quantity of

flask,to reduce

the

titrate with

state, and

solution

This

zinc-dust

pure

from

iron

the

until

is added

solution in

the

to

ferrous

the

ferric to

decinormal

the

389

CALCIUM.

OF

tion. solu-

pennanganate

pink

faint peimanent

a

produced. Multiply the burette reading by .008 to of the stone, ascertain the weight of ferric oxide in 1 gram the percentage of ferric and this weight by 100 to obtain color is

(FcjOj); subtract

oxide

of iron

percentages

this per

cent

alumina,

to

and

from

combined

the

obtain

the

percentage

of alumina.

Determination

258.

iron

the 1

to

and

of the

gram

To

determination

(D), corresponding

add

stone,

it slightly acid.

render

to

alumina

of Calcium."

volume, neutralize and

add

excess

an

Set aside

twelve

for

residue

consists

anunonia, heat

on

hours, then a

of

to

to

venient con-

a

boiling, tion. solu-

of ammonium collect the

tate precipi-

wash quantitative filter, incinerate

ignite the

platinum crucible, then

The*

this solution

boiling-hotoxalate

(filtrate-"), dry and

water

tared

it with

of calcium

of oxalate

cold

of

hydrochloricacid

sufficient

Concentrate

the filtratefrom

almost

filter in

the

residue

calcium

pure

with a

strongly.

oxide

(CaO)

accurately,it may be weighed as such, or, more into the sulphate (CaSO^) or carbonate converted (CaCOj), labor to convert and It requires less time and weighed. into the sulphate, using the following solution: Add volume of sulphuric acid to an equal volume of one and

be

may

and

water,

neutralize

this acid, then

to it two

of ammonium

grams

Filter use

add

calcium

in

reagents Add

the

an as

must

parts

solution

in

of

the

strong ammonia

each

if necessar}'',

determinations. in

of

100 and

with

Dissolve

parts of ammonia.

chloride

be used

excess

three

2

of this solution.

cc.

preserve

it for

Strictlychemically

pure

preparing this solution. ammonium

sulphate solution,prepared

described,to the residue in the crucible,evaporate

dryness, ignite strongly,cool and weigh. The weight of the residue multiplied by .41158 gives the weight of calcium oxide (CaO), and by .73416 the weight of calcium carbonate of the stone, and these numbers plied multi(CaCOj), in 1 gram to

by 100 give the percentages and

calcium

carbonate

of calcium

respectively.

oxide

lime) (quick-

390

ANALYSIS

The

residue if

converted

preferred,as

follows:

carbonate, moisten

at

until

The

by

weight

of

weight

oxide.

calcium

by

The

is the

100

approximately

calciiun

oxide

product

is the percentage

of

100

add

cc,

gram

plied multi-

the

To

"

after

slight

a

1

carbonate

Magnesium.

determination,

in

substance.

of this

percentage

calcium

the

from

the

100

plied multi-

of calcium

weight of calcium

Determination

259.

of

tion operais calcium

of

carbonate

the

this

Repeat

carbonate

the

stone, multiplied by

of the

of

some

expel

80"C.,to

heat.

it

heat

water,

and

50^

weight

gives the

.56

it with

red

a

constant

a

obtained.

Ef

below

then

bonate, directlyinto calcium carMix it with finelypowdered

between

temperature

a

ammonia,

of

may

ETC.

LIMESTONE,

be

ammonium time

OF

filtrate

concentration

to

of ammonium

excess

hydrate,then add podium phosphate solution in excess, drop the magnesium to precipitate by drop, with vigorous stirring, as

a

After

phosphate.

of ammonia.

add

decided

a

excess

Set aside insure

to

fifteen minutes

in

night, during several hours, preferably overcomplete precipitation.Collect the precipitate

a

Gooch

a

wash crucible, of 0.96

part ammonia

1

washing

it with

dilute

specificgravity,to

be continued

should

ammonia,

until

taining con-

3

parts

of silver

drop nitrate solution added acidulated to a drop of the filtrate, with nitric acid, produces at most only a faint opalescence. The phosphate; diy precipitateis anmionium-magnesium The

water.

a

gentle heat, then increase the temperature to expel the ammonia, and finallyigniteit a few minutes in the the residue into pyrophosflame of a blast-lamp to convert phate of magnesium. Cool the residue in a desiccator and weigh it. The weight of the magnesium pyrophosphate (MgaPjOy) multiplied by .36208 gives the corresponding The magnesium is present in weight of magnesium oxide. it, first

at

limestone

a

as

carbonate.

by

.7574

Multiply the weight the

and

percentage of magnesium In

which

limestones

method

proposed

Herzfeld

*

and

by

Forster

1

product by

carbonate

contain

be

the

phosphate pyro-

to ascertain

100

the

in the stone.

very

little

magnesium,

Prinsen-Geerligsand may

of

used.

Zeit. RQbenzucker-Industrie,

Dilute

1896.

modified 2 grams

the

by of

391-

ACID.

CARBONIC

OF

DETERMINATION

hydrochloricacid in powdered stone with concentrated porcelain dish'. Evaporate the solution to dryness on

the

hot-plate

the solution

and

evaporate

part

of the acid.

calcium

of

excess

alumina

of

top

acid.

the

adhere

with

almost

decant

it

set

the

natant super-

filter,using hydrochloric

from

solution, as

the

of ammonium,

oxalate

the

the

the

to

in

precipitateby including precipitate,

Precipitate the calcium

in 25Sf

described

and

lime-water

flask to

Wash

an

iron

Stopper the flask and

Dissolve

may

add

and filtrate,

the

Add

fillthe

filter,and

a

before.

as

particleswhich

any

receive

water.

water.

liquid through decantation

water, and

precipitateto settle, then

for the

aside

with

neck

the

hot

filtrate,mix, then

the

to

a

the residue

Treat

precipitatethe

to

flask to

with precipitate

the

excess

carbonate, a

over

few

a

the solution with

filter,using

and

wash

Dilute

to

matter

a

drops of nitric acid, small bulk, to expel the greater

hydrochloric acid, boil,add

with

dry

the silica insoluble.

flame, to render

naked

the

heat

then

sand-bath,

or

a

and

remove

by filtration;precipitatethe magnesium as ammoniumit into the pyrophosmagnesium phate phosphate, and convert as already described.

it

Determination

260.

usually be

may

with

calculated lime

the

determine

to

necessary

from

Acid.

Carbonic

of

the

magnesia, except

and

acid,

carbonic

quantity required

the

when

is not

It

"

it

as

combine

to

sulphates

are

present.

gravimetric determination

The various is

forms

of the

one

is

of

tube of The

best

Knorr's

of these.

The

with

air

the

through B

preferably

to

more

with

a

of

contains

the

using this apparatus

acid

the

of

the

more,

into

distilled water. draw

during the

the The

current

a

entire

process. the stone,

for

caustic entrance

Open the stop-cockon

the acid slowly;

or

decomposing hydrochloric. The guard-tube

fragments prevent

of

filter-pumpto

apparatus

concentrated

is filled with

soda-lime,

or

cc.

is connected

bulb

the air.

50

the

apparatus, Fig. 94,

method

A

follows:

with

A G

as

of

one

weighed quantity, 5 grams finely powdered limestone, is introduced

the

flask

of alkalimeters.

is made

liberated

the gas

soda, potash, of

carbonic

bulb-tube passes

B

with

or

with

acid and

through

C

admit

the

con-

392

ANALYSIS

denaer

D, where

OF

ETC.

LIMESTOMB,

is condensed,

of the moisture

most

removes

the tared

through of

1.27

the

of

trace

every bulbs

F, containing

specific gravity, which

residual passes

and

moisture,

the The

should

gas

When

flow

bulb

the

at

the

carefully, finally boiling Iwnic a

few

acid.

tubes

absorption

should

after

minutes

carbonic outlet

Air

acid.

of F

while

of carbonic

iscompleted, place case,

in

and

weight

quotient

after divided

a

heat

the

be

few

by

multiplied by

be

patash

the

tion, solu-

abaorbs

and

minutes

to

the

the

the

weight

100

is the

of

of

expel

When F

the

to

flarii car-

for

inlet and prevent

the

the

operation

in the

Ijalance-

them.

The

material

used

percentage

the

of all tite

the

over

second.

aj^jaratus

removal

guard-tubes

weigh

per

contents

weighings,

moisture.

filter-pump.

5 bubbles

placed

the

making

the bulbs

|

F, which

through

insure

to

or

j

acid, and

the

and

the

passed

should

acid

potash solution

carbonic

liquid slowly,

boiling,

Caps

G

of 4 to

rate

is empty,

B

bubblca

gas

94.

through

ecapes

the

guard-tube

Fra.

dry

caustic

from

water

the

through

on

a

absorbs

air, containing

the

water;

!

sulphuric acid,

through the bulbs E, containing concentrated which

thence

increase and

of carbonic

the acid.

DETERMINATION

A

similar

apparatus

flask,with

cork

connections

and

apparatus, proceed

Fig.

refers to

Fill the

95.

acid

with

2

to

the

Lift the stopper open the acid. In the carbonic ^"

The

description the

left,to above

sulphuric

right with dilute Weigh the flask and the

approximately 1.5 powdered limestone, by

the

at

and

D.

concentrated

of the

opening

rec-

introduce

then

grams

as

Schroetter's

with

the

on

that on acid, and acid. hydrochloric

contents,

tube,

U

follows:

as

tube

bulb,

upper

ordinary

an

of the condenser

carbonic

of

using

empty

an

393

ACID.

fitted up,

be

may

determination

the

similar

or

CARBONIC

by Gladding, instead

commended In

OF

tube, hydrochloric-acid

the

on

weigh again.

left,and

admit

stop-cock and

decompositionof

acid is set free and

little

a

the stone, the

bubbles

through

retains any watery otherwise pass o"f with the gas. that would Repeat vapor acid carbonic time time until to no this operationfrom more the

"

sulphuricacid, which

gently disengaged. Heat from the solution, cool, and is

wiping

the

case

a

few

that

of

that

of

100

to

The

to

acid expel the carbonic weigh. After cooling and

apparatus, it should be placed inside the

balance-

weight i*^ acid set free. Divide this weight hy the carbonic used and the limestone multiplythe quotient by minutes

obtain

before

weighing.

the percentage of carbonic

carbonic

acid

in the

loss in

The

limestone

acid. in sugar

used

facture manu-

calciiun;a small with magnesium. sionally Occain combination portion is sometimes the stone contains a vein of dolomite,a carbonate is almost

of calcium In

the

and

entirelycombined

magnesium. of calcium

the

percentages

are

given, the percentages The

acid

or

of

magnesium the

two

percentage of calcium

percentage of calcium carbonic

sulphate of calcium,

of gypsum,

absence

calculated:

with

in

the

carbonate

magnesium

and

if either

carbonic

carbonates

acid be

may

oxide

(CaO) Xl.7857

(CaCOj);

the percentage

carbonate

(MgCOj)

=

of

tiplied mul-

by 1.91(5=the percentage of magnesium carbonate. contains 54.8 per cent A sample of limestone Example. calcium oxide and 43.4 per cent carbonic acid; required,the "

percentages of calcium

and

magnesium

carbonates.

394

ETC.

LIMESTONE,

OF

ANALYSIS

Calculation. 54.8

1.7875=97.96,

X

97.96

=43.16, carbonic

54 J5

"

"43.16

43.4

calcium

percent

in

acid

0.24, carbonic

"=

carbonate.

acid

calcium

the

-

in

bonate. car-

the

magnesium

magnesium

carbonate.

carbonate. 1.916

0.24 X

0.46, the

"

cent

per

calculate

sugar-house chemists

Many

order

in

this way,

economize

to

will supply all the

method

time.

the

In many

information

in

caibonates

this

cases

relative necessary usuallyadvisable to

purity of the stone, but it is not depend entirelyupon it. A serious objection to this process is the fact that there may in the determinations be slighterrors to

the

calcium

of the

false both

deductions. bases

the

the

and

limestone

Digest

5

a

small

more

the

drops

at

boilingand a

a

cium, of cal-

sulphuric

powdered limestone ter Dilute the solution,fil-

beaker, to

add

The

"

of the

hydrochloricacid, using heat. it,and wash the residue thoroughly with

heat it to

of

percentage

with

a

Acid.

quantities of sulphate

from

or

grams

in the filtrate,

lead to

rule, to determine

Sulphuric

of

is calculated

which

would

which

acids.

contain

may

acid

advisable, as

It is

Determination

261.

acid.

carbonic

and

solution

volume

a

of barium

centrate Con-

hot water. of about

50 cc,

chloride,a few move Re-

time, maintaining the boiling temperature.

lamp, after each addition of the chloride, to permit the barium sulphate to settle,and test the Continue the boiling supernatant liquid for sulphuric acid. the

from

beaker

of the solution

and

the

additions

the

of the

reagent so long as a Collect the precipitated

precipitateforms; set aside over night. barium wash it with sulphate in a tared Gooch crucible, hot water, heat it to redness,cool and weigh it. The weight of barium sulphateX. 343 -^ weight of limestone used X 100 percentage of sulphuric anhydride (SOj); the weight of =

barium =

sulphateX

.5833

percentage of calcium 262.

Notes

on

be necessary in some portion of the stone

weight of sulphate. -=-

tlie Analysis of the

than

limestone

of Limestone."

determinations

1 gram.

used X 100

to

use

It may a

larger

If so, it is convenient

to

396

ANALYSIS

(e) Heat add

OF

filtrate and

the

from

washings

solution

concentrated

a

ETC.

LIMESTONE,

oxalate

of

(d)

boiling,

to

also

of ammonium,

boiling. Allow the mixture to stand until clear, which, if the analysishas been rightlyconducted, requirestwo heated

to

three

or

decant

minutes;

dissolve

the

solution

clear

the

hydrochloric add

precipitate in

cipitatewith ammonium hydrate. Allow as before, and then wash the whole the

filter and

and

oxalates.

wash

with

into

hot

until

water

filter,

a

and

repre-

settle and

to

cant de-

precipitateinto chlorides

free of

Dry the filter and contents, ignite in a blasta crucible,at first cautiously, then over

platinum lamp, until (CaO); weight

the

cool

under

as

a

Divide normal

calcium

into

oxide

calculate

and

desiccator, weigh

a

of calcium

to terms

methods. acid

is converted

residue

the

(CaCOj) as in the previous with normal hydrochloric

carbonate

Titrate the residue

check.

percentage of calcium

the

hydrochloricacid

carbonate calcium

for

required

by

(=cc. of

5

carbonate),

of cubic centemeters quotient from the number of normal hydrochloric acid required for (a), and multiply the remainder by 4.2 to obtain the percentage of MgCOj.

subtract

the

Sundstrom

that

states

this

ANALYSIS

"

Determination

Add

to form

in

the

form

of

with Transfer

the

portions cc;

with

a

a

of

the

mix

of the 264.

the

=

lime, and

the X

Oxide

in Lime.

filter. of

lacmoid

weight 100

Determinatio^

=

Brix

to

a a

of

grams

excess

forms

residue

mortar

10

an

of 35-40"

above

solution

phenolphthalein or readingX.028

and

Calcium

Add

lime, which

and

normal

rapid and

LIMB.

ca.) to

cc.

solution

solution

from

(30

thick milk.

the

solution

sugar

100

a

OF

of the

sufficient water

mortar,

very

for technical purposes.

accurate sufficiently

263.

is

method

lime, in

of pure and mix

soluble 100-cc.

sucrose

mately it inti-

saccharate.

flask,using

the compositon to wash and to complete the volume Titrate

10

of

cc.

hydrochloric acid as

an

of calcium

indicator. oxide

a

the

a

last to

filtrate

(300), using The

(CaO) in

percentage of calcium oxide. of the Proportion of

burette 1 gram

Un-

DETERMINATION

burned

and add

water, heat

OF

Slaked an

Lime.

expel carbonic

to

solution

cochineal the

of lime

gram

with

sulphuric acid (302) and

if present;

other

or

1

suitable

add

few

a

drops of

indicator,and

tain ascer-

sulphuric acid used, by titration with hydrate (304). Calculation: (cc. of nonnal of

excess

sodium

normal

acid

397

OXIDE.

Slake

"

normal

of

excess

CALCIUM

soda the solution)X. 028 sulphuric acid" cc. of normal total weight of calcium, as calcium of the oxide,in 1 gram "

lime, andX

This

oxide.

number

slaked

and

Metliod.

with

lime

Both

"

calcium

as

oxide

calcium

as

of Gaicium

Determination

ner-LiUnge

calcium

percentage of calcium

"

of unbumed 265.

of total

the percentage

100=

oxide.

Oxide, etc.

the above

centage per-

"

Dege-

determinations

may

titration, using phenacetoline as suggested i"y Degener and appUed by Limge. Slake a Weighed portion of the lime with water, add a few be made

one

drops of phenacetoline solution and titrate with normal the acid until the yellow color hydrochloric acid. Add This reading mul-^ changes to a red, and read the burette. Continue tipliedby .028 gives the weight of calcium oxide. of a red color the addition of the acid; the solution remains calcium

is saturated, then

until aU

the

yellow.

It is advisable

to

practice with material burette reading multipliedby

calcium are

calcium

as

determined

limestones

known

of

golden

few

times

composition.

The

gives the total weight

.028

unbumed

The

a

a

and

slaked

of

limes

by difiference.

Complete

206.

oxide.

to

this titration

make

for

dhanges

Analysis.

be

may

applied for

The

"

methods

further

a

described

for

analysis of the lime

if required. ANALYSIS

OP

SULPHUR

Estimation

267.

of

AND

the

SULPHUROUS

Impurities.

of the powdered sulphur to gram at well-fitted glass stopper. Add

bromine-water

saturated dissolves

2 to 3.25

and,

part

of

as

at

the bromine

water

flask

a

per cent of bromine least 15 parts bromine

to

insure

to

U3e

Transfer

"

0.5

provided with

time

one

shake

and

sulphur, it is advisable

ACID.

an

a

of

excess

thoroughly. Water at ordinary temperatures,

from

are

required 275

to

400

for cc.

1 of

sufficient of the reagent for the

398

ANALYSIS

ozidation

of

to

expel

with

Wash

the the

hot

convenient

sulphur

in

acid

practical

impurities

freedom

cent

f eld

Pass

M

If

acid. volume must

of

gas

collected

be

and

dried

water,

sulphate

barium

(SOa)

the

in

1

the

quantitative

a

in

of

1911,

used

gas

917;

the

is

and

the

filter

and

weight

a

Sugar

Journ.,

washed

phuric sul-

sulphate with

weight

sulphuric

1912,

cipitate pre-

measured

of

anhydride

used.

Int.

tion por-

of

of

precipitated

The

per

addition

desired,

of

a

presence

be

50

insoluble

An

redness.

to

the

X0.343='

in

to

Test the

by

by

40

a

minutes.

test

Gooch

a

ignited

volume

Zeitschrift.

be

must

into

acid.

forms

color

recommended

acid

hydrochloric

its

Sulphurous

in

gas

twenty

ity qual-

fragments.

is

sulphuric

sulphate

barium

of

of

Its

from

Acid

acid

to

ten

for

and

chloride

barium

phuric sul-

accuracy

pure.

small

method

for

solution

the

cf

of

percentage

determined and

sulphurous

the

soliitiop

sucrose

the

the

of

sufficient

very

Salptauric

of

following

^The "

Her/

of

percentage

the

usually

dust

from

Estimation

Adds.

is

satisfactorily

be

generally

268.

is

100.

roll-sulphur

relative

and

and

that

from with

or,

residue crucible

The

subtracting

by

purposes,

Commercial can

(261),

filtrate

the

from

directly

calculated

be

may

tion solu-

weight

The

impurities.

of

percentage

the

Gooch

A

residue.

the

the

collect

weigh.

and

dry

collecting

200*

X

bromine,

of

Boil

acid.

sulphuric

to

excess

water;

for

residue

for

sulphur

ETC.

LIMESTONE,

OF

14,

113.

hot the

LUBRICATING

Applied

Tests

209. oil tests

be

may

expensive

OILS.

Lubricating

to

in the

made

given here, while

Some

assuring the

not

^A

"

few

out sugar-house laboratory with-

specialapparatus.

or

Oils.

of the

methods will

greatest accuracy,

for sugar-house purposes. The analysis generally answer linity acidityor alkausually includes the "cold test," viscosity, and purity tests. Pour a portion of the oil,to the depth Cold Test. 270. "

and

approximately one

of

in

three-eighths inches

and

one

inches, into

half

a

test-tube

a

diameter.

Plunge

the

stir with and thermometer a freezing mixture until the paraffinebegins to separate, or until the oil ceases Remove the tube from the incliningthe tube. to flow, on into

tube

mixture the

be

cold

be

a

beginning with

noted

temperature a

one

of the

at

which Test.

flow-viscosimeter.

of the

mean

the

as

oils,and

separation of

note

oil

The test

readings

two

temperature

with

certain

of

other

the

not paraffine canthe reading is made at

hence

The

light and

Repeat the

test.

another,

the "

the

paraffinedisappears.

the

dark

very

and

eye

entire

the

accuracy,

Viscosity

271.

in

With

test.

the

record

and with

best

the

which

during

times

agree

oils, the

with

stirred

three

which

the

at

temperature

or

the

it between

hold

and

oil must two

a

to

ceases

viscosity

flow. be

test may

Engler's viscosimeter

made

is shown

is arranged for accuinner or oil-chamber The rately Fig. 06. is surrounded measuring the oil. This chamber by closes the exit-tube. A plug at the center water-bath.

The

is

apparatus

the exit-tube under In

making

a

so

arranged the

same

test, the inner

that

the

conditions chamber

oil will flow

through in comparative tests.

is filled to

the 399

mark

400

LUBHICATING

with

water

the

water-bath.

seconds

during

The

ia notel

that

experiment by

the

is

plug

lifted

required

u

temperature, and this

standard

other

or

ia maintained

temperature of

29' C.

at

OIL8.

for

and

200

means

the

time

in

of

water

to

is used

in

cc.

^

flow

into

timing

the

the

dried

cham)"er

oil

the

of

for the

flow

divided

by

a

will

given

that

teat

is

the can

in

made

a

the

the

oil.

volume

a

the

the

time

time 200

cc.

ie usual,

cumber

the

of

It

of

The

at

This

flow

of the oil to flow

same

absence be

for of

oil.

lifted and

again

of oil is noted.

cc.

required

volume

the

thoroughly

next

are

maintained

are

the viscosity as

the

temperature, In

tube

bath

specificvisoosity

pass

the

atop-watch

is filled with

plug

of 200

oils, to state tor

and

The

temperature.

ia the

A

and

the ctiamber

and

ture

flask.

flow.

inner

The

graduated

of eeconds

through

standard

an

tempenstandard

required in seconds of

water

testing

in

reqtund

orifice, which

oil,

at

the

saoie

given time of

a

with

viscosimeter, a

a

large pipette

moderately The

accurate

pipette should

'

TESTS

have

FOR

ACIDITY

be heated

to the

,

it should

and

oil

oil that

other

or

of

cc.

pipette is then

its flow

is noted Redwood

cordingto of 50

F.

at 60^

the

means

the

sample

time

required rape-

pure

in

of

state

a

for the

of

flow

of

a

to

be tested

and

before.

Ac"

conditions

same

average

rape-oil,with

of

cc.

the

obtained

required

by

noted

filled with

under

with

standardized

easily be

rape-oilis

the

be

may time in seconds

The

great purity. The

4di

ALKALINITY.

water-jacket that the oil may

a

temperature

50

AND

stop-watch.

as

required for the flow

his visco^meter,

is 535

seconds

in viscosityof the oil under examination of the viscosity of rape-oilis calculated as follows: terms of seconds required for the flow of 50 Multiply the number and divide the product by 535 (seconds cc. of the oil by 100 the

and

at 60" F.); multiply required for the flow of 50 cc. of rape-oil this quotient by the specific tion, gravityof the oil under examina-

the

the

of

experiment, and divide by .915 the specific gra\ityof rape-oilat 60" F. It is very difficult to graduate the orifice of a pipette to siderable give the desired flow. For houses of large size using conquantities of oil,it is desirable to provide a viscqsiat

temperature

important in judging of the oil for the required purpose. the suitability for Tests 272. Acidity and Alkalinity." Shake a The

meter.

test viscosity

portion of the oil with After for

oil and

the

acidity and Oils

paper.

are

273.

alkalinity.It usuallytreated

Purity Tests." and

the latter,which

testing

vegetable fats method:

bath is in

and

water

to

with

a

after

should mineral

a

be

soda.

oil for

oils,proceed

The

otherwise

test-

to

two

to

acid

the

portion of the clear and

remain

neutral

cially espe-

bearings

oil with

dis*

separate, examine

transparent.

admixture

with

animal

or

follows

by the tion saponificaTransfer a weighed portion of the oil,e.g., 2 and heat it in a watersteampressure-bottle, or

25

and

a

test-tube.

a

sulphuric acid followed

with

allowing the

cc.

of alcoholic

prepared by dissolving 40 one

should

caustic

Boil

in

standing, test the latter

on

be

tilled water,

grams,

distilled water

hot

completelyremoved, machinery may be injured.

of the

In

most

separate

water

by washing with should

is the

litre of 95

per

cent

as

potash solution. grams

alcohol.

of

good

The

This

caustic

solution

solution

potash must

be

r 452

LUBRICATING

filtered

if not

The

of

Continue

flask

from

time

bottles

the

be

the

transfer it

several

flable

the

times

with

matter

ether

to

the

oil

alcohol

oil,

be

present

by

tion, distilla-

and

extract

oil; The

residue.

vegetable

or

titrations

two

mineral

the

remove

weigh

animal

i.e.,

the

fimnel,

separatory

a

and

saponification

The

in

above, of

cc.

of

grams

extract

weigh residue

present.

the the

oil;

contents

mineral

residue,

weigh

closed

58

less

also

may

rate evapo-

saponi-

determined

is

100

heat of

by

oil

flask

with

ether;

consisting than

to

2

of

the

grams

a

the

distilled as

before;

evaporate

pure

sium potas-

cool, funnel

the oil.

saponifiable

scribed dePour

water,

separatory

mineral

as

alcohol.

of

hot hour

one

the

without

grams

of

grams

conducted,

be

flask, but

containing in

the

the

transfer

test

a

solution

a

hydroxide 2

to

animal

of

difference.

the

2

residue

using

absence

of

the

remove

the

titrate

(300),

saponifiable

a

titration,

solution

ether

the

Should

the

the

only.

reagent

acid

the

parallel

A

the

hydrochloric

strong

revolving

and

oils, the. results

and

same.

by

indicated

with

In

Kjel-

the

with

contents.

temperature

indicator.

an.

fats

vegetable

should as

as

its

blank,

room

half-normal

phenolphthalein and

in

made

down

hour,

one

mix

in

pressure-bottles.

tifed

about

to

the

to

with

contents

time be

be

must

heating

to

should

experiment Cool

the

used

suitable

are

bottle

the

flasks

The

determination

stopper

twine.

clear.

perfectly

nitrogen

dahl

OILS.

ether,

upon and and and

Should

the

bodies

are

404

For

tiibe C:

of hot of

tube

cupric chloride solution

parts

suffident

Wash

washing

a

little bottle

dilute few

BS

with

U

jMece

200

the

solution

jneoes

of copper

tube

D.

of copper

cc,

use

Each wire

to

separatee

wire

or

Wash

of the in it.

120 copper

the solution

of

grams

add

the

to

coloc

its

from

as

white

a

several

after

times

the

should the

precipitate

of

turnings time

glass tubes

to time

in

D

into and

Place

water.

in

In

be exposed

hydrochloric add cc.

last

predpitate.

the

chloride

air.

about

and

to

of concentrated with

and

precipitate

close

cuprous

the

35

change

to

water, the

water

the

possible

sti^per it, and in

off the

manipulations

these as

pour

of water

decantation,

by

water,

Kssolve

of

solution

a

87.

in

chloride, insoluble

distilled

with

filled with

chloride

staimous

crystalline precipitate.

be

quantity

Fio.

Cuprous

parts

solution

caustic-potasaum

follows:

as

small

a

of

is to

tube

prepared in

in 50

pyrogsllic add

Briz.

This

D:

chloride

cuprous

100

50"

approximately Fcrr

5 parts of

Dissolve tind add

water

PLtTEtaASBS.

OP

ANALYSIS

the as

should

a

bottle, required have

a

SAMPLING

followingmethod

The

chloride:

cuprous

bottle, add a

200

cc.

then add

chloride

the

bulb, oil may

be

may

of the

obtained

making it in the laboratory.

of

bulb then connected

the rubber

Stopper the

foil.

and

be filled half full of the solutions

should

tubes

U

and

hydrochloricadd copper

a

water.

cc.

Ready prepared cuprous dealers,and used, instead The

or

in

cupric chloride

days, shaking it occasionally,

it aside for two

set

120

turnings

preparing the

in

used

of

35

grams of concentrated

quantity of copper

bottle and

also be

may

Place

405

FLUE-GASES.

OF

with

the branches,

or

in lieu of

poured on the surfaces of the liquids. The bulb is preferable, however. 276. Sampling of Flue-gases and their Analysis. A piece of half -inch iron pipe should be inserted into each flue, leading to the chimney, reaching about half-way to of the flue. A double-actingrubber-bulb the center pump, be

"

suitable

with

flue and

valves, is used

discharging it into bulb

The

several times, to and with

expelall

pinch-cock.

a

the air it or

the

sample and

a

as

ceiver. re-

have

to

closed

tube

of

humbet

a

drawn

be

may

contain,

may

its rubber

duplicatesamples

analyzingthe samples proceed

In

and

the

open

fills the cock

burette

pinch-cock

and

from

tube

U

Open the

rise to still

the

tube

the

mark if the

D^in

and

then

the

let the

and

on

the

upper

pressure same

at

and

D

until the water

connecting and

3-way F

with

lightplug

a

of

E.

cautiouslyopen

the

cock

caustic-potassium solution

part

is not

way,

BC

on

table.

is connected

branch

B

tube

little water

a

pinch-cock and

U

more

rubber the

on

containing

in each

cotton

the

on

Fill the bottle

close the

mark, then

upper

place F

the burette, and A

the

to

:

the cocks

G to the air; lift F

cock

3-way

follows

as

close

F, Fig. 97,with distilled water,

C

used

flue.

each

on

bulb

the pump

It is convenient

that

Jbulbs so

these

soft rubber

a

the

from

the gas

drawing

should be filled with the gases and emptied

be filled with

then

in

of the

tube, lowering F

sufficient.

Fill the

fillingthe burette

with

tubes water

With by altering the position of the bottle F. of each the absorption branch u tube filled with its solution each

and

time

the

burette

with

water,

the

apparatus

is

ready

for the

r 406

ANALYSIS

Connect

tests.

the

sample-bulb with the small

the

permit a little of the

E and

side branch

FLUE-GASES.

OF

of the

gas to escape

3-way

cock

G,

U tube

into the air to

on

through

expell the air

or

previous sample from the connections. with the apparatus, and Open the cock to G to connect the the pinch-cock on the water-tube and let the gas displace in the

water

that

the bottle F,

in it will be level with

of the water

the

disconnect

Hold

burette.

sample-bulb and

levels of the water

the

zero

of the burette,

manipulate the cock

in the

bottle

Lift the

the

that the level

so

F

bottle

and

G

burette

so

will

and

caut'ouslyopen the cock on /?, and let the gas displacethe caustic potassiuni, and emptying the (J tube with gas by manipulating filling time lettirgthe water above the the bottle,bat at no rse caustic potassium solution The the burette. ICO mark on As soon will absorb the carbonic acid. as absorption ceases,

be

the

same.

hold the bottle with the surface of the water of that in the burette

and

note

the burette

in it at the level

reading,which is

tlie percentage bf carbonic acid (CO2). Next repeat these manipulationswith the residue of the gas using (J tube C. the total

Note

reading of the burette and subtract it to

obtain

the

first

the

percentage of oxygen (O). reading from last residue of gas as before,using Again proceed with the second burette reading subtracted The from U tube D. the third gives the percentage of carbonic oxide (CO). The of nitrogen(N) final residue usuallyconsists almost entirely and the percentage is obtained by subtracting the third The gases may contain very small burette reading from 100. quantitiesof sulphuretted hydrogen and sulphurous add; these introduce a slighterror in the determinations. Sulphuretted hydrogen is tested for with filter-paper lead acetate with moistened or subaoetate,which turns black

in the

of the gas. be detected acid may

presence

Sulphurous

by shaking

a

the gas in a test-tube with iodized starch solution. acid is present the blue color is discharged. After from The and

each

analysisthe

the apparatus

and

residual

the

gas

burette

should be well greased with tallow. mutton cocks

should

mixture

If this

be^expelled

left filled with a

littleof

water.

of vaselino

QUALITY

THE

OF

TREATMENT

chemical

The

WATER-SUPPLY,

THE OF

IMPURE

composition of the

is of

A

importance.

AND

WATER.

supplied

water water

be

may

sion-battery diffu-

to

a

so

heavily

matter and organic impurities as to charged"with mineral The essential seriouslyaffect the qualityof the diffusion-juices. requirements for water used in the millingprocesf except for the generationof steam, are that it be cool and dean. ,

Sugar-house.

and

waters

waste

is often

It

"

Waters*

Waste

of

Treatment

277,

them

return

to

waters, if required for the condensers

this

The

most

means

of

cooled.

be

must

cooling is by

in

usually constructed consbts

of

framework

The

entire

the

ground.

of the

apparatus

vacuum

"of

accomplishing

Such

tower,

a

as

in

and

beet-sugar countries, several stories in height. The ^oor-

of each story, in

timbers

above

a

sugar-house. Such

the

water-toWer.

Cuba

the '

practicalplan a

the

economize

to

necessary

from

Europe,

should

structure

The

are

usually covered extend

feet

30

is

waste-water

with or

lows. wil-

^ore

froi^ the

pumped

sugar-house to the top of the tower, and then flows or drips lows or down through th^ wilthrough openings in the framework floor to

from This

lowers

treatment

considerably,and of

the In

oi^anic

also

the

The

by the carbonic The

378. "

should

it should

and

acid waters of lime

of lime

in

a

pond.

water

very the oxidation

is

to

in

be

used

slight excess

i^the Is

an

completely precipitated

acid of the air.

for

Water-supply of

solid matter

determined,

and

submitted

to

be

the

itaprovesits qualityby

impure excess

^The amount be

of

temperature

diffusion-battery,the addition advantage.

finallycollected

matter.

of very

case

is

floor, and

if in a

the

tery. Diffusion-bat-

contained

excess

of

.3

in the

part per

water

1000

quantitative analysis. If the 407

r 408

analysisshows the

be

of .3 part per

excess

of waters,

for

possible in the selection of water that containing sulphate of sodiimi these

juiceswould affect the

accumulate

to

of crystallization

depositson

the

of

tubes

it also continues incrustations

forms

and

to on

Bicarbonates

apparatus. in the

the

the

materially

to

of calcium

Sulphate

sugar.

of

the

move; heaters,and is difficult to rebe deposited in the evaporation, the tubes of the multiple effect

lime

of

T^ellsof the

avoided, since

be

sufficiientextent

a

the chlorides

or

in the concentration

and melassigenic,

are

far

So

diffusion-battery,

a

magnesium, calcium, etc., should

salts

tion examina-

for the

calcium,

or

in

not

are

quantitativeanalysis.

on

as

of

solids

methods

For

1000.

works

see

if the

rejected even

calcium,

of

large proportion of sulphate

a

should

water

SUPPLY.

WATER

THE

OF

QUALITY

magnesia

and

battery, and

posed decom-

are

the

depositedon

are

impede the diffusion. seeking to improve waters containingsulphate

chips and In

substitute

we

sodium

salt in

for the

lime, still leaving

solution; but

obtain

we

heating its solutions,or of the juices. the concentration

depositedon For the To

add

improvement

waters

milk

of

formed

are

To

precipitated. containing sulphate

in

as

follows: and

magnesia, carbonates

normal

lime

is

sodium

of lime, add

precipitated and

the

sodium

bonate. car-

sulphate

in solution.

containingbicarbonates

waters

chlorides

the

of lime and

and

certain

systems

iron

a

Sodium

of lime

sulphates of these

and

magnesia

bases, add

mechanical

of

filtration, employing alum

by

removed

impurities are or

chloride

of

coagulaat. may

be

substituted zeolite

for

in the

lime

and

magnesia

as permutite process. through zeolite is regenerated by treating it with a common the lime and sodium replacing solution,the magnesia.

filtration

milk

caustic soda.

oiganic and

Many as

lassigenic me-

b not

serious extent

a

of lime

The

very

a

salt which

and

waters

remains

and

proceed

containing bicarbonates lime in slight excess.

The

To

of waters

to

a

lime,

of

by The salt

FERMENTATION. Fennentatioil.

379,

of

Ferment.

"

capable

substance

pr()ducingfermentation. Vinous

alcoholic

or

in temperature

fermentation. ^Liquid disturbed; rise and increase in volume; carbonic acid escapes, "

forming peculiar bubbles 15"

between

18" and

rapidly; it

very

liquid.

18" C. is favorable

and

the

30"

is checked

of the

15" C. and

below

this fermentation;

to

fermentation

A

prooeeds

entirely

ceases

12" C.

below

fermentation. ^The favorable

Acetic

with

surface

the

on

between

temperature

35" C.

ropy

substance.

Viscous

lime

Use

solution

to

check

turbid

becomes

sediment

and

starchy

and

matters

substances.

follows the

eliminate

tanks

with

this ferment

Lactic

a

sugar

is checked

may

dilute

transformed takes is

solution

(5-per cent exist in the

acrid, taste

is repulsive.

into

place

taneously. sponcharacteristic.

hydrogen are liberated. sulphuric-acid solution to

"

Odor

are

is

acid and

fermentation. ^This fermentation and

acetic

thick, slimy,

becomes

mucilaginous appearance

quantities of carbonic the

and

this fermentation.

fermentation

This

clears up

fetid odor

"

is filled

viscous; ammonia

and

deposits. The fermentation. ^The solution a

A

Wash

Finally, the solution

tween be-

are

turbid, and

"

free,and

gununy

liquidbecomes

fermentation. ^This fermentation The

stage.

Small

The

acid is formed.

Putrid

ropy;

temperatures

"

20" and a

acetic

set

Any

"

very

by acidity; hence

presence

of 66" takes of the

acid).

place spontaneously, viscous

ment.. fer-

disagreeable. This ferment use sulphuric add in washing

the tanks.

fermentation. Sugar-cane juices are

Mucous

"

this ferment

Mannite, becomes

in the presence

gum

thick

and and

carbonic

of

attacked

by

nitrogenous bodies and the air. acid

are

formed.

The

ropy. 409

liquid

SPECIAL

either (a) directlyfrom this

coloring matter

should

be

not

This solution

Solntion."

Litmus

280.

REAGENTS.

azolitmin

pure

without

used

prepared (6,c) by separating

or

litmus.

crude

from

maybe

The

crude

litmus

purificationof the azolitmin

in

the test-paper, preparation of either the solution or since the other coloringmatters present impair the sensibility. the

(a) Dissolve alcohol

containingabout

(6) Boil

100

and

residue.

to about

the filtrate to 300

with

a

and

it aside

acid.

Heat

it with

litmus cool

and

with

and

16.2

the mixture

cold water,

peculiarfieryred color and

deposit

on

dilute

100

the

of

the

on

and

add

grams

cc.

the

cc.

of

pire

the water-

precipitatewhich til the washings pssume the

addition

on

and

four hours

up

600

evaporate it

distilled water

frequent stirring. Collect wash

alcohol, by

cent

it as indicated in (6).

to

containing

of dilute

cc.

Filter the concentrate

cc.

with

cc.

sulphuric acid

concentrated

forms

200

per

preserve

the clear sDlution

Decant

water-bath

set

of 85

cc.

in 100

commercial

of

grams

of distilled water

bath

20

Filter the solution and

weight.

dilated

azolitmin

of pure

1 gram

of caustic

alkali

a

Reject the washings and dissolve out the purifiedcoloring-matterwith 100 cc. lukewarm few drops of ammonia 90 per cent alcohol to which a been Distill off the alcohol, after filtration, added. have the water-bath. the residue to dryness on and evaporate deep blue and

Dissolve neutralize

not

the

dried

residue

solution

the

solution should have Litmus

violet color.

a

solution

a

in 600

with pure

of distilled water

cc.

sodium

hydrate.

The

and

neutral

violet tint.

decomposes

when

stored

in

stoppered be kept in a salt-mouth It should bottle. bottle, which and a loose plug should be only half filled with the solution, of cotton should be placed in the mouth of the bottle to keep out

dust and

admit ^

A.

a

air.

Puschel, Oest. Chem.

Zeit.,13, 185. 410

412

this

BEAGENTS.

SPECIAL

haying in

dry the brown

just verges sensitive

a

brown

all

for

The

factory

is

This paper

tint.

exceedingly reddish

a

neutral

paper

usually sufficiently curcumin

The

purposes.

an

turns

paper

yellow with add.

alkali and on

again n^itralized. Again

This

is obtained.

paper

with

been

repeat these operations until

and

paper

sensitive

the meantime

be

may

by the followingmethod: Evaporate the alcoholic solution,obtained as in the preceding with the residue method, to dryness and extract

extracted

ether.

to form

a

solution

purer

and

Filter this extract

from

ether

the

remove

the

Dissolve the by distillation and dry the residue. this residue in alcohol and precipitatethe curcumin from solution with acetate of lead. After washing this precipitate

solution

and alcohol, suspend it in water decompose it with hydrogen sulphide gas. Collect the precipitateon a filter and it with water wash and then dry it. Dissolve the curcumin this solvent from the precipitatewith ether and remove by evaporation. The residue is very pure curcimiin. with

Turmeric

or

the control

curcuma

of the

of sufficient sensitiveness

paper

ordinsirydefecation

first method.

This

control

first carbonation.

this

of the

use

acid and

much

It is not

used

in the

satisfactory for

alkaline to turmeric.

Turmeric defecation

time

by the

disturbing influence of carbonic and potassium. Normal of sodium

the carbonates

sulphitesare

one

is made

of the

account

on

at

was

paper

process

for

is ver^ useful in the control

paper

The

process.

is turned

paper

a

of the

ordinary

reddish

brown

by lime and this color may easilybe seen by artificial light. Cane-juice that has very slightturmeric alkalinityin the cold neutral on heating, due to the combination usually becomes of the lime

with

the organic acids at the

higher temperature. Solution." Phenolphthalein Dissolve 1 gram of phenolphthalein in 100 cc. of diluted alcohol and neutralize 288.

it with

acid

defecation

or

alkali

as

may

be

necessary.

For

use

in the

cane-juice,especiallyin raw-sugar work, the solution prepared as above is too sensitive. For this purpose of

it should

sensitiveness

be

acidulated litmus

until

it has

about

the

same

good paper. 284. Phenolpbthalein or Dupont. This Paper." by soaking the very finest qualityof filter-or paper is made as

a

CORALLIN

glazed

in

paper

ROSALIC

OR

alcoholic

an

the

Dupont

solution

sensitiveness

413

SOLUTION.

ACID

of

phenolphthalein.

of the

regulated by adding paper dilute sulphuric acid to the alcoholic solution and made the sensitiveness correspond to different proportions of lime or is much used in the other alkalinityof juices. This paper control of sulphitationprocesses. 2S5.

Corallin

Rosalie

or

Acid

Soltttioii.~Dige8t-

gether equal quantitiesof carbolic,sulphuric, and oxalic acid totime at 150*^ C; dilute the mixture for some with

water,

mixture

the

evaporate matter

calcium

dryness;

to

and

alcohol

with

with

free acid

the

saturate

carbonate the

extract

neutralize

nearly

and

coloring-

the

solution

corallin in 90 (Sutton). A solution of commercial per be used. cent alcohol,nearly neutralized, may For determining the alkalinityor acidityof molasses (137) the

corallin used

alcohol-soluble

as

stain in

a

microscopy

i3

recojimended. 3S6"

with

cochineal

neutralize

287.

the

50

^Extract

"

of strong

cc.

3

day

a

of

grams

alcohol

agitation,for

occasional

water, with and

Solution.

Cochineal

and

ized pulver-

200

Filter

two.

or

of

cc.

the extract. Solution.

Plienacetolin

resident in 1000

cc.

Dissolve

"

of strong alcohol

and

2

of

grams

neutralize

the

solution. S88* 100

cc.

Paper.

lodate

with

of water

heating and

potassium, dissolved in this solution and dry it. This in

even

blue

is used

paper

Dissolve

"

in

5

cc.

2

add

grams 0.2

of water.

gram

Soak

of

starch

in

of iodate

of

in filter-paper

testing for sulphurous acid, which,

slight traces, frees the iodine

and

colors the paper

through the reaction with the starch.

289.

Nessler's

iodide in 250

Solution. cc.

of water.

"

^Dissolve 62.5 grams Set aside about 10

of potassium cc.

of this

larger portion a solution of mercuric formed chloride until the precipitate no longer redissolves. Add the 10 cc. of potassium iodide solution; then continue

solution; add

the addition

to

the

of mercuric

chloride very

cautiouslyuntil only

a

Dissolve 150 grams of slight permanent precipitateforms. caustic potash in 150 cc. water, cool and add it gradually to

the above

solution,

Dilute the mixture

to I liter.

414

SPECIAL

Subaeetate

290.

REAGENTS.

of

IjesLd.""oncenirated

Heat, nearly to boiling,for about neutral

lead

water.

Add

water

Cool,

ti"Hi.

Solution.

*!f".

of

grams

for the loss

to compensate

decant be

may

hour, 860 grams Utharge, and 500 cc.

of

an

by

of

evapora-

the clear solution.

preapred without

heat, provided

is set aside several

the mixture LUiUe

260

settle,and

solution

This

100^

acetate,

half

Sdutian,"

hours, with frequent shaking. Proceed described as above, except use The solution should be diluted with cold,

"

of water.

recentlyboiled,distilled water to 54.3^ Brix. Z9U of Bone-black for Decolorizing Preparation ^Powder bone-black Solutions* and digest it several hours with hot hydrochloric or nitric acid to dissolve the mineral

|

"

Decant

matter.

until the

Avater

add

the

washings

Dry the powdered

red.

C. and

loO"

a

saturated little

ammonia

alum

additional

The

paper.

the

When

^This

"

of

of

to render

sulphatesmay

should

also

quently fre-

water

add

in

remain

in solution to

precipitate

wished, the hydrate

by decantation with of sulphates. of Pure Sugar," The for

purifying sugar,

appointed with

analysis used solution

not

be washed

adopted by the Fourth Chemistry, Paris, 1900,

and

1

is

in

in

International

precipitatethe

following testingpolariscopes, Congress of Applied of

the

of unifying the methods countries: Prepare a hot

view

to

various

purest sugar

until

wat^

reconunendation

the

on a

of the

in

use

commercial

with

absolute

sugar

able, obtain-

ethel

alcohol.

laboratory centrifugal Redissolve and reprecipitatethe and wash it with alcohol. as before, washing it in the centrifugalwith alcohol. sugar be dried between should obtained The so pieces of sugar blotting-paperand preserved in a stoppered jar. The moia* Spin

the

precipitated sugar

in

the

{

at about

slightexcess, then enough the solution slightlyacid to litmus

was

saturated

bath,

reagent alum

conmion

by little until

only traces Preparation

committee

air

paper

cream.''

solution

it contains

method

an

litmus

blue

tightlystoppered jar.

a

precipitationof the lead is

of alumina

sugar

in

with

of lead.

excess

293.

bone-blaick

the

longer turn

no

of Alumina.

called ''alumina To

wash

bone-black

it in

preserve

Hydrate

202.

and

|

INVERT-SUGAR

OF

PREPARATION

ture

in the sugar

made

for it when

should

415

SOLUTION.

and

be detennined

weighing the sample

allowance

proper

analysis

for

for sugar of the followingmethod Wiley recommends beet or unknown origin: Dissolve 70 parts of high grade sugar the sugar from this solution in 30 parts of water, then precipitate of 90 per cent alcohol. at 60** C. with an equal volume and wash Decant the supernatant liquid,while still warm, H. W.

the

sugar

beet

sugar

Finally

alcohol. strong, warm in contain, is removed

with

may wash

alcohel

the

with absolute sugar acid in a desiccator.

alcohol

the

sulphuric

over

rafiinose,which

The

solution.

dry it

and

writer

of drying to that of the prefersWiley'smethod International Congress, as, in the latter,fibers of paper may The

adhere

to the

product. Preparation

294.

Dissolve

2.375

it to

dilute

100

fifteen hours After

sucrose.

10

at

the

it with

cubic

centimeters

1000

cc.

solution

1.188

night

over

to invert

solution

the

with

or

the

water

hydrate solution,

dilute sodium

to

of this

stand

temperature

room

very

complete the volume

and

mixture

"

and

water

hydrochloricacid, of

cc.

inversion, dilute

nearly neutralize

in

sucrose

pure

let the

specificgravity and about

of

grams Add cc.

Solution,*

Invert-sugar

of

with

Twenty

water.

contain

0.05

formula

for

gram

of

invert-sugar.

Feliling*s Solution."

295.

solution

is

as

The

34.64

grams

of pure

crystalline copper

150.00

grams

neutral

potassium

Dissolve

Fehling's

follows:

the

copper

dissolve the neutral

sulphate in

potassictartrate

sulphate;

tartrate.

160

cc.

in 600

distilled water;

to 700

cc.

caustic-

solution,specificgravity 1.12, equivalent to approximately a 14-per cent solution,by volume; add the copper solution to the alkali, stirringthoroughly after each addition,

soda

and

dilute to

1000

cc.

to strong Fehling solution decomposes readilyon exposure light. The author prefersViolette's solution for commercial method. work by a volumetric

-

Zeit. Angew.

Chem.,

1892, 333.

416

REAGENTS.

SPECIAL

VIolette's

296.

This

Solution."

solution

should

be

prepared in small quantities at a time, since it is liable to in the cold, on deposit oxide of copper, even long exposure this solution proceed as follows: to light. To prepare 34.64

chemically pure crystallized sulphate of chemically pure tartrate of soda and

grams

187,00

grams

copper;

potash

(Rochelle salt); caustic soda.

chemically pure

78.00 grams

sulphate, accurately weighed, in 140 and add it slowly to the solution of Rochelle water salt cc. and caustic soda, taking care to thoroughly stir the solution Dissolve

the

copper

after each addition. The

sulphate

copper

the solution to

Dilute

should

be

liter.

one

carefullyexamined

for

been impurities. Considerable quantities of iron have found of the most in copper sulphate from one reputable manufacturers. If the salt is impure it must be dissolved be finely and recrystallizedrepeatedly. The crystalsmust before weighing. filter-papers powdered and dried between If it is desirable to make up a large quantity of Fehling's all risk of depositionof the copper oxide or Violette's solution, in the cold may be avoided by making a separate solution of the

liter;dissolve the copper

one

liter.

Use

10

of water,

of each

cc. as

usual

of the

and

and

to

dilute it to

exactly one the

omit

tion addi-

Violette's solution.

with

invert-sugar (S94) under The

analyticalmethod.

the Violette's solution

it up

make

of the solutions

this reagent with

Check

the alkali and

sulphate. Dissolve

copjjer

should

be reduced

in

copper

by

the

0.05

10

ditions con-

of

cc.

invert-

gram

sugar.

Soxhlet's

297. solutions

are

(A) 34.639 and

Solution.

employed, prepared

diluted to 500

(B) 173 dissolved

is

copper

as

method

two

follows:

sulphate dissolved

in water

cc.

grams

tartrate

in water

and

containing volume

of

grams

Soxhlet's

In

"

516

completed

of soda

mixed

grams to 500

with caustic

cc.

potash (Rochelle salt)

and 100

cc.

soda

caustic soda per

Chemically

liter and

pure

tion soluthe

salts should

be used. 29S.

Soldaini's

Solution."

Dissolve

4Q

grams

of

NORMAL

sulphate of

ACID

and

copper

separatelyin water; on

filter and

a

to

or

boil

the

2000

cc.

heat

Acid ^

and

'^Normal

contains

normal N 2 as

one-fifth

has

Acid

of this

to

normal

49.043

are

so

pared pre-

solutions.

HjSO^

grams HCl

grams

and

are

Normal,

per

liter,

per

normal

one-tenth

frequentlyused,

prepared

half-normal

usually indicated*

are

"

etc.

"

,

,

5

as

solutions

These

hence

contain

solution.

than

prepared and

are

10

in the

following sections.

HydroQjiloric

specificgravity contains

rather

sure to in-

ing Accord-

"

rule,

a

normal, and

the

36.458

attempt

--*

The

reagent

1.20, approximately.

40.78

per

100

grams

cent

of

of

chloric hydro-

it

are

quired re-

form

a

to necessary to dilute a somewhat

grams

It is advisable

to

Acid.

of

little less than

a

quantity of the acid, e.g., 80 water,

anunonia

N

N

described

acid,

Soldaini's

with

hydrogen equiviUent. in grams (H ="/)." Thus

usually a specificgravity

acid

be approximately

the

solutions, etc.,

Standard

300.

When

ceases.

Solutions.

acid, 36.458 hydrocHloric

(decinormal) solutions are by diluting the normal

checked

add

solutions, as

sulphuric acid

",

a

cc.

plate several

hot

treated

Alkali

weighed

N,

in all 1400

they contain

case

reagent

one-fifth

be

to

liter shall contain

one

active

follows:

long approximately a

this substance.

Half-normal,

etc.

or

cipitate pre-

given off, filter the solution and minutes^ then cool and dilute it to

be boiled in

Sutton

liter; normal

the

reflux condenser;

a

of carbonic

Solutions

from

that

precipitate

is

few

a

Normal

normal

the

specificgravity of the solution should

should

the

a

acid

freedom

of

on

of sodium

Transfer

water.

water-bath

carbonic

1.185.

to

cold

evolution

The

29a.

solutions,collect

until the

filtrate

reagent

the

for this purpose. Add of bicarbonate of potassium, and

more

no

of carbonate

grams

answer

distilled water;

417

SOLUTIONS.

40

it with

wash

will

grams

hours

mix

ALKALI

largeflask fitted with

a

glass tube 416

AND

cc.

to

to

1000

cc,

with

lai^ger distilled

closely approximate

the

alkali quantity. Titrate this solution with a noimal Solution (304)fmeasuring the acid from a burette into 10 cc. other suitable indi* or of the alkali solution, using cochineal correct

cator.

The

preliminarytitration should, 1

Volumetric

Analysis.

most

conveniently,

418

SPECIAL

show 9.6

be added

checked

further

the

alkali

determination.

chlorine

of water

other.

The

strength, and should

and

add

with

ease

(Mie

should tent. con-

preparing

in

use

solutions, since and

acid

17.725

is

its

hy

accuracy

half-nonnal

contain

make

to

solution

for

cc.

add

of its chlorine

one

The

10

of the

cc.

determination

ascertained

be

to

oc.

convenient

a

suppose

neutralize

9.6X100=960

=40

cc.

a

standard

accurate

strength may a

is

add

This

by

required

to

exactly neutralize

solution

very

--960

1000

strong; for example,

are

alkali solution, then

of the must

be too

to

solution

acid

of the

cc.

be

solution

the add

REAGENTS.

venient con-

a

of chlorine

grams

liter.

per

1

normal

cc.

hydrochloricacid

.036458

=

=

=

Standard

301.

normal

of the

oxalic acid

Oxalic

solutions

.03545

''

a

.02804

"

CaO

This

is

and

prepare,

it may

all the

preparation of

the

to

obtained

be

can

Acid."

HCl

gram

when

be

standard

the

strictly pure

used

alkali

simplest

in

and

checking

acid

solu-

oxalic

add,

tions.

Repeatedly crystallizethe from

solution.

water

of

indications

at

normal

solution,

the

weaker

solutions than This

exposed cc.

303. 28

cool

cc.

the

titration

the

to

normal

direct

of

solution, and normal

Dissolve dilute

and

63.034 1000

to

the

is

to

the

latter

from

the

show of

prepare

powdered

advisable

the

grams

cc,

45.018

use

It

add

grams

in pre-

to

employ

normal

mal nor-

tion solu-

keeps well, provided it is

sunlight. =

.06303

sulphuric dilute alkali.

to

HjC20^.2HjO.

gram

Acid."

Sulphuric

concentrated

with

Reject all crystals that

prepared

oxalic acid

Standard

in

normal, usually the one-tenth

be

should

required, since

as

1

weight solution.

normal

paring

acid.

and

crystals thoroughly

preferably,dry

or,

100" C. t.o constant

not

the

efflorescence.

in distilled water

this acid the

Dry

ordinary temperatures.

air at

obtainable

purest

add

1000

Add to cc.

approximately distilled Standardize

water,

by

'

420

REAGENTS.

SPECIAL

""

Phenolphthalein

be

cannot

used

as

with

indicator

an

ammonia.

Decinormal

305.

Dissolve

3.16

decinormal acid

soon

The

60*^

approximately

addition

acquires

and

little

a

must

be

time

of

cc.

approximately little

by

pennangana^e

pink

as

color.

rose

or

maintained

at

allowed

be

must

in

tightly

a

time

time.

to in

change from

the

time

bottle,

stoppered

to

solution.

time,

It rather

should

and

formation

The

for

of is

decinormal

cc.

of

permanganate

Determinations. 1

a

Solution "

is

cc.

grams and

dilute

^This

solution

equivalent of to

reducing-^ugar

composition.

1

"

J

Permanganate

306.

water

from

indicates

determine

to

to

attempt

potash

4.9763

preserved

checked

precipitate

a

simpler

than

be

be

a

factor

a

maintain

the

strictly decinormal.

solution

that

should

solution

potassium

of

Permanganate

by

the

faint

solution

the

C,

a

few

a

to

oxalic

solution of.

with

titration

reaction.

the

1

the

of

temperature

solution

the

1000

to

decinonnal and

water

permanganate

solution

the

as

of

dilute

by

of

cc.

the

Discontinue

little.

10

Warm

add

and

To

volumes add.

sulphuric C,

C0"

acid.

several

checked

"

permanganate

and

water,

conveniently

Potassium.

dry

pure,

distilled

in

is

oxalic

add

dilute

chemically

(KMnOf)

solution

This

cc.

of

grams

potassium

of

of

PermanKanate

to

.01

1000

cc.

This

determination

be of

of

in

Cu

such

strength Dissolve

copper.

potassium

solution

"

Beducing-susar

should gram

KMnOi

gram

00636

".

for

of

permanganate

.0316

shoidd

material

in

distilled

be of

checked known

REFERENCE

TABLES

FOR

SUGAR

USE

LABORATORIEa

IN

TABLES.

REFERENCE SHOWING

TABLE

307.

REAGENTS;

COMMERCIAL

SOLUTIONS,

ETC..

Acid Sulphuric (Oil of Vitriol).

ALSO.

HjSO*.

Impurities.

Pb,

PRESENT

THE IN

RECOMMENDED

Symbol.

Name.

IMPURITIES

THE

IN

STRENGTH

OF

ANALYSIS.

Stbxmoth

Solution,

op

btc.

and Concentrated dilute. As, Fe, Ca, 1 part To dilute acid N,04. pour 9 into by measure parts

HNO"

distilled

Use

water.

celain por-

dish. Acid.

Nitric

flNO,.

HCl.

H,S04,

Concentrate to

Hydrochli)ric

HCl.

CI, FejCU,

HaS04,

Acid

JMuriaticAcid).

SOa,

Dilute

Nitro-hydroctiloric

(Aqua

by

Acid.

add

1

=

dilate.

1 part

9 parts water. Concentrated

parts

As.

and

dilute

To

and

acid

dilute.

acid

part

9

to

water.

Prepare adding

regia.)

when 4

1

to

aQid.

required chloric hydronitric part

parts

Use

conceutritted

acids. Acetic

Acid.

H4C'j|Oj.

H,S04,

Cu/Pb,

HCl, Fe, Ca.

Concentrated Dilute

1

=

acetic

dilute.

and part acid

cial gla-

pui-e 1

to

part

water.

Sulphurous

HjSOi.

charcoal,

To add

Acid.

in

Boil,

wash

erated

Ha804.

the

gas

gren-

it by passing water, and finally

through

into

it

pass water.

flask,

a

concentrated

in

cold

very

Preserve

the

lution so-

tightly -stoppered

bottles. Oxalic

Acid.

HfCgO^

Fe, K, Na, Ca.

Dissolve

1

of

part

acid

in

9

parts

crystallized tilled dis-

water.

Snlphui'etted

Use

HoO. in

Hydrogen.

the

Hydrate

Sodic

KHO.

Potassic

or

NaHO,

in

and chlorides.

drate. Hy-

NH4HO.

Sulphate,

the in

(Soda and for

Ammonic

ride, chlo-

ate, carbon-

tariy

or

Wash

gas.

Al, SiOa, phosphates, Dissolve phates, or sulpotash

Hydrate.

state

gaseous solution.

water

is

will most

stick 30

soda

parts

less

ter. wa-

sive, expen-

usually purposes

swer an-

in

place of potash.) water Stronger of monia am(.96 specific gravity) and i above strength.

matters.

Baric

Hydrate.

BaOsHj.

Dissolve

crystals in filter, and stoppered

1 20

part pnrts

preserve bottle

422

of

the

water

;

in

RBAGENT3

AND

STRENGTH

RE^QENTS. Nams.

Stmbol.

"

OF

Conf

423

SOLUTIONS.

t ntied.

Strength

iMrURITIBS.

Solutioh,

of

KTC.

Calcic Hydi"te.

Sodic

Aramo-

OaOgH,.

Slake lime in water, filter off the solution, and preserve out of coothe air. tact with the Dry and powder It may salt. be made as follows: Dissolve 7 parts

Na(NH4)HP04.

nic

Hydric Phosphate. (Mici'ocoHQiic Salt.)

disodic hydric phosphate

(NaaHP04) ammonic

and 1 chloride

part 2

m

ter, filwater, and separate the quired resalt by crystallization.

parts

boiling

Purify by Sodic

Biborate.

recrys-

tallization. Heat to expel water of crystallization and

NaaB40v.

powder. Sodic Carbonate.

NaaC0|.

Chlorides,

phosphates,

sulphates,

or

Use the powdered salt dissolve in 5 parts

water.

silicates.

Aramonic

Sul*

Dissolve

(NH4)aS04.

1

part

in

5

Dissolve 1 Purify the commercial parts water.

part

in

6

phate.

parts water. (N 1X4)01.

Amnionic

Chloride.

Fe.

dition adof ammonia: filter. Neutralize trate filwith HCl ;

salt

by the

concentrate

and

recrystalllze. Aramonic

Saturated

(NH4)N0,.

solution.

Nitrate. Ammonic Oxalate.

(NH4)aCa04.

Ammonic Carbonate.

(NH4)aC0,.

Purify by recry stallizition.

Pb, Fe,

sulphates, chlorides.

Dissolve

parts

1 part

in

20

water.

1 part in 4 Dissolve 1 add parts water, and specific part ammonia, .880. Dissolve the

gravity Ammonic

mo-

lybdate.

salt

in

decant ammonia, the clear solution slowlv into nitric acid, stroDg

strong

stirring thoroughly till redisthe precipitate Ammonic

Yellow Ammonic

Potassic Potc"slc Iodide.

phide. sul-

solves. Saturate 8 parts with HaS, add 2 parts ammonia.

(NH4),8.

Prepared by dissolving phide. sulsulphur in ammonic

(NH4)aSj phide. Sul-

Dissolve

phate.KaS04. Sul-

KI.

monia am-

then

1

part

in

10

1

part

in

60

parts water. lodate,

Dissolve bonate. parts water. car-

424

KEAGENTS

AND

CoA^^ntied.

REAGENTS."

Symbol.

Name.

IMPUIUTIES.

Stbbnoth

Dissolve

Bi-

chromate.

Potassic

Ferri-

Dissolve

10

1

part

in

10

1

part

in Better when

to

solution

prepare Potassic

in

water.

parts

cyanide.

part

water.

p^rts

K"Fe,Cyja.

1

water.

parts

Chroiiiate.

btc.

Solution,

of

Dissolve

Sulphates.

Potnssic

PotAssic

SOLUTIONS,

OF

STRENGTH

12 quired. re-

in 13 1 part Dissolve glucose parts water, or, for work, 1 part in 50

K4FeCy6.

.

Ferrocyaaide.

parts water. Chloride.

Baric

BaCl,.

Di. solve commercial parts water. salt bv passinfr HaS through it

Purify

the

1

part

in

10

1

part

in

15

and

crystallizing. Baric

Nitrate.

Dissolve

Ba(NO,),.

water.

parts Baric

Add

BaCOs.

Carbonate.

Calcic Chloride

CaClf.

Calcic

CaSO*.

Fe.

Ferrous

MgSO*.

Chloride

Dissolve water.

serve pre-

tle. bot-

1 part in 5 parts

water.

parts

Dissolve parts cold

FeSO^.

Sulphate. Ferric

dered pow-

of the much as Dissolve salt as possible in water (in the cold), filter, and the filtrate. preserve 1 Dissolve part in 10

Sulphate. Magnesic Sulphate.

the

to

water

and carbonate in salt-mouthed

FeaClft.

1

in

10

part

in

10

part

in

10

part

water.

1 Dissolve water. 1 Dissolve parts water.

parts Cobaltous Nitrate.

'

Cupric Sulphate.

CO(NOa)a.

Fe, Ni, etc.

CuSO*.

Fe, Zn.

For

by *'

work

sugar

C.

For page work

purity

tions. crystalliza-

repeated

the so-called Even ways alsalts p." cannot be depended upon. see Fehling solution 415. For ordinary I part in 10 dissolve

parts water. Mercuric

HgCl,.

Mercurous Nitrate.

Dissolve

parts

Chloride.

HK,(NOa)a.

1

part

in

90

water.

1 Dissolve part in 20 water acidulated 1.2 part with nitric acid. into a bottle Filter taining conlittle metallic a

parts

mercury.

ATOMIC

WEIGHTS"WEIGHTS

AND

REAGENTS."

308.

INTERNATIONAL

Conetnu"d.

ATOMIC

WEIGHTS

FOR

Journal

iFrom

of the American 0-16

Aluminum.

..

Antimony..

.

Cadmium Calcium

Cu F Au H I Fe

Pb

206.9

205.35

Ca C

Carbon

Chlorine Chromium. Cobalt

..

a Cr

Co

Copper Fluorine Gold

Hydrogen... Iodine

Iron Lead.

TABLES

309.

Chemical

120.2 75.0 137.4 208.5 11.0 79.96 112.4 40. 1 12.00 35.45 52.1 59.0 63 6 19 197.2 1.008 126.97 55.9

As Ba Bi B Br Cd

Arsenic Barium Bismuth Boron Bromine

H

2t.l

.

OF

0-16.

Magnesium. Manganese Mercury Molybdenum.

Avoirdupois

Meter U. S. mile Kilometer 1 Acre 1 Hectare 1 U. S. liquid 1 U.

1

From

Tables

107.93

Tin

Na Sr S Sn

Unmium Zinc

U Zn

23.05 87.6 32.06 119.0 238.5

Strontium

Sulphur.

OF WEIGHTS

THE AND

.

H-1. 24 18 54.6 198.5 95.3 58.3 .

13.93 16.88 30.77 19".3 38.85 223.3 78.6 28.2 107. 11 22.88

86.94 31.82 118.1 236.7 64.9

65.4

UNITED

No.l.)

STATES

MEASURES.*

EQUIVALENTS.

"=

"="

"

lbs.) lbs.)

...

Sodium

"

av.

..

Radium Selenium Silicon SUver

-=

av.

Hg .Mo

Platinum

"

ounce

Mn

Potassium.

"*

S. apothecaries'dram S. dry quart S. bushel

"

Ag

.

....

Phosphorus.

EQUIVALENTS

pound

1 U. 1 U. (2240 1 Long ton ton (2000 1 Short 1 Metric ton

Ni N O P Pt K Ra Se Si

.

Nitrogen Oxygen

.

Mg

24 36 55.0 200.0 96.0 58.7 14.04 16.00 31.0 194.8 39.15 225 79.2 28.4

.

Nickel

MlSCELLANSOUB 1 1 1 1

LIST)

Society, Vol. XXVII,

=

METRIC

CUSTOMARY_AND

(PARTIAL

1905.

l. 26.9 119.3 74.4 136.4 206.9 10.9 79.36 111.6 39.7 11.91 35. 18 51.7 58.55 63 1 18.9 195.7 1.000 126.01 55.5

Al Sb

425

MEASURES.

453 39

5024277 grams. 37 inches (U. S. law 1 60935 kilometers. U. S. mile. 0. 62137 0. 4047 hectare. ,

2. 471

29, 574

of 1866).

acres.

cubic

centimeters.

3. 6967 cubic centimeters. " 1 1012 liters. 0. 35239 hectoliters. i"1016. 05 kilograms. = 907 18 kilograms. =2204. 62 avoirdupois pounds. "^

ot Equivalents," 4th Ed., U. S. Bureau

of Standards.

426

3

:?; m " " p "y

Est

o QQ

TABLES

OF

EQUIVALENTS.

428

MENSXTRATION.

MENSURATION.

310.

Parallelogram: area

Area

tude; paraUelogram" base X altiproduct of two adjacent sides

of

of rhombus

any =

them. angle included between of perpendicular let Area (diagonalX sum TrapeBium: it from of the two fall on opposite angles)-5-2= Area trianglesinto which it*may be divided. half the two Area of the Trapezoid: parallel sum them. sides X the perpendicular distance between Divide the quadrilateralinto two Any Quadrilateral: of the areas of these, or area trianglesand find the sum of

Xsine

=

"

=half

diagonalsX the sine of the

the product of the two

angle at their intersection. base X half the Area Triangle:

altitude

=

sides X the

half the

=

included

sine of the

uct prod-

angle half each side severally; the sum of the three sides minus and the three remainders together multiply this half sum 'and extract the square Area of an root of the product. equilateraltriangle one fourth the square of one of its of two

==

=

sides X0.433013.

Hypothenuse and being .given to find V

side of

one

the

right-angled triangle side: Required side== a

other

given side'; if the Hypothenuse* side hypothenuse XO.7071 "

two

sides

area

-^

are

equal,

=

.

Area

given to find base:

Base

=2

X

perpendicular

height. Area Two

both

to find

base. height: Height 2 Xarea-^ sides and base given to find perpendicular height,

given

angles at base

difference

of

the

made

base

this difference

=

are

sides

the

by added

acute: :

or

of the sides

: sum

difference

drawing to

Base

of

the

the

divisions

::

of

perpendicufar. Half

subtracted

from

give the divisions of it. of Area Polygon: irregular polygon; dividing the polygon into trianglesand

half the base

will

the

diagonals

find the

sum

of

of these.

areas

Area

draw

of

regularpolygon: Area distance

of

side

to

=

(length of

center

X number

a

side X pendicular perof sides)

429

MENSURA.TION.

-r-2"half to

of side

perimeter X perpendiculardistance

the

center.

Perpendicular to

center

half

=

of

side X cotangent

one

angle subtended by half the side. method): (Laboratory Irreg^ular Figure of the

figure

on

weight of this piece with

the

compare

thickness

uniform

of

paper

the paper of known area. circumference Ratio of Circle:

Draw

and that

diameter

.to

Length of ::

diameter

=

360

arc:

an

length of the of

Area

is

usually

number

:

of

degrees of the

arc

:

arc.

circle

a

3. 1415929

eter length of the arc, or diamof degrees in the arc X 0.0087266

of the circle X number =

of

Xx.

of the circle

circumference

sheet

a

=*

number 3.1416). This as (usually taken representedby the Greek letter pi, x. Circumference

it out;

cut

of

the

of the

square

=

radius Xir="' square

of

diameterXO.7854. of circles

Areas

to each

are

other

the squares

as

of their

diameters.

Ellipse

Area

:

product

=

semi-axes

of the

X3.1416

=

product

of the axesXO.7864. Prism:

Area

two

(perimeterof baseXaltitude)+areasof

=

ends.

Volume

of base X altitude.

area

=

Convex

Pyramid:

surface

Volume of

Area slant =

frustum

a

height X of

areas

them

between

X

one

proportionalbetween product). Rectangular which sides Volume

two

Prismoid bases

parallel,and =

(sum

height.

regular pyramid perimeters of the

of the two

area

two

a

regular pjrramid^

a

third of altitude.

one

the

frustum

a

the

of

of

of

sum

surface) +

convex

Volume of

of base X

area

=

of

X half the slant

perimeter of base

(

the

of

bases

two

of

numbers

(a soUd

the bases

two

bases.

regular pyramids

a

and

third

Half

=

a

mean

the =

sum

proportional

altitude. square

=

root

(Mean^ of their

bounded

by six planes,of are rectangles,having corresponding the four upright sides are trapezoids):

of the

areas

of the bases -|four

times

the

430

MENSURATION.

of

area

parallelsection

a

the

equidistantfrom

bases)

sixth of the altitude.

Xone

circumference of convex Area surface Cylinder: base X altitude. Convex end surface + the two

of

=*

"

total

area.

Volume Cone:

of

cylinder

a

height (= Volume

area

of

Frustum

circumference

=

surface)+

convex a

cone

of

^

of frustum

a

a

of

cone

of the two

them

frustum

a

third of the

Xone

of

bases. bases -|-a

(area of two

=

of the

sum

tude. alti-

pyramid relative

a

to

proportional.)

mean

Parabola

Area

:

Sphere: circle

of

third of altitude.

(half the side X

bases)-h area

between proportional

(See Volume

=

slant

of the base.

area

Area

circumferences of the two Volume

base X half

of

of base Xone

area

cone:

a

of base X altitude.

area

=

Total

mean

areas

Surface =

X circumference

diameter

==

of

square

I altitude.

base X

^

diameter

X 3. 1416

=

its

of

convex

great

surface

of

the squares

of

its circumscribingcylinder. Surfaces

of

spheres are

to each

other

as

their diameters. Volume "cube

of

sphere surface X

a

=

one

third of the radius

of the diameter X 0.5236.

Volumes

of

spheres are

to each

other

as

the cubes of

their diameters. Cask:

Volume

of

a

cask in U. S.

gallons (39 X -

square

bung diameter +25 Xsqueu*e of head diameter + 26 product of the diameters) X length-:26,470. Molasses Tanks, Crystallizers: ^ee table 35%.

L

oi

X the

OF

EVAPORATION

311.

TABLE

SHOWING

THE

CONCENTRATING

OF

EVAPORATION JUICE

431

WATER.

TO

(Percentages by Weight.)

SIRUP.

WATER

IN

432

TABLE

OF

EVAPORATION

SHOWING CONCENTRATING

THE

EVAPORATION JUICE

TO

WATER.

OP

WATER

SIRUP."Continued.

IN

1 EVAPORATION

CO

OP

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to CO CO CO CO

cdof^t^h^tNiooododoo

o"OiOO"-4"-icsicieO"^

dcotot^Od

"-tcotoooococoo"coto

F*4

cdcdcdcdco

torototoodooooodoio^

oor4i-ie"coco"^tocc"

totoa""-4eo

tooOtHcocoo"t".^co

i-itoeoOMtotooacoo*

cOcdcot^^to

tot"Jxada6o"c"oioo

"-""-(

tOt-^COCOOO

rH

cototobJto

ooododaio"oiod"-^"-"

TfooOi-i^

to

o

"

OS OS OS O

00

1 M

-

O o

C4

H

^

CO

"-i

i^.co

o

oo to

r^

o"

QQ o

$

o

csicoco^ to

cooooa

bt

o

2

00 CO

'^ t^

O

"^ 00 W

CD w

to

'*|"^OJOOOOO^OOeo

C4cocQ"^iOtoa6oc""^

s "o 00

to

to to 00 00

"^ "

ei

to c^i 00 -^

"H

OJOOMO""**f-iOT*"Ti*eo

O

CO

CO -^ "0 to

i-H

rl

rH

rH

rH

i-H

O ^

rH

to

*-i

i-i

to to -^ CO 00

r-) i-t

CO

"-"

1-1 CJ

1^

1-4

i-l

OS

"Oto'o6pCS""*to.-IocO fH

f-4

K-l

^

d

d

C9 CO CO

^tot-^toos

coooco"todOOsosi-"

to 04 e" CO CO to to

OOXOSOftOS

0O"-i"-i0IC0^^t0to

00 p T-l d

C4 '"4(to *^ CO 04 94 d CO CO -^

04 to

to

1-(

f-l

1-1

r-l

i-H

1-1

^

iH

1-1

o

'"4"

OS

-^^ to

1-itOOdCOOO

COOStOOIOOOMCOCO

osoaosoo

i-i"-i04co"^to"ot"^odocsi^t"^i-i"d'^toco rH

1-4

1-4

o

th

04 CO ""}"to CO to

rH

*-4

1-1

rH

rH

tH

04

CO X

"H

04 04 04 CO CO ^

f-4

CO

lO to

h tocotoxok

'3^

CO

OSOSOO"H"-icicO"^^

^1-1

Ho

t-i

-^WNtoCSOO^CSOOS

1-1

0.0.2

to 04

OSf-i"^t*iH

CI

o CO

Ci "* N d

loOOQO"OS

^^^^^^rHi-l

CO

X

GO a"

Q4-ie^

^^^^s^ss^l^g

COWDENBBR-WATBR.

CON

u

DGNBER-W

ATBtt.

439

CONDBNBBR-WATBB.

CO b. lO U3

CD CO "o "o t" "^ t^ r""

oc9iot*"oeocoa)eqt" "D "e" "D

to

oo

C4

ob0"

1^^

00 r"" K3 to t^

64004000

0" O

d

OOQOCOO

OH

Tfi

04 CO

C4t"ocoa"t^cocDoocoo

t^""^r* t"^00

00

^0

ach""oeo"oa"cot"e'"t""

d cc"r^t"r"r"aoo6d d

Cli-iObC4CO

a"oidd"-HC4co^coa6

S

0^-""ao

0""o"DO"cOf-"e9i-i

O.-4i-4C""C0^C000OC0 rHl-if^fHf^f^^Hf-^Pie4

Oeocoaa'^ooc4a0'4"o

x"ot^a"'"4ies'^eoi-iio

"do

""r"""tN.aoaoaba"0'H

"-ic"4eQ-4"coaoocot".c4

o^

1-tf^

"DO^00C000^OXt""

OH

iM

"-4

i-i

^

*H

^

04 es CO

i-tVi4i-"*^

co*cdodddt^c4 i-H

1-1

tH

^

i-H

0-" C9 C"l CO ^ lO

^OOCOOO^oNOitvOOO

iQ CO iQ iO CO r^ o" ^

Qdo6da"d"Hi-ie"icod

doddcotrctd^

eoa)^"-4a)aooo"-4io^

iCkQ^XOcO

o"dd^oHc^codcooo

ocor^NoH-^

KdoHObooo'HO^r^r'

"oo""-"ao

do-ii-Hcicoddoodco

r^eslr-i-^

*^

1-4

rH

i"N

f^

"-i

C4 CI

O05a6cvit"iooot^"i-i C4'C4 ,_i

^

..^

^

r^

"

C4C0^^

^o

d d d odd ^

"

*

94CO^*0

rHT-4e4C4

i-lfiH"-4v-ti^rH

^H

^"o

XO^"4tC^C4cOt""C4

i"oda6ooddd'-4"-iM'

rH

C0"DC"O

^

CO tr CO o* gs) CO

i-id ^u5

o

o

go

itOOkOQ

o

"2

""

*"'

iCOl

S.2oSa,|i (8 " .55

SOS'S: .2

o

wo

:r.9" 9i

(X /-"""

3

3

"

oJja

"'goo

0)

_

w

""*

Oi-tc^co"^"o"h"goo" COCQCOCOCOCOCOCQCOCO

g$ "B

d

O'-iCIC0^"0"t^000J

6

^

M

4J

M

O'-iNCO'*

lOiOiOiOtO

440

REDUCTION

TABLE

314.

FOR

VOLUME TO

A

OF SIRUP

Initial

SIRUP

A

OF

A

64.3"" BRIX

OF

OF

REDUCTION

THE

30"

Equivalent Sirup of

Density.

Brix ao*" Baum6. 64 3*

3

^

U V

^

5

BRIX.

WEIGHT

THE BRIX

DEGREE

GIVEN OR

54.3"

TO

SIRUP

OF

BAUMfi.

Equivalent Sirup

Initial

of

or

Density.

2

OR

OR

BAUMfi

.""

5

Brix Baum6.

64.3"

80O

^

"8

or

"

O.O.S

64.46

64.61 64.83 65.01 66.19 65.88 65.74

65.93 66.11 66.80 66.48 66.67 66.85 67.03 67. 8*2 67.40 67.69 67 77 67.95

68.14 68.32 68.50 68.69 68.87 69.06 69.24 69.42 69.61 69.79 69.96 70.16 70..34 70.58 70.72 70.90 71.08 71.26 71.45 71.63

ET 69.19 69.88 69.58 69.77 59.96 60.16 60.36 60.56 60.75 60.94

89.0

61.14 61.38

40.0

.1 .8 .8 .4 .6

.6 .7 .8 .9

81.8 21.3 21.9 81.9 88.0 22.06 2S.1 82.2 82.8 22.3

.1

223 82.4

61.7-2

.2 .3

22.4 82 5

61.92

.4

82.5

62

.6 .6

82.6

61.53

12

62.31 62. .W

"

62.70 62.91

"

.8 .9

82.6

22.7 22.8 82.8

71.88 72.00 72.19 72.37 72.66 72.74 72.98 78.10

7S.89 73.47 73.66 78.84 74.02 74.21 74.40 74.58 74.76 74.94 76.13 75.81

69.18 69.38 69.58 69 78 69.93 70.14 70.34 70.64 70.74 7k).94 71.15 71.85 71.66 71.75 71.96 72.16 78.87 72.58 78.79 73.00

73.41 73.61 73.81 74.01 74.82 74.43 74.64 74.86 75.06

.1

82.9

61

.2

23

63 70 63 90 64.10 61.30 64.49

.3 .4 .6 .6

230

.7 .8 .9

23.85 28.3 23.4

75.50 75.68 76.87 76.06 76.24 76.42 76.60 76.78 76.97 77.16

23.4 23.6 23.5 23.6 23.6 23..7 83. .7 23.8 28.8 23.9

77.84 77.62 77.70 77.80 78.06 78.26 78.44 78.62 78.81 79.00

63.11 63 31 63

64. G9

64.89 65.09 65.29 65.49 65

69

41.0

42.0 .1 .2 .3

65.90

.4

66.10 66. .30 66.50 6B.70 66 90

.5 .6 .7

.8 .9

82.9 0

23.1 23.1 23.2

67.10 67.80 67.51 67.71 67.91 68.12 68.82 68.58 68.79 68.98

73.21

REDUCTION

TABLE

FOR

OF

THE

REDUCTION OF

A

SIRUP,

SIRUP

OF

TO

THE

"4.3" WEIGHT

JETC"Continued,

BRIX.

OR

441 VOLUME

442 TABLE

REDUCrriON

FOR

THE

OF

REDUCTION OF

"

8IRUP,

TO

SIRUP

OF

THE

54.3" WEIGHT

ETC.-Co}""i"i4"d.

BRIX.

OR

VOLUME

444

AND

CONCENTRATION

FOR

FORMULA

DILUTION

(a) In percentages by weight of originalsolution: B" degree Brix after concentration; "-= initial degree Brix; cent water evaporated in terms of the weight of the x^per solution. original

^-XlOO.

X

(6) In percentage by volume of the origmalsolution: (?" specific gravityof the solution after concentration; gravity; specific ^^^initial B and h, as in formula (a): water cent evaporated in terms of the volume a;=per

of

solution. original

the

gb

x

=

100-10(";^. GB

(4)

To

F of

the volume

determine

a

sugar

solution before

concentration.

specificgravityof the solution degree Brix, and s=the before concentration;B =degree Brix, and iS" ^specificgravity 6=

after concentration

to

a

of 100.

volume

lOOSB ^^

y

"=a

"

'

Sb 316.

TABLE

SHOWINQ

A

OF

COMPARISON

THERMOMETRIC

SCALES.

(Schubaitirs Handbuch

der

techn.

Chem.

III. Aufl. I. 61.)

COMPARISON Kahren-

OF

SCALES.

THERMOMETRIC Centi-

grade.

lieit.

146 145 144 143

143 141

140 139

188 187 136 185 134 133 132 131 180 129 138 127 126 125

IfU 123 122 121 120 119 118 117 116 115 114 113 113 111 110 109

108 107 106 105 104 103 102 101

100 99

98 97 96 95 94 93 92 91 90 89 88 87 86 85 84

445

SCALES.

THEKMOMETRIC

28.33 27.78 27.22 26.67 26.11 25.55 25 24.44 23.89 23.33 22 78 22

22

21.67 21.11

20.55 20 19.44 18.89

J8.8" 17.78 17.22 16

67

16.11 15.55 15

14.44 13.89 18.33 12.78 12.23 11.67 11.11

10.55 10 9.H 8.89 8.33 7.78 7.22 6.67 6.11

i.55 I4.44 3.89 8.33 2.78 2.22 1.C7 1.11

0.55 0. -0.55 -1.11

-1.67 -2.22 -2.78 -3.38 -8.89 -4 44 -6 -5

55

22.67 22.22

21.78 21.83 20.89 20.44 20 19.56 19.11

18.67 18.22 17.78 17.38 16.89 16.44 16

15.56 15.11 14.67 14.22 13,78 13.83 12.89 12.41 12 11.56 11.11

10.67 10.22 978 9.33 8.89 8.44 8

7.56 7.11 6.67 6."

5.78 5.33 4.89 4.44 4

3.56 3.11

2.67 2.22

1.78 IM 0.89 0.44 0.

-0.44 -0.89 -1.33 -1.78 -2.22 -2

67

-8.11 -8.66 -4 -4.44

~Obn."n"ed.

446

SCALES.

THESMOMETRIC

TABLE

317.

SHOWING

A

COMPARISON

THERMOMETRIC

OF

SCALES.

FORMULiE

318.

OF

FOR

SCALE

THERMOMETRIC

ONE

OF

CONVERSION

THE

INTO

DEGREES

THE

THOSE

OF

ANOTHER.

C-8(2?'-32)-|/?. are algebraic.

if=-!C+32-ll?+32. Additions 319. HEATED

and

l2-|(F-32)-tCr.

subtractions

TEMPERATURES

APPROXIMATE UNTIL

IT

HAS

THE

OF FOLLOWING

IRON

WHEN COLORS:

MELTING-POINTS.

dIZO.

SHOWING

TABLE

EXPANSION

"

OP

MELTING-POINTS

THE

447

GLASS.

Olf

THE

METALS.

Meltingpoints " C.

Metal.

Aluminium .

657

Lead

630

827 ,

.

Arsenic

449.5

Magnesiuln. Mercury.

Bismuth Cobalt

269

Nickel

Antimony

Meltinepointa ^ C.

Mbtal.

...

633 .

-38.85

.

1435

Potassium.

1464

62.5 .

SST':::::: Iron, Iron, Steel

3"1.

1753 .

962

Sodium.

97.6 .

wrought,

GLASS

232

1373

Zinc

419

THE BT

Bailey's

OF

''

OF

ALTERATION

HEAT,

THE AS

TAKEN

BEING

COEFFICIENTS

.

Tin

VESSELS

(From

.

1600

SHOWING

TABLE

.

Silver

1060 1075-1276

cast

OF

332.

Platinum.

1084

Chemist's

EXPANSION

VOLUME

PER

Pocket-

15"

C.

Book.")

(CUBICAL)

DBORBB

AT

VOLUME

UNITY.

GLASS. EXPANBIOIV

THE

FROM"

OF

ORDINART

448

DENSITY

3J83.

DENSITY

(IN

OP

GRAMS

PER

TEMPERATURES

1

According

to

Reichsanstalt, 'From

Cireuiar

4,

M. No. No.

WATEB.

Wiss.

Thiesen, 1, 19,

0"

Abh.

der

TO

S.

Bureau

of

102"

WATER

C."

Physikalisch-Technischen

1904. U.

OF

MILLILITER)

FROM

Standards.

Al

WEIGHT

OF

1

CUBIC

FOOT

AND

1

449

GALLON.

FOOT 1 GALLON CUBIC AND (U. S. A. of P. densities the based WATER' water on des Poids Travauz International et Mesures, (Bureau Chappuis Thiesen 1907) for 0" to 40" C. arid of M. XIII; et M^moires. der Physikalisoh-Technisohen Reichsanstalt. 4, No. 1 : (Wis. Abh. The weights in air are for dry air at the 1904) for 41" to 100" C. the water 40" C. and to at a (corrected) as same up temperature

324.

WEIGHT

^31

cu.iN.)

OF

1

OF

of and of 760 mm. weights barometric against brass pressure of the air is 40" C. the temperature Above 8.4 density at 0" C. based The 20" C. v"4umetric are assumed computations to be 1 cubic that 1 liter si. (X)0027 relation decimeters, ard the on cubic inches. " 61. 023378 cubic decimeter

"16"(60"F.)

28258.580

tl6i[(62"F.)

28253.57

1

Calculated

1016.

62.2994 62.2884

by the U. S. Bureau

of

3777.623 3776.953

8.32820 8.32670

Standards, Washington, January,

450 WEIGHT

WEIGHT

OF

OF

1

CUBIC

1

CUBIC

FOOT

FOOT

AND

AND

1

1 GALLON.

GALLON."

Con"tntt"d.

i62

CAPACITIES

TRUE

SZQ.

TABLES

OF

CORRECTIONS

CAPACITIES

TRUE

WATER

IN

OF

FOR FLASKS

FROM

DETERMINING THE

THE WEIGHT

OF

AIR.i

data assumed are barometric pressure coefficient of expansion

(Following Observed cent;

FLABKS.

OF

ordinary conditions: approximating as relative =76 humidity =50 cm.; per of glass .'^0.000025 degree C.) per

of corrections give for eacfh nominal capacity and observed the amounts be added to to the apparent weight (in air contained by the flask to give the against brass weights) of the water Centimeters Cubic at 20" C. capacity in True Example: Apparent 22.3" =99.68; at adding correction weight of water 0.325=100.005, the actual capacity, The

tables

temperature

1

From

Circular

No.

19, U.

S. Bureau

of Standards,

April 1, 1914.

OF

CALIBRATION

327.

table

Circular

of Standards

Mohr's of

water

weight

weighed

as

graduated of

to

TABLE

grams.

the

check

SHOWING

weights

brass

cubic

This

table

calibrations

THE

330.

giren

MOHR'S

in

air at

the

be

is designed at

in

U.

S.

Bureau

occupied by

volume

17.5^

C.

used to

Solutions.

1

17.5** C. with

obviate

Frbutzel.)

gram

Flasks

the

normal

the

sity neces-

169.)

(See page

BOILING-POINTS

(Flourbno, SucBoss

Table

data

TO

19, April, 1914.)

should

centimeter

SOLUTIONS."

See

the No.

is the

unit

or

with

Mohr's

26.048

of "ftl""g

327a.

centimeter

cubic

from

calculated

been

has

FLASKS

CENTIMETERS.

CUBIC

(This

OF

CALIBRATION

THE

FOR

TABLE

'4K

FLASKS.

OF

SUGAR

454

EXPANSION

329.

SHOWING

TABLE

ON

AND

DISSOLVING OF

SUGAR

( From

**

Manuel

BOILING-POINTS

"

CONTRACTION

THE IN

CANE

CONTRACTION.

OP

ALSO,

WATER; SOLUTIONS

THE ON

Gallois

Agenda"

Cent

Sugar.

CODtracUoD.

Volume.

SUGAR

CONTRACTION INVERSION.

and

Dnpont.)

Specific Per

INVERT

Ome-Sogar

Gkatitt.

Invert-Sugar

Solution.

Solution.

0.00000

1 0000

1 0000

5

.99663

0.00137

Loan

10

.99744

0.00256

15

.99639 .9^46

0.00454

.99462

0.00538

1.0413 1.0630 1.0S"4 1.1066

1.Q206 U0418 1.0631 1.0656 1.1086

1.00000

0

20

330.

TABLE

0.00861

SHOWING

THE

SOLUTIONS.

BOILING-POINT "

(GsHiJkCH.)

OF

SUGAR

OF

SOLTTBILITY

d31.

TABLE

SHOWING

THE

SOLUTIONS

330.

TABLE

SHOWING WATER."

333.

TABLE

SHOWING

The or

SOLUBILITY

(After

OF

LIME

IN

SUGAR.

OF

SUGAR

fN

FXiOURENS.)

SOLUBILITY

OF

SUGAR

IN

(Hbrzfeld.)

of a small quantity of orgaolo by presence increased by a large quantity.

solubility is decreased

inorganic salts, but

THE

455

SUGAR.

SOLUBILITY OF

THE WATER.

AND

LIME

466

334.

SOLUBILITY

TABLE

OF

SHOWING

SUGAR

THE AT

SOLUBILITY

17.6'" C.

(Otto

OF

335.

TABLE

SHOWING SUGAR

SUGAR

IN

ALOOHOI

ScHRBnoLD.)

(Zeit. f. Rabenzucker-Ind.,

*

STBONTIA.

AND

44, 970.)

Calculated.

THE

SOLUBILITY

SOLUTIONS.

OF

(Sidersky.)

STRONTIA

IN

OF

SOLUBILITY

336.

TABLE

SHOWING

THE

SUGAR

(PsLLBT

337.

TABLE IN

(Jacx"B8THAl,

and

WATKR

Zeit.

La

THE

SHOWING IN

SOLUBIUTY

du

fabrication

OF

18,

640;

!" 186.)

sucre,

OF

PRESENCE

Rilbenzuckerind

CERTAIN

d'analyae

des

Matih'ea

SALTS

SUCROSE.

takjn

from

,

TraiU

IN

^

SOLUBILITY

THE

BARYTA

OF

SOLUTIONS.

SsNcnBR,

457

ETC.

BARYTA,

Suaiea,

p.

11

)

Sideraky^s

PROPERTIES

OP

1

THE

CAHBOHyDRATES,

-

!5 IIP

1-8 SI

i;^=

His

!i

t

"

I*

f

i

lip

i-i e

I

3

I

fit

pill fii,4

111 %l r-i'i

hill

iiiiii.

mm

3|J.

I :.S I;

II;

liii

J

OP

THE

CARBOHVDRATI

liillMi:! ""' fill l ! . 1 II

11^;

m

":

\i

I'i i

;

i

iiiiiMiiiilnt :

iu

m

ili.

i jiiiU'iiMi^

PROPEHTIES

OF

THE

CABBOHYDRATES.

llil

i .

"Ill Is ^i^i SaB!""!S=a:=K|

ill n "

ii|

.1 if if

lill I

i Mi

I

^

uiii

ilia

llllj^

I :,ii

111

mm

I

i iiin

'.mn

ill \\:

iln

I

M ;

-

Iml Jliiiiil

-1

mk

lit

"ill

iifU 1

J if

i

lilpilli .liiM ill ! iJiiiin i ;

hi:

11 I I

I I-

I !i:

k ll^^l Mil i

iiiiilji

468

PROPERTIES

OF

l-HE

CARBOHYWIATES.

5o

Sfl

1 ^'^

1^ "

9

"at:

S 3

il

II

ss

o

'a

9D

o

AS

o

o

o

S55Z5

fa

|2i

m

**^

0B4

SO-a "E"

92"M i^

9"n

'^

O

i

S3

1 .

g

8

o

II -"3 8|

I

1=

I

s

II

pa a

la

8

a

a

"

IC O 9"

fa

0

i

S

g

P

fa

O

a

tH

o

n

ii|i

I

Is

!=."? ?_^

g

ft

K

Pi4

93 of

5-5j-S

O

" m

(4

n

m ^"3

S

8 I

8

o

8

s

o

n OQ

s n

I

i s

lis

a

BO a a

I

SgT"

I o

4"

PROPERTIES

OF

THE

"3

S a

go d

g

d

"S

:

"

"

hi

o

"

s

^^ t .

"

0)

"

"

"^

o

s " "*

d

"

2

O*^

o " m

go

"Sp 02

n

2

"^ O Ah

I GQ

CARBOHYDRATES.

469

470

MIXTURES

FREEZING

FREEZING

339.

MIXTURES."

(Walker's

Ltst.)

T"MPERAT(TRK

Parte

From

Ainmonium Water

Nitrate.

Ainmonium Potassium Water

Chloride. Nitrate ^

to

.

.

to

From

"

to

Nitrate

,

Carbonate :

Water

From

..

....

to

.

to

Sodium Sulphate ...... Chloride.. Ammonium Nitrate Potassium Nitric Acid, diluted....

From

Sodium Ammonium Nitric

Snow Sodium

Sulphate .

From From

16*.l

-

-

10*

From

to

-

to

From

to-

8*

-12*.9

to

From

8* -18*.6

4 to

4- 50*

From

-19*5

+

3*

10*

8*

-17*3

-j-8*

12*

+

8* -15*.5-

-f to

-f 50*

From

-40*

From

7*

-f 50* to

28*.3

to

-H 50*

8* 9* .3

-

-{-8* to-12*.4

From-f

-\-50*

to-

+

From

40*

4- 8* to

32*

-

ice..

pounded Chloride

10*

From

3*

-

-12*.4

to

+ 60*

to

24*. 4

-

+ to

.

From

From

10*

4-4*

to-

10* 21*.7

-I-10*

From

Nitrate. Acid, diluted....

or

-

-f 3*.5 to

-f-50* to

19* .4

From

4- 50*

From

-

R6auraur.

-\-40* + 4*

to +

-f 10"

to

"

From

From

-|-10*

From

Sulphate Sulphuric Acid, dilut.. Sodium

l(y* la^.a

to

-

+

...

diluted..

Acid,

From

-f 10* i5*.5

+ to

From

Phosphate

Sodium Nitric

-

to

.

Nitrate.

Ammonium Soilium

From

.

Acid, diluted...

Fahrenheit.

15"".5

-

+

From

.

4" .4

-f

.

.

Chloride. Ammonium Nitrate Potassium Sodium Sulphate Water Sodium Nitric

Centif^rade.'

FAIXS"

mon (com-

to

-

20*.5

to -5*

24*.4

to-

27*.7

to

81*.6

to

to

-

16*.4

salt) Snow Sodium "

Chloride

Chloride

Chloride

Sodium

to

1

Chloride

-

-

to

22*.8

-

ice. ] .

(,com-

to

salt) Nitrate.

Ammonium

From

Sulphuric

Acid, dilu'd

0* to

Acid

to

to .

-

-25*

-f to

From 32*.8

-

+ to

to

32*

From

23*

to

32*

From

27*

-

to

-f 32*

From 34*.4

-

.

25*.8

-

to

to

0* 24*.4 0* 26*.2

-

From

30*

-

-

-

0* 27*.6

I

Snow Calciiun

From

Chloride (Chloride of Lime)..

0* to

Snow Calcium

Chloride, crystallized

From 30*.5

0*

From

,.

Acid, diluted.

-

0*

From

Snow

Hydrochloric

-

..

Snow

Snow Potash

18*

19* .5

-

(com-

pounded

or

Snow Nitric

fo

Chloride.. Nitrate ..^

Ammonium Potassium

mon

12*

.

salt)

m"on

-

ice. i

pounded

or

to

..

Ammonium

Snow Sotiium

.

(com-

salt)

mon

Sqow

ice.

pounded

or

40*

-

0*

From to

3

From

-

From 45*.5

0*

From to

-

to

to

From 46*. 1

to

+ 32*

From

0*

40*

to

-82*

-f 32*

From

50*

to

-|-32*

From

-

-

-51*

to

0* -

36*.4 0*

-

W*.9

STRENGTH

340.

TABLE

^OIL GRADE."

OF

OP

SHOWING

THE

VITRIOL)

OF

(Otto's

Tablb.)

; ULPHURIC

STRENGTH

DIFFERENT

471

ACID.

OF

SULPHURIC

DENSITIES,

AT

ACID IS"

CENT!

172

DILUTION

341.

TABLE

ANTHONYS

ACID.

SULPHURIC

OP

THE

FOB

DmUTION

OF

SULPHURIC

ACID.

342.

TABLE BY

SHOWING

SPECIFIC

THE

STRENGTH

GRAVITY.

Tempkraturb

(Fresenius. Zeitschrift

OF

HYDRATED

NITRIC

AND

ACID

ANHYDRIDE.

15"*.

f. aoaljrt. Chemie.

5. 449.)

(HNO,)

STRENGTH

TABLE

*

SHOWING

Formula

343.

OF

THE

:

NO,H

TABLE LIMB

ACID,

OF

THE VARIOUS

NITRIC

AMOUNT DENSITIES

473

ETC.

ACID.

t Formula:

+ IHHaO.

SHOWING OF

STRENGTH

NITRIC

OF

NOsH CaO

AT

IN

15"" C.

-Continued.

+ 8HaO.

MILK

OF

474

MILK

344.

TABLE UME

345.

TABLE

OF

LIME.

SHOWING OF

AMOUNT

THE

(Muriatic Lehrb.

OF

CaO

IN

MILK

OF

DENSITIES.-CMatbgczbk.)

STRENGTH

OF

HYDROCHLORIC

Acid) SOLUTIONS.

Tempkrature, (Graham-Otto*s

ACID.

HYDROCHLORIC

THE

VARIOUS

SHOWING ACID

"

d. Chem.

16'* C. 3 Aufl.

IL

Bd^

1. Abth.

p

3S-3.)

476

a48.

SODIUM

SHOWING

TABLE

SOLUTIONS

349.

TABLE

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SOLUTIONS

POTASSIUM

AND

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THE OF

THE OF

VARIOUS

QUANTITY VARIOUS

HYDRATES.

OF

SODIUM

OXIDE

DENSITIES.

OP

POTASSIC

DENSITIES.

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2

482 TABLE

351. AND

SHOWING

BAUM^,

SOLUTIONS

A

AND

AT

OF

17^" C"

SOLUTIONS.

SUGAR

OF

COMPARISON

COMPARISON THE

OF

THE

DEGREES

GRAVITY

SPECIFIC

BRIX

OF

SUGAR

(Stammbb.)*

I

3

.1

0 1

.2 .3

0.1 0 2

1.7 1.8 8 9

.4

0.8

9

.6 .6

0.3

.7

0.4 0.45

2

0.5

2

0.0

.8 .9 1.0 .1 .2

.3 .4 .5 .6

.7 .8 .9 2.0 .1 .2 .3 .4

0.0

1

2.3

0.6 0.6 0.7 0.7 0.8 0.85 09 1.0 1.0 1.1

2.3 2.4 2.4

2.5 2.55 2 6

2.7 2.7

2.8 8 9 95 0 1

1.1 1 2 1.2

1.8 1.4

1

1.02378 1.02413 1.00454 1 .02494 1.02535 1.02575 1.02616 1.02657 1.02694 1.02738

1.01570 1.01610 1.01650 1.01690 1 01780 1.01770 1.01810 1.01850 1.01890 1.01930

1.02778 1.02819 1.02860 1.02901 1.02942 1.02983 1.O8024 1.00064 1.03105 1.03146

1.01970 1.02010 1.02051 1.02091 1 02131 1.02171

1.03187 08228 03276 08311 03352

.5 .6

1.4 1.5

8.2

1.02211

.7

1.5

8.2

1.02252

.8 .9

1.6

3.3 3.35

1.02292 1.02338

1.6

CORRECTION

^

0 20

0.3

1.01178 1.01213 1.01252 1.01292 1.01332 1.01371 1.01411 1.01451 1.01491 1.01581

The

degrees

FOR

Baum6

BRIX

TEMPERATURE,

of

degrees according to Gerlach.

this

table

are

03893

03434 08475 03517 03558

SPINDLE,"

the

corrected

(Qkrlaoh.)

or

new

484 TABLE

OF

COMPARISON

SHOWING

A AND

SUGAR

OF

COMPARISON BAUME,

SOLUTIONS.

ETC."

THE

Continued.

DEGREES

BRIX

COMPARISON

TABLE

SHOWING

OF

A AND

SUGAR

COMPARISON

BAUMfi,

SOLUTIONS.

OF ETC."

THE

ConKnwed.

DEGREES

485 BRIZ

486 TABLE

OF

COMPARISON

SHOWING

A AND

COMPARISON

BAUMfi,

SOLUTIONS.

SUGAR

OF

ETC."

THE

Otwttntted.

DEGREES

BRLX

OF

COMPARISON

TABLE

SHOWING

A

AND

OF

COMPARISON

BAUME,

SOLUTIONS,

SUGAR

ETC."

THE

Continued.

DEGREES

487 BRIX

COMPARISON

OP

BUOAH

SOLUTIONS.

CORRECTION

3fi2.

BRIX

OP

TABLE

3CALE

STANDARD,

Add

FOR

REAIiINQS

THE

FOB

to

THE

BRIX

OF

CORRECTION

VARIATIONS

n"i" C. {N^'

the coirecdoD

ON

IN

SCALE.

READIHOS

TEMPERATURE

ON FROM

F.)." (GKBi^Acn.)

re^din^

at

'e

X7H' C. ma

F.) anil

Bubtnet

THE THE

490

o

SACCHAROMBTER.

OP

READINGS

TEMPERATURE

*-"

o ^

"""

o o

O

H

"

9i

08

S

a)

:s s

Q Pi

Q " H

:S

-^

o

^

a

QQ

09

"o

o

H

"*"

;^ o

'S

+"

o8

*"

S

M a

"" "a

a

TS

O

U

IS

" o

a o

"o

OS

9-

o

08

h In

O

BQ

73

oa

CO

*i

OS M

a OD

O " 08

o

S P

o CO

X O

"0 "

C"l"OOCOt^ eow^^i-iO

QOQ-^00 "o"o"o^co "

a

"

"

"

"

o o

2

^

a

a " a M

""

5

"

08

0)

0"

00

"C'O'^'^CO

COMt-ir-iO

CO t*

MO0eQ00-"4t lO^^COCO

OOCOOOMCO WNi-ii-iO

09

0)

o

-a

"^

s *x

OQ

i

73

o

a 00 "

a o

"

"

"

"

"

O

9 -a

a;

08 08

"

"o

1 O

V a

tm

OQ

Pi

"

S

0)

ea

"a "a 73

^

"

V "*"

"o 00

08

.

3

OS

08

2 M

-3

a

o M

m

a"

"2

03

ti

08

"^ a

ao

O

"0

O"HWC0'"J"

iOOt^"OS

"

"

492 354. HOUSE

SUBSTANCE

DRY

GEERLIGS' PRODUCTS

IN

TABLE

SUGAR-HOUSE

FOR BY

ABBE

[Intern. Sugar

DRY

SUBSTANCE

REFRACTO

J., 10,

PRODUCTS.

METER, p.

69.]

IN AT

SUGAR28*"

C.

DRY

GEERLIGS*

SUBSTANCE

TABLE

IN

FOR

SUGAR-HOUSE

DRY

PRODUCTS."

SUBSTANCE

Continued.

rRODUCTC.

IN

SUGAR-HOUSE

493

494

CORRECTIONS

s

s

s

s

I ^

s

FOR

THB

TEUPBRATDBB.

PER

WEIGHT

355.

CUBIC

FOOT.

CUBIC (Brix)

WEIGHT PER THE SHOWING TABLE SOLIDS U. 8. GALLON (231 Cu.iv.) AND / AT SOLUTIONS 17J" C.

(Based

upon

Stammer's

Table,

p.

482.)

495 AND FOOT OF SUGAR

496

WBIGHT

PEE

CUBIC

FOOT.

WEIGHT

WEIGHT De-

gree Weight Brix.

65.60 .76 66.0.26 .60 .76 67.0 .26 .60 .76

68.0 .25 .60 .76

69.0 .26 .50 .76

70.0 .26 .60 .76 71 .0 .26 .50 .75 72.0 .26 .60 .76 73.0 .25 .60 .75 74.0 .26 .50 .75 75.0 .25 .50 .75 76.0 .25 .50 .75 77.0 .25 .50 .75 78.0 .25 .50 .75 79.0 .25 .50 .75 80.0 .25 .50

.75

1 cu.ft. 1

PER

PER

CUBIC

CUBIC

FOOT."

Solids of

(Briz)

Lbs. 64.04

54.31 64.67 64.84 56.11 56.38 55.66

55.92 66.19 66.46 66.73 67.00 67.28 57.66 67.84 68.12 68.40 58.68 68.96 59.24 69.62 69.80 60.08 60.36 60.65 60.93 61.22 61.50 61.78 62.07 62.35 62.64 62.93 63.22 63.61 63.80 64.09 64.38 64.67 64.96 65.26 65.56 65.85 66.15 66.44 66.73 67.02 67.32 67.62 67.92 68.22 68.52 68.82 69.12 69.41 69.71 70.01 70.31 70.62 70.93 71

71

24 65

Continued. Solids

De-

greeWeight

per

Briz.

gal. 1 cu.ft. 1 gal

Lbs. Lbs. 82.49 11.02 82.68 11.03 82. 68 11.06 82. 77 11.06 82. 87 11.07 82. 96 11.08 83.06 11.10 83.16 11 11 83.26 11, 12 83.35 11, 13 11 15 83.45 11 16 83.64 83 64 11 17 83, 74 11 18 83. 84 11 20 83 93,11 21 84. 03 11 22 84, 12 11 23 84. 23 11 26 84. 32 11 27 84. 42 11.28 84. 51 11.29 84. 62 11.31 84. 72 11.32 84. 82 11.33 84. 92 11.34 85. 02 11.36 85.11 11.37 85.21 11.39 85.31 11.40 85.41 11.42 85.51 11.43 85.61 11.44 85.71 11.46 11.47 85.81 85.91 11. 4" 86.01 11.49 86.11 11.60 86.22 11.62 86.32 11.63 86.42 11.65 86.62 11.66 86.63 11.58 86.73 11.59 86.83 11.60 86.93 11.61 87.04 11.63 87.14 11.64 87.24 11.66 11.67 87.34 87.45 11.69 87.55 11.70 87.65 11.71 87, 75 11.72 87. 86 11.74 87. 96 11.75 88. 07 11.77 88. 17 11.78 88.28 11.80 88.38 11.811 88.49 11.821 88.59 11.83

497

FOOT.

Lbs. 7.22 7.25 7.29 7.32 7.36 7.39 7.43 7.47 7 61 7. 55 7. 58i 7. 61 i 7. 65, 7. 69i 7. 73 7. 76 7. 80 7. 84 7. 88 7. 92 7.96 8.00 8.03 8.07

81.0 .25 .60 .75 82.0 .25 .50

.76

1 cu.ft. 1

Lbs. 88.70 88.80 88.91 89.02 89.13 89.23 89.34 89.44

89.66 89.65 89.76 89.86 89.97 90.07 90.18 90.29 90.40

8.19 8.23

83.0 .26 .50 .76 84.0 .26 .50 .75 85.0 .25 .50 .76 86.0 .26 .60 .75 87.0 .25 .50 .75

8.27

88.0

91.70

.25 .50 .76 89.0 .26 .50 .75 90.0 .25 .50 .75 91.0 .25 .50 .75 92.0 .25

91.81 91. 92

8.11 8.15

8.31 8.34

8.38 8.42 8.46 8.49 8.53 8.57 8.61 8.64

8.68 8.72 8.76 8.80 8.84 8.88 8.92 8.96 9.00 9.04 9.08 9.12 9.16 9.20 9.24

9.27 9.31

9.35 9.39 9.44 9.48 9.52 9.56

-

.50

.75 93.0 .25 .50

.75 94.0 .25 .60 .75 95.0 .25 .50 .75 96.0 .25 .50

of

9Q.50 90.61 90.72 90.83 90.94 91.04 91.15 91.26 91.37 91.48 91.59

92. 92.

gal

Lbs. 11.86 11.86 11.88 11.89 11.91 11.92 11.94 11.96 11.97

92. 25 92. 36 92. 47 92. 58

92. 69 92. 80 92.91 93.02 93.13 93.24 93. 35 93. 47 93. 58 93. 69 93.80 93.92 94 .03 94 .14 94 25

per

1 cu.ft. 1

gal

Lbs. 71.86 72.17 72.48 72.79 73.09 73.40 73.71 74.02 74.33 74.64 74.96

11. 99 12. 00 12. 02 12. 03 12.05 12.07 12.08 12.09 12. 11 12. 13 12. 14 12. 15 12.17 12.18 12.20 12.21 12.23 12.24 12.26 12.27

Lbs. 9.61 9.65 9.69 9.73 9.77 9.81 9 86 9 89 9 94 9 98 10 02 75.26 10.06 75.67 10.10 75.89 10.14 76.20 10.18 76.62 10.22 76.84 10.27 77.16 10.31 77.48 10.35 77.80 10.40 78.11 10.44 78.43 10.48 78. 75 10.52 79. 08 10.57 79. 41 10.62 79. 73 10.66 80. 06 10.71 80. 38 10.75 80. 70 10.79 81.02 10.83

12.28

81.34

10.88

81.66

10.92

82.00 82.32 82.67 82.99 83.32 83.65 83.99 84.32 84.66

11.00 11.05 11.09 11.13 11.17 11.22 11.26

11.9^

03112.29 14

(Briz)

12.31 12.32 12.34 12.35 12.37 12.38 12.40 12.41 12.43 12.44 12.46 12.47 12.49 12.50 12 52 12, 63 12. 55 12. 66 12. 58 12.69 12.61 12.62

10.96

M.31

84.98

11.35

85.22

11.40 11.44 11.49 11.53 11.58 11.62 11.67 11.71 11.76 11.80 11.84 11.80 11.94 11.99 12.04 12.08

85.66

86.99 86.32 86.66 87.00 87.36 87.69 88.03 88, 37 88. 71 89. 06 89. 40 89. 74 90.09 90.44 12 90.78 91.13 12 12 91.48

94 37 94.48 94.60 12.64 94 71 12.66 94. 83 12.67 94. 94 12.68 95. 06^ 12.70 95. 17 12. 71 95. 29 12. 73 95. 40 12. 91.83 95. 52"12 76l 92.18

12 12

12 17 22 26 30

WANTAGE

386.

TABLE

FOR

(EMPTY

(TANK AND

(Lat

m

THE

CUHIC

IF"nDU"";

fiva

OF

THE

WANTAGE

CYLINDRICAL

HORIZONTAL

CRYSTALLIZERS,

ETC.).

IN

TANKS U.

8. GALLONS

FEET. D

tr-(0"X^XL)+231, 1728

TANKB.

CALCULATION IN

BPACE)

CARa.

CYLINDRICAL

nDta"e

-diameter

ol

in

waatsce

in cubic

Unk;

fen.

U.

All

/-depth S.

(alloiu.

dimeiuioiu

at

or us

empty

apace

dividi;iBby in

ineW.)

SCHMITZ'S

500

ONiaTXH

FOR

fHc^eo^toor^xo)

I

Q

TABLE

SUCROSE.

e"HC4co^to"or"QOO"

e^nci

0"OOOi-tCO"-4COi^CO IOt^OC4"Or"OC4tOt"

""lcDi-t OC"4tO

Mcicocoeoeo-^'^^^

"itoto

iot"ooitot"OMtor"

eciio

MC4cococoec^'4"'"t*^

loitQto

e^iot"oc4tot^oc4

"Hr^C4C^Oir""M00C0X i0r^oc"4tQt"ooi*or""

MOO ee^to

ddd"-i"-4^"-iC4ci

Mcicococoeo^^^^

latoio

"0 do C4 lO b"

Mt"C^O0C^

O

"

o

H

d

"00'00"00"00t0 Ol to t" O C4 "0 1^

O

d d d

"-"

^

C"4

1-H

1-1

e^c^

"-i

Ki

esi C4

1^ oitot"oc40i"o"N

Q

i

d

d

o

1-1 ^

tOQ"0"-""DrH(Ci.-i" o

"* en

Q

0)

OD

"-t

?D

O

0"

0.(N iO r" O 1-1

00 W l0t"OC4"Ot"OC4"Ob-

r*

C4

00 "*"

CO

^o"^ OtNiO

00

ddd"-""-" "-I"-iwN

"icieococoeo'*^^'^

loitoto

O

iO'-^"0'-""'-"t^Nt* c4iot"oiNtot"oe4

MOOCOXCOOO^a^Q ior^oc4toi"o6iiooo

MOtO ocoto

"

00* ddd"-i"-Ht"""-ioie^ OTCsiooeococo^^^^

2P a

o

00

p

O 00

go

M "^

U

"2

to

o

o

a P

ddd

1-1 "-"oiei mo^eoeoneo^'^-^yi

-Si

QQ

o

"

3"

n

Q

"90t* ocoto

i-i

loitoto

lOrHtoi-tts-Mt^cox (NtOt"OMtQr"OOI

^d^q)to"-4cp"-4oc4 Mb"06|tOXOe"9tOX

t"c")x OCOtO

ddd^^i-"i-ie""e4

Mcieoeoeooo^^^^

M"toto

"Oi-i"ciK.POXeooo e"4iot^OMtot"-oc^

^OtOOcOMr"c"t"eo lexocotoxoraiox

Meoa" ecoto

dddrHf-"i-i*-ic^c4

Mcicqooeoeo^'^^^

lotoio

to"-i"c"it"-c9o"^q"

i"otoooc4t"cox^ lOXOCOtOXOCOtOX

C" to t^

O

C4 to l" O

CO

d d d

"-"

1-1"-""-"

o""-! i""

cFi

e" "

^d

"^~o~ OCOCO

"foieoeoeoco^Tj*^^

Mftioto

to "^ "o ^V* lOXOCOtOXOCOtOX

o"o v4C0

to

cs X CO " C^tOr^O(NtOt"OcO

X

to

ddd

o

"o"Ht^wxcoo"'*o citot"oe^tot^Oco

tOfHcpcixcoa^a} laxocotooooeoto

to

ddd^i-I"Hf-lNC"

WINCOCOCOCO^^^ ^

to

t^csi X "o ^ C4tor^OC"tOXOCO

N

d "^

CO

"ien*cococoeo^^^^ i-*i-I"-ii-"Ne"

"

"

lOto

"

"

"

.

"

O

M O H

P

55

O

1^

*a"t; ^ o

Q o

to o

Q

^

"

"

"

"

"

"

"

"

"

"

"

"

"

dddi-*i-Ii-i"-HciN

Mcicocococo^

""-it^COX"^"*OtOi-"

""NXC0O"^

"

"

"

"

"

es)tot"Oc^toxOeo

loxocqtooo

"

"

"

.

...

v-eox'^ ooooco

CO

dddi-Ii-Ii^fHNci

Mc^icoco

o

"DC4toCOO"tOOOCI 04tot"oe^toxoco

"0C0 lex

CO

s

"

to

iM fi CO Oi cmot^owtoxo

C9

OOOi^*-t"^iHCI

to

^

CO

"-"

'"

"

'"

'"

"

"

"

"

'"

'"

"

'

^""^

^

I

!

I

"

"

"

1-11-JfHcicsi MCii '.'.'.'.'.'.'.'.

ddd"H lo

03

"

^~~^

(0"Nh"coa"toQOi-4 WtoNOWtOXOCO

""a

"

'oiNcocococo

to

"

"^^ ^~~^

ci F^roxco"

lOXOCOtOOOO

dddiH"-"i-Ii-Iwc"i

a

"

"

"

OB

H H

-"

"

" "

d

o

"

'. '.

''

"

'

~

'

'

"

...

(4

o

CO Csi X CO WiOt^OMtOX O

O

o QQ

to

iAt^ocmor"oeotox

c^

M

S

H

o

o

o

5

o

"-""-"

""M^oa^ t"

P

is

QQ

o p

io

QQ OD

P

o

OS^OO

to^to^t^Mr^wx. o (N

c"4 to t"

Mfttoio

"8

to

O

1^

o" "o

1^

co(n1""^o"

^

"-"

"-"

.

.

^~~'

^~~-

"

"

"

"

"

'"

^

'"

^~~-

'"

'

.

.

'"

;

.""""..".

""""....."

o

o

1-1

C4 CO ^

"^

^^

...

....

...

00

."3

ONiavaH

to CO t" X

o"

Oi-

"

.

.

r~T

Wtoi".ON o

"

."

;

"

^~~'

e^co-^iocot^xoft

e"-4d

r

'"'St:"''g*

a'"g""3""ffl"""~^

5!5:S2 5? i

iiil i! lis

scruitz'b

tablb

for

sucrose.

BCHUITZ'S

TABLE

FOB

SUCBOSB.

BCHUITZ'S

"j

3;3!33:SS%S3

TABLE

K"B

SS3S2SS"S3

STTCBOSE

S53S8SSS33

SS

SCHMITZ'S

SUCROSE

FOR

TABLE

SCHMITZ'S

FOR

TABLE

505

SUCROSE.

METHOD)."

(HORNE'S

Continued.

.

Degbebs

Bbix

and

Feb

Centb

o

Sucbobb.

20.5

21.0

21.5

22.0

22.5

23.0

9.61 9.86 10.10 10.34

9.60 9.84 10.08 10.32

10.58

10.56 10.80

9.06 9.80 10.04 10.28 10.52 10.76 11.00 11.24 11.48 11.72

9.64 9.78 10.02 10.26 10.49 10.73 10.97

49

10.82 11.06 11.30 11.54 11.78

9.68 9.82 10.06 10.30 10.64 10.78 11.02 11.26 11.60 11.74

9.61 9.76 10.00 10.24 10.47 10.71 10.95 11.19 11.43 11.67

9.80 9.74 9.98 10.22 10.46 10.69 10.93 11.17 11.41 11.66

9. 9. 72 9. 96 10. 20 10. 44 10. 67 10. 90 11, 14 11, .38 11, 62

fO 51 52 53 54 56 66 67 68 69

11.08 12.27 12.61 12.76 12.98 13.22 13.47 13.71 13.96 14.19

11. 00

11.98 12.22 12.46 12.70 12.94 13.17 13.41 13.65 13.89 14.13

11.95 12.19 12.43 12.67 12.91 13.15 13.39 13.63 13.87

11.98 12.17 12.41 12.66 12.89 13.12 13.36 13.60 13.84 14.08

11.90 12.14 12.38 12.62 12.86 13.09

11.88 12.12 12.35

11 12 12, 12

12.83 13.06

12

13.33

13.30

13.67 14.05

13.54 13.77 14.01

13 13

60 61 62 63 64 66 66 67 68 69

14.48 14.67 14.91 15.15 15.39 15.63 15.87 16.11 16.35 16.59

14. 14. 14. 16.

14. 8T

14.84 14.58 14.82 15.06

14.81

16.46

14.18 14.52 14.76 14.99 15.24 15.48 15.71 15.95 16.19 16.43

14.16 14.49 14.73 14.96 16.20 16.44 15.68 15.92 16.16 16.39

70 71 72 73 74 76 76 77 78 79

16.84 17.08 17.32 17.66 17.80 18.04 18.28 18.52 18.76 19.00

16. 17 17 17 17 18 18 18 18 18

68 92

16.78 16.97 17.21 17.46 17.69 17.93 18.17 18.41 18.65 18.89

16.70 16.93 17.17 17.41 17.65 17.89 18.13 18.37 18.61 18.86

16.66 16.89 17.13 17.37 17.61 17.85 18.09 18.33 18.57 18.81

16. fl 16.09 16.86 16.83 17.10 17.07 17.34 17.31 17.68 17.55 17.81 17.78 18.02 18.06 18.29 18.26 18.53 18.49 18.77 18.73

16. 16.79 17.03 17.27 17.50 17.74 17.98 18.22 18.46 18.69

70 71 72 73 74 75 76 77 78 79

80 8r 82 83 84 85

19

19. 16

19.11

19.08 19.32 19.56 19.80 20.04 20.28

19.04 19.28 19.62 19.76 19.99 20.23

19.00 19.24 19.48 19.72 19.96 20.19

18.91 19.16 19.40 19.64 19.88

80 81 82 83 84 85

40 41 42 43 44 46 46

47 48

14

11.04 11.28 11.62 11.76 12. 24 12. 48

12. 12. 13. 13.

72 96 20 44

13. 68

13. 92 14. 16 40 64 88

114.61

114.85

14.11

15. 36

116.09 15.33

16. 60

|16.67 16.54

12

16. 84 16. 08 16. 32

16. 56 80 04 28 62 76 00 24

48 72 96

19. 10 19. 44 19. 68

16.81 16.06 16.29 16.53 16. 17. 17. 17. 17. 17. 18. 18. 18. 18.

19.

77 00 24 48 72 96 20 44

116.30 15.78 16.02 16.26 16.50

40119.36

{19.64

19.60

19. 88

19.84

12

20.08 20.32

20.

11.21

11.46 11.69

14.55

14.79 16.03 15.27 16.61 15.74 15.98 16.22

13.81

12.59

23.5

24.0

20.0

13

13

13

9

9 .70 9 10 10 10 10 11 11 11

.94 .18 .41 .64 .88 .12 .36 .60

80 11 09 12 33 12 67 12 81 12 04 13 28 13 ,52 13 ,75 13 98 13

14.81 14.46 14.69 14.93

15.17 15.41 15.64 15.88 16.12 16.35

18.96 19.20 19.44 19.68 19.92 20. 15

14. 14 14. 14. 15. 15. 15. 15. 16. 16.

07 30 53 77 01 24 48 72 96 19 42 66

90 14 38 61

86 09 33

20.10

04 40 41 42 43 44 45 40 47 48 40 60 51 52 53 64 55 56 67 68 59 oa 61 62 63 64 65 66 67 68 69

iK=s!"K

sssma

iiii

igjgggH;

:"5"iSiS- :S5

SSiJH'SS

^!H*"!S5 llii

HiSSSHS

^S5H;3HS 'fS*

13K'!?35

HSH;35H

SS'2'HH

HHSS'S

I If

ii

CALCOLATrON

m

OF

PER

t

SiS-";S

^S"!S'';SI^5MHi

sssssi

isiona

-SSiS

S5i!52K"

iSismi

msSi

dlS^"??^^

*^-^S^^w^^

CALCU^TION

OF

PER

CENTS

SUCROSE.

60S

510

CALCULATION

r^le:;"Q"""!;33

9^^%Z'9S^9Z

OP

PER

CENTS

SUCROSE.

SsSSZSS^SS

gSSffSSS"SS

SsSSZSSlaSS

S"38SSS"S"

i

"

OP

CALCULATION

80HMITZ'

TABLE

FOR

THE

SUCROSE."

Dborbb

Brix

CENTS

PER

OF

CALCULATION

C?ontmM"d.

from

23

to

51^

SUCROSE.

24.

PER

CENTS

512

TABLE

359.

FOR

TABLE

FOR

THE

THE

CALCULATION

CALCULATION

SOLUTIONS."

OF

(Dr. Chas.

SUCROSE.

OF

A.

ZN

SUCROSE

Crampton

SUGAR

)

^Take 50 cc. sugar solution; darifv, dilute to 100 oc. aad polarize in a to the tube; multiply the reading by the factor corresponding

SOO-mm.

density

*

of the

Factor

plate

1

mm.

the

solution

to obtain

the

for Laurent instruments thick. Polariscopes of

factor.

per

cent

sucrose.)

graduated thji m'ake

by should

means

be

of

tested

a

quarts

mine to deter-

TABLE

TABLE

"

FOR

FOR

Factor

plate

1

mine

the

mm.

THE

THE

CALCULATION

CALCULATION

OF

OF

factor.

Conhnued.

SUCROSE."

instruments graduated by for Laurent should thick. Polariscopes of this make

513

SUCROSE.

meann

be

of tested

a

to

quartz deter^

514

AVAILABLE

SUGAR

TABLES.

09

d

o

0 "s

*

CO Ok

a o

a

516

OF

RECIPROCALS

361.

OF

"RECIPROCALS

"

See

pace

25C

for

11 TO

FROM

NUMBERS BY

NUMBERS.

38, ADVANCING

TENTHS.

suggestions

relative

to

the

use

of this

table.

TABLE

519

SUGAR.

INVERT

FOR

"^-ooo"o^He"eo'^l^cp^.oo"Q1-^c^eolO"p^go"o^e^^

00 00 Oft a" o" ct a" Ob a" Ob a" o

00 CO 00 00 Oft O^

Cb 0" O

O

O

O

..^^ ^ .^..^(.^(^ ,^ ^' eiC4 csiC4

o

o

o

o

"-* *H

^

i-i

d

94 C4 M

04 C4

csiesi e^' C4

o

o

iM Tf (O 00 p CO lo CO CO 00 o CI lo b- o 01 *o t"" a OOQOaOaftO"Ob06C"OOOOi-ii^^"~i0404040I^COCOeceO^

e

^ ^' ^ ^' ,4 iH

f-4

1-4oi oi 04

o*

o*

oi 04

o"

oi o"

o

C4

o

(H

CO CO

1-4

1^

w

CO PO Tf

e^'94 e^ ei c^C4

t" o" c"

04 04

fH

'"" "c a" 04

oi oioi oi oioi

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O

a

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c

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o

H Pi

US "0

Q p

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^^^^^^^^^^^^^^^

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03 O

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O

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to cot*

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"""

04 CO ^

to OO

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^

^

i~ii-li-i

1-4

04 -" "D W

P

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lo

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vH

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to CO to

X

Oft P

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d ddddd

^

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oi04oi04CO

CO

CO to t* Oft 04 "" CO 00

1-)

04 0)04

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OQ

OQ

Q^,H^iM04oio40404coeoeoco^^^^^totoioio"odd

"*"

e^OtO4O"OIO4OIO"O)04OtO4O4O4O4O4O4O4O4O40404Ol04O4O4

H

H

o

iQpioptoptoptoptopio

t".p04"5toP04"Oh-004tOt"_ ^

SS

udptoptopto

to o ^ ^ 04 tJb t* p 04 to Oft Oft Oft P O O Ol 04 Ol CO CO CO ^

to to to CO CO CO CO to to h. to 00 00 00 00 9

04040tO4O104040l04e"04"l04O404OI0404

to to 0 1-4 CO CO

o

S d o

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a "8 N

c

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.O

O 08 OQ

o

5 o

04 04 04 04 CO CO CO CO ^ tH ^ ^ i4" to to to to CD CO CO CO to t* to to to 04 04 04 04 04 C4 01 04 04 C4 04 04 04 04 04 04 04 04 Ol 04 04 04 O) 04 04 04

"o 9

to to to t" to to h" t* to to to t^ h. to 1^ 1^ t. t* b. t* t^ to t"- ts. to l". 1-1 CO to to o) 1-4 CO to to Oft ^ CO to to Oft f-i CO tc to to Oft 1-1 CO to to a

POftpOPPPi-"^i-4"-ii-4e404040404COCOCOCOCO^'^^Tf 1-1

ri

04 04 04 04 04 04

O) 04 04 04 C4

04 04 04 04 Ol O) 04 04 Ol 04 04

04 04

TABLE

INVERT

FOR

US SCO c5 o

r^ a o o

C4 ^

CD 00

i-i

1-1

,-11-1

N

"H

521

SUQAR.

CO CO r" o C4 ^ (O O) *-" CO ko 00 o CI to ^ -^ ^ "o "c "o "* CI w eo " eo 00 00 ^

COOCOCOCOCOCQCOCOCOCOCOCOCOCQPOCOCQCOCOCOCOCOCOCO

co^aoociiot""a""-i'^"owototot"Aci"i4""Dooi-ieoicao "_)00"-"r-""-"i-ii^cicicicieococoPOw"i""i""i""^"o"o"o"5

e

a

coco

CO CO CO coco

coco

coco

cooococococQcococococo

CO

coco

o ^ d

00 1^ eo -^ CI t-" o g" 00 h- " fo "O 'J' CO CO CO N "N CI w 1-1 1-1 1-1 00 CO 00 CO " CO 00 CI t* ci t* w 1^ w t" CI 1^ M t* CI t^ CI ^- CI o 1-) 1-* CI CI CO CO ^ CI CO CO ^ ^ "o t4 CO o t^ t^ oo 00 Ob a" o

COCOCOCOCOCOCO"OCOCDCOCOCOCOCOCOtot^tot^t"t^t"*t"t"

o 00 CO ^ CI o 00 00 r"fHcOi-ico,-Hiooi CI CO CO -^ -^ to to CO

o

"

(

ico*-4a"oor""ococ4f-4a"QQh"co^coci lOlOO^Oi^Oi^OCOQOCOXCOOOCO )t"t^t""xoodfta)OOi-i^cicicoco^

00 COCOCOCOCO(OCOCOCOCOCO"OCOCOCOCOt"t*t^Wt*t^t^t"t"

OCI""f"OQQOCI^(OOOOCI^COOQQC|U3t^O"rH-^(Oa"CI Cl CO ^ lO " W O) O f-i CI ^ to CO t^ 00 O 1-) CI

o

o CO

CO ^

"0"^

00 Oi

1-4

cococdcd(OcdcdtN"'t"'t""'t"it""'h^f""it"ododododxooooxxa)

It

o

OOOCI^(OOOOCI^COOOQCI^COOOOCO"Ot^^C1^CDa)

ci"4iu3CDr""xoiHe"ico-^St""cioo)Ocico^"cco"OdOi-i

CI

s

cdcdcdcocDcdt^t^t"t""r"ii"t^t^i"xooooooaoaoooooAct

h."-t^XCI"0Q^XCI(OP^qQC"C0O"09C0r""CIC0O^ ac5 "'itooa 1-1-^ co" cooooc* lO h-oci ^t^

o

i

*H

cocooo

^

"H

cic"c5cococo^^'^"^^"o"o"o"cjcocdco^t^t"t"^""

CO

cocococOcOcocOcOcOoOcococococococococococococococo

c

C0"^O^00C|OO'f00CIC0Q"00"'^00C0t*Clt*CIC0i-"C0

coooi-icb"ooooeoiot"oci*5t^ac4^i^0bci^t""aci^

e

cicic2cococo'^'^'*^"o"o"o"c"c"cocococo"^r^"^t""oo" '

o

CO CO CO CO CO CO CO CO CO CO CO CO CO CO CO CO CO CO CO CO CO CO CO CO CO

iiOO."OQ"00*OQ^QU30"C"

)iOQ"CO"COiO"

to

u5 1" O CI u) t^ " ici"oSOci"oi""ciifth-oci"5t^ 00 OO 00 Oi Oi 06 Oi C- '000^"-"i-"-"cicicicicocoeOeo 00 CO CO CO vD coco^^*^^^^^^^^^^^^^^

)d

5

coco

o

t"oc4U3t^ociior""( a" CI '4" CO 00 "-" CO to r"

_

s o

"

"

)Citor"ociu3t"Qc"iot""ocitor" (

"'

"ci^coa"i-ico"oQOOC9 i(Ocococot"t^r"""-Q000(

cococOcococococococococococococococococo*

~

'"

t^oai-ico 00 00 0)06 CO CO CO CO

Ott9C0C0OC0C0C0'c0C0C0C0t0*0t0t0"0"0U3i0*Ci0"0i0 1-^ CO "O t* o" "-" CO "o r*?5" 1^ CO "o t^ CD 17* CO M? t* CD i-Heo"Oh"( CI CI CI CI CO CO CO CO CO 3 -^ ^ :^ -^ ) ri f-t ,1 *-i i-i n OOOQ" "

COCOCOCOl

~

) CO CO

CO CO CO CO CO CO CO CO CO coco

coco

CO CO CO CO CO

^ 622 363.

DETERMINATION

TABLE

FOR

OF

THE

DETERMINATION

PURrrY.-"0.

OF

COEFFICIENTS

OF

KOTTMAN".)

PURITY.

COEFFICIENTS

OF

524

DETERMINATION

TABLE

FOR

OP

THE

COEFFICIENT

DETERMINATION I^VRITY."

OF

OF Continued.

PURITY.

COEFFICIENTS

OP

DETERMINATION

TABLE

FOR

OP

THE

DETERMINATION

PURITY."

OF

COEFFICIENTS

OF Conanucd.

525

PURITY.

COEFFICIENTS

OF

hornb'b

526

table

HORNE'3

334.

FOR

TABLE

COEFFICIENTS

W.

Dr.

OF

^

Home's

D.

analjrsisafiFords

sugar

The

and

will sink

in it

with

solutions in

lead

subacetate

solution.

the

the

filtrate.

In

reading, is the

lead

Dr.

Home's

be

the

ordinary

This

is

Brix

is the

noted

that

this

unobjectionable, provided

this

the

of

the

solution

polarize

ple: Exam-

Under

the

latter

coefficient

of

purity,

using the

solution the

of of

purity

the

Casamajor's

formula,

as

Brix

Degree

Journal

*

See

also

subthan

is used

salt. in

lating follows, in calcu-

26.048

1

38.9.

lead

method

same

ber num-

dry

table:

of

pages,

polariscope

solution.'

the

"__

p,^^^

Coefficient

to defecate

tests.*

used

Home

under

tion, solu-

drous anhy-

following

coefficients

the

using

of the

sand

a

such

powdered

the

method,

lower

After

prepare

shake

and

purity

15.4** Brix

method,

comparative

Dr.

of

can

dry

on

of

eter hydrom-

sand, filter,and

table

degree

gives somewhat

acetate,

all

and

salt

pans

dissolved

mark.

portion

coarse

15.4"; polarization 24.4.

should

It

he

cylinder and

coefficient

opposite

and

a

the

opposite the corrected Brix

that

be Brix

15^

sufficient

little

the

Cover with

thoroughly

find

the

the

unmeasiired

an

and

that

to

glass cylinder, add

small

a

To

ease.

quite

optical

199,

should

molasses

will

chemist

little practice the

in

diluted

or

in

obtaining the samples

of

described

so

nearly

VACUUM-

controlling the

of

means

or

solution

the

THE

dry defecation

of

are

of massecuite

sample

in water

IN

OP

CONTROL.

methods

molasses

and

massecuite

CALCULATION

PURITY

rapid

crystallizers. The

and

THE

method a

pubitt.

of

CRYSTALLIZER

AND

PAN

coefficients

of

purity of page

"

American 170.

Factor

X

Chemical

X

Specific gravity

,

*

Polariscope reading. Society,

36,

No.

2, 186w

HORNE's

table

of

COEFFICIBNTS

OF

PURITY.

52

f

528

HORNe's

table

op

COEFFiaENTS

OP

PURITY.

hokne's

table

op

coeppxcients

op

purity.

529

630

horne's

table

of

coefficients

of

purity.

532 aee.

INDEX

inde"

of

USED

OF

SUBSTANCSS.

substances

FOR

that

are

SUGAR-CONTAINING

been

have

or

DECOLORftiNG

PURIFYING.

FYING CLARI-

AND

SOLUTIONS.*

(A list of the abbreviationa

of

r^erenoes

is given

end

the

at

of

this

iadez.)

I. SvLPHUB;

Compounds

Acids,

DBBrvATiyiiB.

and

III, 86; 1836). Sulphide (Sievier, 1847,

(Leuchs

1. Sulphur 2.

Its

Hydrogen

in

Wooderoft,

Hlavati,

94;

Chs.. 28, 1180).

Persulphide (Hlavati, Chs., 28, 1180).

3. Hydrogen

Sulphuric Acid (Achard, about 1800, Gesch., 407; Keaaler, Z., 16, D. Z., 12. 491). 760; Hagemann, f 'S. Sulphuric Acid with Lime (M"ge, D., 115, 215). 6. Sulphuric Acid with Zinc Chloride (Thiele. Chi., 20, 404). 7. Sulphuric Acid with Zinc Sulphate (Terry, 1833, in Wooderoft, 54). 4.

8.

Potassium

9.

Ammonium

Sodium

or

Sulphate

Sulphate

10.

Sulphuric with

11.

Sulphurous Paris,

X.

1811,

Zerban,

Gesch., 423).

1830.

(Dullo, D., 155, 71; Beanes.

Sulphurous

Aoid

(Macfadyen,

Aoid

D., 167, 220).

(Possos, D., 170, 64).

(Drapies, "Bull, de 56; Perpere, 1812,

la

d'encourag.,"

Soci6t6

and

Dubrunfaut,

1829,

1908.

12. Sulphurous

Acid

and

13.

Sulphurous

Acid

14.

Sulphurous

Acid

Hydrogen

with

Sulphide (Hlavati.

Calcium

with

Bl. Ass.. 16, 759).

Bisulphite (Stolle,D., 114, 305).

Chloride

Lime

of

Phenol

and

(Menier,

Bl. Ass., 10, 165.) 15.

Sulphurous

16.

Sodium

17.

Potassium

Acid

and

Phenol

Sulphite (Perrier and

(Kowalski,

Z., 55, 396).

Possos, Z., 12, 128;

Rttmpler,

N.

Z.,

30, 204). S. ind., 47, 684). Sulphite (Cassel and Kempe, Sulphite (Beanes, D.. 167, 220). Sulphite (Prout, 1810; Melsens, C. r., 55. 729; Calvert*

18.

Ammonium

19.

Calcium

20.

Barium

21.

Magnesium

22.

Z., 12, 500).

Sulphite

with

Oxygen

(Bouillant, S. ind., 50, 189). Z., 23. 47;

(Mehay,

Sulphite

Drost

and

23.

D. Z., 24, 203). 1847, in Wooderoft. 98). (ScofTern, Sulphite N. Z., 16, 70). Ferrous Sulphite (Englert and Becker,

24.

Aluminum

25.

Aluminum

1885, 891;

Degener,

Lead

Sulphite (Boulin, 1846,

Z., 44. 456;

*

Schuls, Oe.,

Compilation

Deutsche

supplied Sugar

by

Prof.

Zuckerindustrie, through

Trade

the

with

Dr.

Calcium

Edmund

Vol. XXXIV,

courtesy

Laboratory.

15;

Brandt,

1846,

Z., 23, 27).

Mehay,

Sulphite

in Zerban,

of

Dr.

Hydrate

O. p. 9

von

(Schubarth,

Lippmann,

(Jan., 1909).

Charles

A.

"

Browne,

Z.. 2, 129).

printed

in

Translation New

York

INDEX

26.

Aluminttm

27.

Aeid

28.

Acid

29.

Acid

30.

Acid

SSA

SUBSTANCES.

OF

Manganese Sulphate (Maas6, Z., 10, 256). Sulphite (Z., 1, 254; Cassel and Kempe, S. ind., 47,

Sulphite with

Potassium

684).

Sulphite (Perrier and Possoi. Z.. 12. 128). Bisulphite (Allabard, Engl. Sulphite with Calcium

Sodium Alkali

Patent

Acid

Reynoso.

Calcium

Sulphite with

Sulphite, also with Alum

Acid

Barium

34.

Acid

Strontium

36.

Acid

Acid

(Lapeyi

(Lapesrrere,see

above).

S. ind., 9, 379).

Sulphite (Melsens. Magne^jim Sulphite (Mehay,

Z., 23, 26; Hulwa,

Oe., 13

Saillard, S. ind., 42, 82).

465;

37.

Calcium

S. ind., 27, 568).

33.

Add

Melsens. D."

(Leyde. Z.. 1, 365). Hydrate and Alum

Alum

Sulphite with

rere,

36.

Zerban. 15;

Z.. 12, 500).

Calcium

32. Acid

in

Sulphite (StoUe. 1838.

117, 136; 31.

7).

No.

Calcium

Sulphite (Becker, N.Z., 16, 6). Aluminum Sulphite (Stolle, 1838, S. ind., 8, 295;

Iron

Becket

Z., 35, 924). 38.

Sulphite with

Aluminum

Acid

Aluminum

Phosphate

(Schiller,

Z. B.. 12, 509).

Trisuiphite (?) (Labarre. Oe., 18, 36).

30.

Calcium

40.

Basic

41.

Hypoeulphurous

42.

Sodium

43.

Sodium

Sulphite (Berggreen.

Magnesium

Acid

Hyposulphite Hyposulphite

B., 16, 2542).

(Talamo,

N. Z., 29, 211; Baudry, Z., 53, 260). (Thiele, Chi., 20, 404).

with

Lime

and

Aluminum

Acetate

(D. Z., 33

912). 44.

Sodium

with

Phosphoric Acid

Phosphates

or

(Stein

Crosfield, Z., 53, 1384).

and 45.

Hyposulphite

Hyposulphites

of

the

Alkaline

Price, 1849, in Woodcroft, 46.

Hydrosulphurous

47.

Ammonium

48.

Sodium

49.

Calcium

Acid

Earths

and

Magnesia

(Reece

and

106).

(Ranson,

Oe., 26, 737).

Hydrosulphite (Descamps, S. ind., 65, 673). Hydrosulphite (Thiele, Chs., 20, 404; Schiller,Z. B., 22,

683).

Hydrosulphite

with

Barium

Hydrate

(Descamps

S. ind., 65, 673^ 50.

Hydrosulphite

of

Calcium,

Barium

Strontium

or

(Descamps,

S.

ind.. 65, 673).

6},.Magnesium 52. 53. 54.

Hydrosulphite (Becker, Z., 36, 978). Hydrosulphite (Urbain, S. ind., 50, 31). Zinc Hydrosulphite (Urbain, see above). Salt of Zinc Double Hydrosulphite with Sodium Cadmium

Bromide

and

Ammonium

Chloride

or

Fluoride

Chloride

(Harding,

S. ind., 66. 742). 65.

Iron

56.

Aluminum

57.

Hydrosulphite

58.

Hydrosulphurous

or

Manganese

Hydrosulphite (Descamps,

Hydrosulphite of Alumina

Acid

and

(Descamps,

see

S. ind., 65, 673).

above).

(Becker, Z., 36, 978). Phenol

or

(Kowalski, Z., 55, 396).

534

II. 69.

OP

SUBSTANCES.

Acidb,

Coicpoundb

INDEX

Its

Phobprorub;

Sulphide

Phosphorufl

60.

Phosphoric

61.

Sodium

62.

Potassium

63.

Ammonium

64.

Sodium

65.

Calcium

Acid

(Hlavati. Chs.. 27. 254).

Z., 9, 433).

(Stammer,

Phosphate

DBBXTATiyBS

and

(Kuhlmann,

Phosphate

Z., 2, 130).

(Blanchard,

B., 6, 153).

(Kuhlmann,

Phosphate

Amer.

Beanei,

Z., 2, 92;

1862).

patent,

Calcium

(Ozland,

Phosphate

Z., 3, 292).

(Gwynne,

Phosphate

Z,, 2, 130; Ostermann,

S. ind., 40,

698). J56. Barium 67.

Phosphate

Strontium

(Hcffter. Oe., 22, 71).

Phosphate

68.

Magnesium

69.

Phosphate

70.

Acid

71.

Acid

(Heffter,

(Kessler, Z., 15, 525).

Phosphate of Alumina

Ammonium

(Oxland,

Z., 2, 130).

(Packert, S. ind., 25, 25).

Phosphate

Ammonium

''

above).

see

Barium

with

Phosphate

Hydrate

(Chameroy,

S. ind., 51, 173).

72.

Acid

Calcium

(Richter, 1834. Z., 44. 446; Schott, N.

Phosphate

Z.,

14. 314). 73.

Acid

Calcium

74. Acid

with

Phosphate

S. ind., 52, 468). Calcium

Calcium

Bisulphite (Barthel^my,

I Sulphate

Phosphate with,Magnesium

(Kessler, Z., 15,

51). 76. Acid

Barium

76.

Acid

Magnesium

77.

Acid

Phosphate

78.

Calcium

79.

Superphosphate

Phosphate

J. Fabr., 29,

(Manoury,

Phosphate

(Oxland,

of Alumina"

Superphosphate

24).

(Kessler, Z., 15, 51).

(Maguin,

of Alumina

Z., 2, 130).

J. Fabr., 29, 23).

1857, in ling-Roth.,

(Daubeny,

23;

Stubbs, 61. Ass., 9, 912). 80.

Commercial

81.

Tribasic

Superphosphate Caleium

82.

Tribasic

83,.,Tribasic

also with

Phosphate,

S. ind., 25, 25).

Z., 34, 1269).

(Casamajor,

Calcium

Phosphate

with

Calcium

Phosphate

with

Alum

Tpbasic

(Packert,

(Kessler, Z., 15, 51).

Phosphate

Ammonium

Z., 12, 193). 84.

Acid

Sulphurous

-

(Leplay,

^

of Alumina

Phosphate

with

Sulphurous

.Acid

(Paekert,

S. ind., 25, 25). 86.

Manganese

86.

Metaphosphoric

87.

Sodium

88.

Sodium

Phosphate

Acid

(Lefranc, S. ind., 58, 410).

(Bielmann,

S. C,

28, 386;

MoUer,

S. ind..

47, 410). Woodcroft, 89. 90.

Metaphbsphate

Calcium

Young,

1836, in

59).

Calcium

Phosphorous Phosphite of

and

(Gwynne

Pyrophosphate

Acid Alumina

(Gwynne

and

(Hlavati, Chs., 27, 254).' (Spence, Z., 31, 231).

Young,

see

above).

Phosphites and

91.

Aeid

92.

Phospho-9ulphites

535

SUBSTANCES.

OF

INDEX

Sulphites (Kahnel,

Mailctb.,

Prager

1888

168). Grobert, 93.

III.

of the Alkalies

Alkaline

Earths

and

(I^angey

(Hlavati, Chs., 27, 254).

Acid

Hypophosphorous

Thdib

Cabbon,

Silicon,

BoBON,

and

S. ind., 54, 425). -

Compounds

Acids,

'

"'

Db*

and

BIVATIVBS.

94.

Boric

Acid

(Payen,

95.

Boric

Acid

with

96.

Boric

1828, in Weber

Sulphur

Powder

I, 565). and

(Fancher

Clarke, Bl. Aas., 9,

912). Acid

and

Z., 30, 533;

of

Borates

Earths

Alkaline

the

(Oppermann,

Brear, B.. 15, 1224).

97.

Ammonium

98.

Borax

99.

Hydrofluoboric

(Besson, J. Fabr., 43, 1).

Borate

(Brear, B., 15, 1224).

(Hlavati, Z., 52, 758).

Fluoride

100.

Silicon

101.

Siheic

102.

Silicic Acid

(Hlavati, Z., 53, 256).

Acid

(Leuchs III, 86, 1836),

Acid

(Kieaelguhr), (Heddle. and

103.

Kieselguhr

104.

Hydrated

105.

Potassium

106.

Sodium

107.

Polysilicates of Magnesium

Silicic Acid

Silicate

with

(Wagner,

108.

Zinc

109.

Silicate of Alumina,

110.

of Alumina,

Silicate

(Schubarth,

Silicate,also Silicate

Oe., 16. 441).'

(Soxhlet, Z., 43, 972).

Saw-dust

(Hlavati,

Gypsum

(Sohott, D., 251, 91).,

Z., 9. 331). and

Aluminum

(Hlavati, Chs., 28, 1180).

above).

see

e.g..

Z:, 2, 92).

Brick

(Maumen6,

Dust

e.g.. Brick

Dust,

with

textbook).

Caustic

Lime

(Breyea"

Z.. 54, 1271). 111.

HydrofluosiUcio Schoonjans,

112.

Hydrofluosilicate

Ammonium S. C,

(Kessler, Z., 16, 760; Chz., 30, 382). Acid

(IJills,N.

Gin,

Z., 46, 627;

Z., 39, 115;

Whiteman,

1903, 565). Hydrofluosilicate with

113.

Ammonium

114.

HydrofluosilicicAcid

Calcium

with

Lime

(Hlavati, Chz., 28, 1110).

Carbonate

(Marix,

Bl^

1869,

346). 115.

Magnesium

116.

Zinc

117.

Lead

(Kessler, Z., 16, 760). (Rividre, Bi. Aas., 25. 603).

Hydrofluosilicate

Hydrofluosilicate Hydrofluosilicate

(Vivien, Bl. Ass., 8. 24;

Sokol, Ohs.,

21,

R., 68). 118.

Basic

Lead

119.

Aluminum

120.

Iron

Salt

of Hydrofluosilicic Acid

Hydrofluosilicate

Hydrofluosilicate

(Hlavati, Chz., 28, 1180),

(Rividre, J. Fabr.. 49, 18);

(Lefranc, Z.. 41, 498;

Drost

Patent,

54,

372). 121.

\

Hydrofluosilicic Acid

Powdered

Iron

or

Aluminum

(Mertens,

S. ind., 63, 659).

Hydrofluosilicate (Kessler, Z., 16, 760).

122.

Manganese

123.

HydrofluosiHcate of HydrofluosilicicAcid

124.

with

Alumina with

(Kessler, Z., 15, 625). Alumina

(Gin, S. ind., 46, 48).

536

INDEX

125.

Carbomc'Acid

126.

Potaaaium

SUBSTANCES.

OF

(BarrudU,

Carbonate,

Leuolia, 1836, III 86).

1811; Oe., 23, 946; alao

(Freimd,

Earth

Fuller's

with

1827,

Getch., 369). Carbonate

127.

Sodium

128.

Sodium

129.

Ammonium

^eber.

Ill

130.

Acid

131. 'Acid

568).

Potassium

Carbonate

Carbonate

Carbonate

(Perier and

Sodium

Carbonate

with

Acid

133.

Potaaaium

IV.

Htdboobn,

Carbonate

Ammonium

Nascent

(Bismer,

135.

Hydrogen

Peroxide

136.

Hydrogen

Peroxide

(Stein and 137.

and

Hydrogen

139.

Oxygen

140.

Oxonised

Thbib

Acids,

Lead

Zinc,

with

Hydroperoxide

or

Z., 48, 140).

or

Alkaline

Phosphates

Crosfield, Oe., 28, 181). wjth Phosphoric Acid

and

Magnesia

(Pechnik

in Z., 25. 127).

Bdgel

138.

(?),).

1830

NiTBOGBN,

(Frank, Z.. 11, 302). with Phosphoric Acid

Peroxide

Hydrogen

about

Dbbivatives.

and

fromi

(Manoury,

.

Oe., 38, 534).

HALOosNa,

Hydrogen,

Manganese

Z.,

(Salisbury, Z., 64, 849).

(Dubrunfaut,

Percarbonate

Oxtokn,

Possoi, St. J., 1863, 350)

Alum

Compounds 134.

211),

Nind,

I. 566;

1828, in Weber,

(Payed,

Sodium

132.

in Woodcroft,

(Richard, 1856,

Z., 9, 430).

Stammer,

1, 595;

in

(?), OAmandot

about. 1830

(Dubrunfaut,

Peroxide

Black

Bone

and

S.

(Reboux,

Gas

(Ranson,

ind., 36, 150;

Oe.,'26, 737). S.

Wayland,

C.

1893.

611). (Schneller and

Air

Wisse, S. ind., 39, 467).

141.

Air

142.

Osone

Air (Steffens, S. ind., 72, 214). Osonised (Beans, 1866, in Woodcroft, 392; Lee, B., 2, 64).

143.

Osone

with

144.

Osonised

145.

Osone

146.

Osone

and

Chlorine

Soda

and

(Brin, Engl. Patent,

2297).

(?) (Lewicki, Z., 54, 245).

Chlorine ft

^^

with

Sulphurous

Acid

Chloride

of Lime

and

Barium

Hydrate

(Verley, S. ind.,

53, 301). with

and

(Brin, ^ngl.

Alumina

Pate"t,

2297).

147.

Chlorine

148.

St. J., 1882, 274). Siemens, 1859, Z., 44, 458; Duncan, Liquefied Chlorine (Reboux, S. ind., 36, 150).

149.

Chlorine

with

Carbonic

150

Chlorine

with

Acetylene (Carlee,

151.

Chlorine

with

Ethylene

152.

Hydrochloric 761;

Gas

(Strathing and

Acid

Hydrochloric

Acid

with

Hydrochloric

Acid

with

155.

Ammonium

Chloride

Z.. 84. 94; 157.

Sodium

Z., 49, 370;

Z., 1, 258;

(Bismer, Oe., 38, 532). D.

Z., 33. 738). II. 2, 49).

(Kitaee, S. C,

(Margueritte,

153.

Potassium

1820,

S.

ind., 8, 71;

Kessler, Z., 16,

Erk, Z., 26. 288).

154.

156.

Acid

Smit,

Metallic Alum

Powders

(Thide,

(Macfadyen,

(Hlavati, Z., 52, 758).

Chs., 20. 404). 1830,

Gesch.,

Licht, St. J., 24, 415).

Chloride Chloride

(Macfadyen, (Nash,

1830. Gesch.. 423).

1852, in Woodcroft.

151).

423;

Reboux,

537

StmSTANCBS.

OF

mDBX

Acid

(Z., 1. 255;

Acid

Anhydride

Oe., 34. 532).

Bismer,

160.

HypochlorouB Hypochlorous Hypochloritea

161.

Hypochlorites of Alkaline

162.

of Alumina Hypochlorite^

163.

Bromine,

164.

Hydrofluoric Acid

165.

Ammonium

Fluoride

Ammonium

Fluoride

with

Fluoride

(Kessler, S. ind., 1. 363). Abraham,

158. 159.

S. ind., 35, 549".

S. ind., 66, 517;

(Dobler,

Alkalies

of

(Lagarigue,

Hafner,

Oe.,

37, 86).

(Herapath, 1862, in Woodcroft,

Earths

320). (used in England

S. ind.,

(Maumend,

about

1880).

18^, 577). Schoonjans,

Z., 15, 43;

(Frickenhaus,

Chi., 29,

889). 166. 167.

Magnesium

168.

Calcium

(Besson,' Chs., 27, 863, Barts, 125). Aluminum (Voss. Z., 50. 438). C.

(Kessler, S. ind. 1, 363;

Fluoride

Z., 11,

886).

Oxide

Nitrous

169.

(Melsens,

1849,

D.

Z., 25, 1360;

Hlavati, Chs.. 28,

1180). Acid

Nitrous

170.

1849. Nitrites

171.

(Drapies,

in Woodcroft, of

in

and

Alkalies

the

Blachette-Zoega, 1833,

264;

Newton,

111). Alkaline

Earths

(Decastro,

Z., 29,

270). Nitric

173.

Calcium

174.

Potassium

V.

(Kessler, Z., 16, 61).

Acid

172.

Nitrate

(Macfadyen.

Alkalinb

Alkalixs,

Ammonia

(Nash,

176.

Ammonia,

also

177.

Ammonia

175.

Z.. 29, 270).

(Decastro,

Nitrate

1852.

with

with

Eabths, in

Gesch.. 423).

1830;

and

Woodcroft,

Caustic

Lime

Magnesium

or

Thkib

152;

(Marot,

Compounds.

Michaelis. Z., 2, 448). B., 9. 643).

Alulninum

Sulphate

(Hlavati,

S. ind.. 65. 673).

with

178.

Ammonia

179.

Ammonium

180.

Caustic

Oxalic Acid (Hlavati, Z., 56, 300). Sulphide (Bandris, 1853, in Ling-Roth. with

Potash

ash) about

Alkali

Carbonate

in Egypt,

700

Gesch., 134

and

.

181.

Potassium

182.

Sodium

183.

Calcium

184.

Caustic 134

Sulphide

Peroxide Lime

Sulphide and

(Margueritte

acetate

and

or

Sodium

and

107).

(partiallycausticated (Bandris,

Maumen6,

plant *

287). see

179).

Z., 28, 845).

(Hlavati. Chs.. 27, 254). Lime

Hydrated

(in Egypt

about

700, Gesch..

287).

185.

Calcium

Hydrate

with

Soda

186.

Calcium

Hydrate

with

Gypsum

187.

Calcium

Chloride

188.

Chloride

of Lime

(Beuster, J. Fabr.. 32, 2). (Nathusius,

(Balling. 1837. Z.. 44, 452; (Brandes,

1824, Z

,

in Bley. 75).

Michaelis. Z., 2, 65).

44, 447, Z.. 7. 423).

538 of

SUBSTANCES.

OF

INDEX

Lime

180.

Chloride

190.

Calcium

Chloride

191.

Calcium

Carbonate

(Maumen^,

192.

Calcium

Carbonate

with

193.

Calcium

Bicarbonate

194.

Calcium

Nitrate

195.

Calcium

Sulphate

196.

Calcium

197.

Calcined

Sulphate Gypsum

198.

Calcium

Acetate

199.

Calcium

Borate

200.

Calcium

Sulphide

(Drapies

Sulphide

with

with

(Hafner

Acid

Sulphurous

and

Bismer,

Oe., 37, 199).

Woodcroft,

201.

Calcium

Lime

with

J. Fabr.,

Milk

of Lime

Sulphate

(Howard. Leyde,

23;

17, 22).

(Dabrowski,

Gesch.,

Z., 1, 378;

368;

Druke,

Lime

(Kassner.

with

Lime

(Leisy, D.

D.

1816.

in

D., 196, 83).

Duquesne,

with

106).

(Pape, Chi.. 12, 30).

of Alumina

1810,

Z., 50, 615).

in Woodcroft,

an(l Price, 1849,

(Reece

with

(Guignard, Z., 53, 446).

Magnesia

or

Z., 29, 2151).

Z., 33, 919).

(Barth, 1832, Z.. 44, 449;

St. J.. 8, 334)

Durieux,

(Klein, B., 9, 1433). in

BUchette-Zoega, 1833, 264). Magnesium Sulphate (Drummond, D.. 203,

325). 202.

Calcium

Persulphide (Talamo,

203.

Calcium

Sulphuret

204.

Polysulphurets

205.

Calcium

206.

Barium

and

and 207.

Carbide

Oxide

Price, 1849, in Woodcroft,

or

Calcium

Sulphide

with

106). Ammonia

Acid (Hlavati, S. ind., 72, 487). (Rividre, Bl. Ass.. 15, 583).

Hydrate

J. Fabr.. 14, 34;

(Lagrange.

Du

Beaufret

Z., 40, 590).

Manoury.

Barium

(Reece and Calcium

of

Sulphurous

S. iiid.,40, 57).

with

Hydrate

Oxide

Ammonium

Phosphate

(Lagrange.

J. Fabr., 14. 34). 208.

Barium

Oxide

Hydrate

with

Soda

209.

Barium

Oxide

Hydrate

with

Iron

210.

Barium

Peroxide

211.

Barium

Peroxide

212.

Barium

Peroxide

213.

Barium

Chloride

(Licht, B., 15, 1471).

214.

Barium

Chloride

with

215.

Barium

D.

(Beaudet, with

(Oppermann, Vitriol

Z.. 40, 592).

(Curely, S. ind., 43. 361).

Z., 18, 1824). Acid

Phosphoric

(Stein and

Crosfield, Z.,

53, 1334).

Hydrate

Carbonate

Weisberg,

(Ranson,

Caustic

(Seyferth

Soda

S. ind., 47.

(Plique, D.

Z.. 25. 611;

251). Z., 2, 51).

Heffter, Oe.. 22, 71;

S. ind., 64, 429).

^

216.

Barium

217.

Barium

218.

Barium

219.

Barium

Carbonate

with

Sodium

Phosphate

and

Sulphurous

Acid

(Packert. S. ind., 25, 25). Carbonate

with

Sulphate

with

Potassium

of Alumina

(Eisenstuck, St. J.,

3, 244). Carbonate

Permanganate

(Talamo,

N.

Z.,

29, 210).

Sulphate with

Barium

Chloride

and

Lime

(Haesendonck,

S. ind., 43, 598). 220.

Barium

Sulphide

and

106; Weisberg, 221.

Barium

682).

Sulphide

with

Sulphuret (Reece and

Price, 1849. in Woodcroft,

S. ind., 64, 429). Caustic

Soda

-

(Romigui^res, S.. ind., 26b

540

INDEX

VI.

SUBSTANCES.

OF

MSTALS

ThBIB

AND

254.

Aluminum

Dust

(HanBon,

255.

Aluminum

Dust

with

256.

Aluminum

Dust

with

Ammonium

Dust

with

Hydrofluoric

CoMIOUNDS.

Chs., 21, 1033).

Alkalies

(Ranaon,

above).

see

BL

Sulphite (Beason,

Asa., 19,

800). 257.

Aluminum

258.

Alloys, also with

Aluminum

Acid

or

or

Zinc

Hydrofluoailicic Acid

Z.. 54. 118).

(Mertens,

Copper

(Bessen, Chs.,

Dust

28. 529). Chloride

259.

Aluminum

260.

Aluminum

261.

Aluminum

262.

Alumina

263.

Hydrate

264.

Colloidal

265.

Fuller's Earth

266.

Sodium

267.

Aluminate

268.

Calcium

(Nash.

Woodcroft,

in

1852,

Heffter,

151;

Oe.. 22, 71). with

Chloride

Lime

(Siemens. St. J., 18, 256).

(Kessler, Z., 15, 525).

Fluoride

(about 700

in Egypt,

Gesch., 135 and

Murray,

295;

about

1802. Gesch.. 368).

(Howard,

of Alumina

Alumina

Z., 2, 9^.

Gesch., 368;

1810.

(Lowig, Z., 29, 905).

(Fritsche. Z., 35, 361).

Aluminate

also

with

Acid

Sulphurous

Bl.

(Besson,

Ass.,

25, 733). of the

269.

Basic

Calcium

270.

Tetra-

and

Aluminate

of

Strontium

or

with

Barium

Aluminate

273.

Barium

Aluminate

274.

Barium

'

Calcium

of

Barium

or

(Gin

Ass., 16, 707). Bl.

Rembert,

1861;

51. 908,

Aluminate

Barium

272.

(Plicque, Bi Z., 2, 51).

(Gui, Z.. 46, 202).

Hexa-Basic

Aluminate

Earths

(Oxland, Z., 2, 92).

Leleux, Bl.

and 271.

Alkaline

Aluminate

French

Patent,

Ass., 20, 747).

Ammonia

with

(Jacquemart, Alum

(Geistodt, Z., 28, 843).

Acid

Sulphurous

(Jaluaot, S. ind., 63,

690). with

Aluminate

275.

Magnesium

276.

Sulphite

277.

Sulphate

Alumina

of

Aluminum

Sulphate

(used about

Aluminate

1888;

(Jaluxot,

above).

see

Hlavati, S. ind., 65, 674).

(Kessler, Z., 15, 525;

Miv"6,

with

(Stein and

1860,

Z., 44,

458). Alumina

of

Phosphoric

Acid

(I?h"sfield,

Oe., 28. 183). 278.

Basic

Sulphate

of Alumina

(Hunt,

Z., 30, 361;

Branjes,'D. Z., 25,

19). 279.

(about 700

Alum

des

Fabrik. Alum

with

281.

Alum

with

282.

Alum

also with

Aluminum

284.

Tartrate

285.

Oxalate

Zuckers," and

Lime

Gesch., 135;

Alcohol

Sulphate

Acetate

Hermbstaedt.

"Anleit.

a.

Berlin. 1811. 86).

Carbonate

Sodium

280.

283.

in Egypt,

(Salisbury, Z., 54, 1274). (Derosne,

(Oxland,

1850,

Oc.. 23. 048).

(Howard,

of Alumina

*

1812, Z., 44, 446).

in Ling-Roth.,

121 ; Schub"rth,

Z., 2, 92). of Alumina of Alumina

99, 482; 286.

Alminum

287.

Aluminum

Dumas, Phosphate

(Dumas,

C. Z., 1906,

939). (Sievier, 1847, in Woodcroft,

94;

C. Z.. 1906, 939).

(Oxland, Z., 2, 92, and

Silicate (Maumen^,

Lehrbuoh).

2, 130).

Miaihe, D.,

288.

Aluminate

28(i. Iron-

Silicates (Gans,

and

Z., 57, 206).

Quarts-Containing

Clay

290.

Aluminum Ferrous

292.

Iron

Hydroxide,

also

293.

Iron

Sesquioxide

also with

Osone

294.

Iron Sesquioxide

Hydrate

(Wackernie,

Sulphide

Iron Peroxide

296.

Iron

Ochre

297.

Iron

Chloride

Iron

300.

Ferrous

301.

Iron

302.

Ferric

303.

Basic

with

(Reynolds, (Martineau,

Licht, N. 299.

(Hlavati. Chz., 27, 254). (Hills,1850, in Woodcroft, 121).

Oxide

295.

Ferrous

Z., 22, 1104).

D.

(Harm.

291.

298.

541

SUBSTANCES.

OF

INDEX

Gypsum

(Rousseau,

Z., 11, 671). Chx., 19, 1519).

(Wayland,

S. ind., 47, 215).

1859, in Woodcroft, 250). 1815, in Woodcroft, 21).

(Sievier, 1847, in Woodcroft,

94;

Krai, Z., 18, 317;

Z., 11, 63).

Chloride

(Maumen^,

Oxy-chloride Carbonate

1895, 577).

Schachtrupp,

(Junius and (Reynolds,

Sulphate Ferric

and

(Spunt

Fluoride

S. ind"

Gouthi^re,

Z., 30, 216).

Chz., 25, 603).

1859, in Woodcroft,

(Sievier, 1847, in Woodcroft,

Sulphate

N.

250).

94; Krai, Z., 18, 317).

(Mehrle, Z., 32, 385).

304.

Ferrous

305.

Iron

306.

Iron

307.

Iron

Sulphate (Bayvet, Z., 10, 256; Mehrle, Z., 32, 385). with Alkaline Earths (Curely, S. ind., 43. 361). Vitrol with Barium Hydrate (Beaufret, Bl. Ass., 10, 803). Vitrol with (Lohmann, Gypsum 1817, Z., 44. 447).

308.

Iron

Vitrol

with

Zinc

309.

Iron

Vitrol

with

Albuminates

310.

Iron

Nitrate

311.

Salts

of Ferric Acid, so-called

Vitrol

(Schetke, Chz.. 1906. 23).

(Krai, Z.. 18. 317). (Sievier. 1847. in Woodcroft, 94). and

Cyanide

Iron

313.

Potassium

Ferrocyanide

314.

Potassium

Ferrocyanide

315.

Calcium

316.

Chromium

317.

Chromic

Acid

Sulphurous

312.

Archiv., 1903,

"Ferrites"

1892).

Z., 50, 957).

(Sievier, 1847. in Woodcroft. 94). also

with

Sulphurous

Acid

(Boot, Java

1046).

Ferrocyanide (Therry, 1833, Peroxide Acid

(Liesenberg, about

(Thompson,

in

Woodcroft, 54).

(Piettre, Bl. Ass., 19, 1381). Salts of Chromic

and

Acid

(Maumen^,

S. ind., 1895,

57). 318.

Acid

Chromic

Salts

Acid

(Maumen6.

see

above).

(Lefranc. S. ind.. 58, 410).

319.

Chromium

Sulphate

320.

Chromium

Phosphate

321.

Manganese

Dutft

(Spreckels. Chz., 28, 1270). (Eachran,

with

Manganese

Oxide

323.

Manganous

Oxide

324.

Manganese

Dioxide

322.

301;

(Lefranc,

Acids

(about

ind,,51, 103).

D., 251, 91).

Frickenhaus, Z.,

10

Piettre. Bl. Ass., 19, 1351). Chloride

(Manoury,

326.

Manganese

with

327.

Manganese

Carbonate

328.

Manganese

Sulphate

329.

Manganates Woodcroft. Sodium

S.

.

1836. Biey, 47;

Chloride

330.

above)

(Manoury,

Manganese

325.

see

of the

about

Oxalic

1880).

Acid

(Fontenille, S. ind., 54, 425). (Newton, 1859. in Woodcroft, 253). (Mass^. Z.. 10, 256).

Alkalies

and

Alkaline

Earths

(Hawes, 1853, in

163).

Manganate

(Knaggs,

1866, in Woodcroft.

384).

542

of Lime

331.

Manganate

332.

Potassium

333.

Sodium

334.

Calcium

335.

Aluminum

336.

Permanganates

Lefranc, Bl. Asa., 18, 962).

(Z., 1, 256;

Permanganate

(Maumen^,

J. Fabr., 1894, 51).

(Knaggs, 1866,

Permanganate

N.

SUBSTANCES.

OF

INDEX

384).

(Fayolle, S. ind., 52, 554).

Permanganate

(Fayolle,

Permanganate with

in Woodcroft,

Barium

see

above).

Carbonate

and

Oxalic

Acid

(Talamo,

Z., 29, 210).

337.

Copper

338.

Lead

with

Sulphate

339.

Lead

with

340.

Lead

Oxide

341.

Plumbic

Acids

Sulphides

of the

(about

Hydrate Wohl

468; 342.

Litharge

343.

Lead

344.

Plumbites

Lime

with

also

Dust

(Hlavati, Z., 56, 300). Alkalies

(Bandris, Ling-Roth,

107).

1836, Bley, 126). Z., 3, 392;

(Cwynne.

and

ind., 51, 103).

S.

(Manoury,

Z., 55,

KoUrepp,

S. ind., 1892,

Lagrange,

60.

(Pfeifer and

Langen, N. Z., 19, 131). S. ind., 1895, 577; Piettre, Bl. Ass.. 19, (Maumen6,

Peroxide

1351). Alkaline

of the

(Galloway, 1852,

Earths

in

Wcjodcroft,

147). 345.

Lead

(Hills, 1850, in Woodcroft,

Carbonate

121;

Besson,

Cbc., 28.

1270), 346.

Lead

Sulphate

347.

Lead

Nitrate

348.

Lead

Nitrate

349.

Basic

Lead

350.

Lead

Acetate

351.

Lead

Subacetate

352.

Load

(Scoflfern,1850, with

Woodcroft,

of Alumina

Sulphate

and

(Wohl

Nitrate

in

(Pape, Chz., 12, 30).

KoUrepp,

Z.. 55, 60).

(Scoffern, 1847, in Zerban, also with

Subacetate

115).

S. ind., 1892, 468).

(Lagrange,

Sodium

15;

Gwynne,

Z., 3, 392).

Sulphide (Maumen").

with

Chalk

with

Sulphurous

(Pajot

de

Charmes,

1321,

Gesch..

369). 353.

Lead

Subacetate

Ling-Roth, 354.

Lead

355.

Lead

81

and

and

(Gwynne,

Saccharate

(Scoffern, D.,

117,

in Woodcroft,

59).

265;

82).

(?) (Gwynne

Triacetate

Acid

1850,

Young, in

Woodcroft,

116;

Wohl

and

Z., 54, 854).

KoUrepp.

and

(Gwynne

Albuminate

356.

Lead

357.

Zinc

Dust

with

Mineral

358.

Zinc

Dust

with

Sulphuric Acid

359.

Zinc

Acids

Young,

(Manoury, and

1836, in Woodcroft,

S. ind.

Barium

59).

51, 103).

Sulphide

(Cripo,

St. J.,

24,416). Dust

with

Sulphurous

Acid, also with

Ferrocyanidefl

(Boot,

Oe.. 27, 717). 360.

Zinc

Dust

with

361.

Zinc

Dust

with

Tartaric

362.

Zinc

Dust

with

Alkalies

363.

Zinc

Dust

with

Dolomite

364.

Zinc

Dust

Hydro^uoric Acid

Acid

(Mertens,

"Koper8ki,

Z., 54, 118).

Z., 54, 1271).

(Ranson,

365.

Coppered

Chi., 21, 1033). (Hlavati, Bl. Ass., 16, 759). with Ammonium Sulphide (BrQnn, Chi., 31, R., 459). Zinc-Powder (Verley, Chz., 24, 596).

366.

Zinc

Iron

Alloys (Mertens,

367.

Zinc

Chloride

(Gauchy,

368.

Zinc

Fluoride

(Hlavati, Z.. 5^9*258).

Z.,.454,118). N. Z., 13, 43; Heffter, Oe^, 22, 71).

INDEX

"69.

Zinc

Oxide

OF

543

SUBSTANCES.

1836" Bley. 126).

(d^out

(Wilson, 1815.

370.

Zinc

Hydrstei

3?1.

Zinc

Hydrocarbonate

372.

Zinc

373.

Zinc

Gesoh., 368).

(Perrin, Chs., 22, 54; Mittelstaedt, D. Z., 23,

1112). with

Hydrocarbohate

Oxalic

Acid

(Moureaux,

BI.

Ass., 19,

1483).

Sulphate (Wilaon, 1818,

Bt"dt, in Weber, 374.

Zinc

with

Sulphate

in

Woodcroft, 27; Z., 44,447; Hermb-

1829, 100). Hydrate

Barium

(Wackemie,

S. ind., 53. 201

61, 718). 375.

Zinc

Nitrate

(Decastro,

St. J., 19, 340).

376.

Zin^ Nitrate

with

Alkali Sulphide

377.

Zinc

with

Calcium

Nitrate No.

see

(Decastro,

Sulphide

No.

see

Barium

or

375).

Sulphide

(Decostro*

375). (Hlavati, S. ind.. 65, 674).

Aluminate

378.

Zinc

379.

Cadmium

Oxide

380.

Cadmium

Carbonate

381.

Tin

382.

Stannic

Oxide,

383.

Stannic

Hydrate

384.

SUnnic

Bl. Ass., 19, 1483).

(Mouraux,

(Mouraux,

No.

see

379).

(Besson, Cha., 27, 863).

Dust

also

with

Soda

(B., 19, R., 520).

(Wilson, 1815, Gesch., 368). (Nash,

Chloride

in

1852,

Woodcroft,

Maumen6,

151;

J. Fabr., 20, 7). 385.

(Nash,

Chloride

Stannous

Zerban,

Manoury,

77;

1852,

No.

see

Z., 34, 1275;

384;

Havemeyer,

Maumen6;

S.

1869, in

ind., 1895,

577). with

Stannous

Chloride

387.

Stannous

Nitrochloride

388.

Stannous

Fluoride

389.

Stannic

390.

Stannous

391.

Tin

Nitrate

392.

Tin

Chloronitrate

393.

Stannic

394.

Stannates

395.

Stannates

386.

396.

(Ranson, (Anderson,

Sulphate

(Reynolds,

384).

1859, in Woodcroft,

(Reynolds,

1859.

of the

Alkalies

(Reynolds,

of the

Alkaline the

of No.

No.

1856, in Woodcroft,

Acid

or

see

Chz., 24, 1026).

Metastannic

Acid

see

1852,

218).

(Oe., 15, 76).

Sulphate

Metastannates

1859.

(Nash,

(Thiele, Chs., 20, 404).

Acid

Sulphuric

Earths Alkalies

250).

No.

see

^91).

(Reynolds, 1859,

sae

(Reynolds. and

1859, No.

1859,

Alkaline

see

No.

see

Earths

No.

Metastannate

(Rejmolds.

1859,

Alumintfm

398.

Mercury

399.

Mercuric

Nitrate

400.

Antimony

Dust

401.

Antimony

Tin

402.

Antimony

Peroxide

403.

Antimony

Sulphide (about li;70, CSesch., 31 1).

Peroxide

see

No.

(Piettre. Bl. Ass., 19, 1351). (S. C,

II. 4, 216.)

(Besson, Chs.. 27, 863). Alloy (Mertens, (Piettre, see

S. tnd., 63, 669). No.

398).

391).

(Reynolds,

391).

397.

391).

391).

391).

544 404.

Bismuth

Nitrate

405.

Bismuth

Salts

406.

Aii^.oniumMolybdate

407.

Salts

408.

Titanic

409.

Ferrititanite

410.

Thorium-

and

VII.

ObQANIC

SuB0TANCEa*AND

(Sievier. 1847, in Woodcroft.

Acid

1853, in Woodcroft,

(Hawes,

Tungstio

of

SUBSTANCES.

OF

INDEX

D.

(Wichardt,

Acid

(Reynolds,

(Liesenberg, about

103).

Z.. 31, 652).

in Woodcroft,

1859.

in England

(Employed

94).

about

259). }

1880).

1892).

Monasite-Earths

C.

(Browne,

COMPOUNDS;

Z.. 1904, 568)/^

BlACK

BONK

It8

AND

Substitutes. 411.

Extract

412.

Tannins

of

Gall-Apples (about

and

Tanning

III. 86;

1836; 413.

Quebracho,

414.

Tannic

Acid

Liquors and

(Wagner,

Gesch., 135).

in Egypt,

(Dorion,

1816, Z., 49, 578;

(Hlavati, Chs., 27, 254).

Sumach

Z., 9, 331;

1863, Z., 44. 459).

Walkhoff,

AVsid (?) (Elias, S. ind., 1895,

415.

Liquid

Tannic

416.

Tannate

of

417.

Tannic

418.

Tannic

419.

Tannic

Acid

wjith Alumina

420.

Tannic

Acid

with

421.

Tannic

Potassium

Leuchs,

Chs., 29, 1091).

Luther,

Valonea,

700

or

20).

| croft, 1853, in Wood-

(Galloway,

Ammonium

171). Aoid

with

Lime

Aeid

with

Salts

Heffter, Ge., 16,

(about 1836, Bley, 126;

442). of Barium

or

(Heffter,

Strontium

No.

see

417).

fluosilicic Aeid Acid

see

No.

417).

Acid, and

Metaphosphoric

Acid.

Hydro-

(Royers, S. ind., 50, 32).

with

Glue, Starch

422.

Pertannic

423.

Gallic Acid

(Royers,

424.

Gallate

Potassium

425.

Acetic

No.

see or

(Heffter,

Albumen

or

(7) (Meritens,

Acid

of

(Heffter,

Tartaric

see

No.

417).

Z., 28. 800).

Chs., 26, 972).

Kowalski,

420;

(Galloway,

Ammonium

1853,

No.

see

416). Acid

with

also

Sulphurous

S. ind., 51, 114).

Wernekinck,

Acid For

Stutser

(Z., 20, 741; look

acetates

under

and

the

list

metals. 426.

Wood

Vinegar

427.

Butyric

428.

Fatty

(Leidenfrost, Z., 20, 746). Acid

Sulphonic

Acids

with

(7) (Spreckels, Chs., 28, 1270).

Sulphurous

or

Acid

Sulphuric

(Spreckels,Z.

(Z.. 2, 91;

429.

Stearic Acid

430.

Ammonium

Stearate

431.

Stearic Acid

with

Wagner,

Z., 9, 331).

(Besson. Chs., 27, 863).

Sulphites of

the

Alkalies

or

Magnesium

Z., 57, 268). 433.

Stearic-Sulphonic Acid (Spreckels, see Palmitic-Sulphonic Acid (Spreckels. see

434.

Margaric

432.

ang.,

Chs., 28. 1072).

1902, 891;

Acid

No. No.

(Pidding, 1853. in Woodcroft

427). 427). 162).

(Stewart.

INDEX

435.

Oleic

436.

Oleic-Sulphonic

437.

Oxalic

Acid

(Pidding,

Acid

see

Acid

OF

SUBSTANCES.

No.

434;

(Spreckels,

Z., 8, 130),

Th^nard, No.

see

1836, III. 86;

(Lcuchs,

545

^

427).

l^isafeldt,

Z.. 9, 331;

Wagner,

Z., 21, 1102). 438.

Oxalic

439.

Ammonium

Acid

Magnesium

Ammonia,

with

Zinc

and

(Besson, Bl. Ass.,

18. 616). Oxalate

Woodcroft,

in

(Sievier, 1847,

Besson,

94;

J. Fabr., 43, 1). 440.

Oxalic

with

Acid

Carbonate

Barium

and

(Talamo,

Permanganates

Iff.Z., 29, 210.) 441.

Tartaric

(Possoz, Z., 23, 27; Stutzcr

Acid

and

S. ind.,

Wemekinck,

51, 114). 442.

Ammonium

443.

Malic

444.

Citric Acid

445.

Citric Acid, also with

Polysilicates (HIavati, Chs., 28, 1180).

446.

Salicilic Acid

Z.. 25, 640;

(Besson, Chs., 27, 863).

Tartrate

Acid

with

Metallic

Bases

or

Metallic

Bases

or

Carbonates

Bl. Ass.,

(Moureaux,

19, 1483). with

Carbonates

Bl. Ass.,

(Moureaux,

19, 1483).

417.

Resin

448.

Pimaric

449.

Pectic

450.

Formaldehyde

Acids

(Leuchs,

Acid

III. 86).

1836;

(Acar in Wagner's

12th

Technologic,

(Boulet. Chs., 20, 12;

Ed., 563).

Friedrich, Chs.,

27, 1183;

Bl. Ass., 25, 531).

Acetaldehyde

(Newton,

Z., 25, 1306;

D.

Z.. 9. 7).

D.

(Schiller,Z. B., 12, 33).

Acid

Simpson, 451.

(Hulwa,

1849, in Woodcroft,

111;

Melsens,

1849,

Boulet, Chs., 20, 12).

452.

Methylalcohol (Trobach,

453.

Alcohol

D. Z., 11, 1302). (Jennings, 1825, in Woodcroft, 33; Pesier, Z., 11, 522).

454.

Alcohol

with

Chlorine

455.

Alcohol

with

Acetic

456.

Alcohol

Gas Acid

with Hydrochloric (Ure, 1830, in Woodcroft,

457.

Alcohol

with

Sulphuric

458.

Alcohol

with

Sulphurous

459.

Alcohol

with

Alum

460.

Alcohol

with

Magnesium

461.

Rum

Gin

462.

Glycerine

463.

Glucose

464.

Saccharites. of

or

Z.. 14, 641;

Nitric

Acid,

Acid

or

19, 376).

Sulphuric Acid,

49).

Acid

and

Acid

and

St. J., 22, 274).

(Duncan,

(Paulet, 1837;

Gypsum

(Duquesne,

D., 196, 83).

(Stolle. D., 114, 305).

Lime

(Derosne,

1810, Oe., 23, 948).

Sulphite (Degencr,

(Stokes, in Weber,

Chz., 12, 174).

III. 236).

(Rabe, Z., 14. 124).

and

its Salts (7) (Bielmann,

Lead

of

or

1849, in Woodcroft,

106;

the

S. C,

Alkaline

Gwynne.

28, 386).

Earths

(Reese

Z., 3, 392;

and

Stammer,

Pric6. Z., 12,

336). 465.

Magnesium

Saccharate

466.

Starch

Caustic

467.

Hydrocarbons

and

468.

Kerosene

with

Ahimina

Oil

469.

Kerosene

470.

Tar

471.

Benzol

with

Acid

Petroleum and

Toluol,

(Kowalski.

1849, also

Z., 4, 31). 1848, in Woodcroft,

(Steinkamp,

(Spreckels and

Oils (Newton, or

(Galloway, Lime

Metallic

Kern,

Powder

Sulphurous

Z., 52, 909).

(Z., 53, 444).

Z., 53, 878).

in Woodcroft,

with

102).

(Carbonelle, S. ind., 33, 455).

111). Acid

or

Hydrosulphurou"

546

INDEX

SUBSTANCES.

or

Z., 21, 313;

Phenol

(Fishman.

473.

Phenol

with

474.

Plllnol with

475.

478.

Oxybenxol (Kowalski, see No. 471). also with Sulphurous Acid oi Ozynaphthalin and Oxyanthracene. Acid No. see (Kowalski, 471). Hydrosulphurous (Kowalski, see No. 473). Oxyanthraquinone with Fats Sulphurous or Sulphuric Acid (Spreckels, Z. ang., 1902,

479.

Tallow

472.

476.

477.

483.

Kern.

Bl. Ass., 10. 165).

Fatty

with

Sulphuric

or

(Spreckels

Acid

53. 878).

(Bouvier, Z. B., 1896,

Oils

Mineral

and

Oils

Sulphurous

Sulphuric Acid

or

386).

(Spreckels,

Z.

ang.,

891). with Soda

Oils

Fat

Neutral

and

Wax

Z., 55, 396).

(Kowalski,

(Menier,

Sulphurous

Z.. 55. 571;

Oils

Fatty

of Lime

with

Fatty

1902, 482.

or

Chloride

Lard

or

and

481.

Z., 9. 7).

D.

Petroleum

Chi., 28, 1072).

891;

480.

Benzol

484.

Spermaceti

485.

Stearine

232).

III. 86).

(Leucbs,

Oil

Spermaceti

and

1857, in Woodcroft.

(Brooman,

(Pidding,

1853,

in

Woodcroft,

162). (Carlee. D.

Palmatine

and

Sulphurous

Oil with

Sulphuric

486.

Fish

487.

Z. ang., 1902. 891). Oil with Sulphuric Acid Linseed

488.

Castor

or

Sulphuric Acid

Oil with

Z., 33, 738). Acid

(Spreckels, Z., 55, 571;

(Spreckels and

Kern,

Z., 53, 878).

(Spreckels. Z., 55, 571).

(Basset, Z.. 7. 381).

489.

Soap

490.

Ammonia

491.

Turpentine

492.

Turpentine and

493.

Tar

494.

Tar

Oil

495.

Tar

Oil also

Z., 8, 449;

(Brooman,

Soaps

(Newton,

Besson, J. Fabr., 43, 1).

1849. in Woodcroft,

111;

Carlee,

D.

Z., 33,

738).

.

Sulphuric

(Spreckels and

Acid

Kern,

Z., 53, 878;

55. 571).

Sulphurous

with

(Spreckels, Z.

Sulphuric Acid

or

ang.,

1902.

891).

496.

(Pidding, 1863,

1902.

Alumina

162).

and

Metallic

or

Sulphuric

Sulphurous

with

Oils

Tar

with

in Woodcroft,

Powders Acid

891).

497.

Resin

498.

Resin

162). (Pidding. 1853. in Woodcroft. Acid (Spreckels and Kern, and Sulphuric

499.

Pitch

(Pidding. 1853,

500.

Creosote

501.

Shellac

(Z., 53, 444). (Spreckels, Z. ang.r

(Newton,

see

No.

Z., 63, 878).

497).

1849, in Woodcroft,

111).

(Grieger, S. ind., 54, 23). Bisulphide (Ckiandi. S. ind., 25, 268).

502.

Carbon

603.

Mustard

604.

Radish

505.

Sulphur-Containing Ethereal

606.

Ethereal

(Leuchs, 1836, III, 86; Newton,

OU

1842, in Woodcroft,

111). OH

(Newton,

No.

see

Sulphurous Chi., 28, 1072).

Oils with

1902, 891;

1842,

Oils or

503).

(Spreckels. Chi., 29, 4307). Sulphuric Acid (Spreckels, Z. ang.,

548

INDEX

660.

Otteine

661.

Ferrocyanide

(Bninon

1817, in 652.

SUBSTANCES.

OF

and

Z., 54. 848).

Roth^;

'

Residues

Coal-setUiogs)

(So-Called

Woodcroft. 26; Gawalowski.

of Powder-Settlings

Stearin

(Cavaillon,

Oe.. 18, 718). and

(Lach

Factories

Benies, S. ind.,

1895, 20). 653.

Graphite with Bone

Black

and

Zinc

(Macherski and

Bloom

Eoper-

ski, Z., 57, 1121). 654.

Graphite with

Sand

Zinc

and

(Macherski

Powder

and

Eoperaki,

Z., 57, 1044). 566.

Anthracite

666.

Coal-Tar

667.

Carbonised

668.

Gravel

559.

Bauxite

560.

Calcined

561.

Cement

562.

Brick-Dust

563.

Pumice

564.

Talc

(Hlavati, Z., 66. 300). with

Lime

Scums

'

S. ind., 9, 56).

(Lemaire,

(Karlik, Oe., 32. 256).

(Bergmann,

Meyer. 1879. Z., 30, 1149).

1840, Z., 29. 1184;

(HlavaU.

Z.. 56, 300). Phosphate-Slag (Lachaux, S. ind.. 50. 677). D. Z.. 25, 1946).

(Harm, with

(Breyef. S. ind..65, 655).

Lime

1835. in WoodcroH, 66). (Hlavati. Chs., 28. 1180).

(Saunders,

Stone

Meerschaum

or

(HUvati, Chs., 28, 1180). Zeolite (Riedel, S. ind.. 70, 230).

565.

Mica

566.

Natural

567.

Permutite^

668.

Soil from

the Beet

569.

Hydrogen Osone

see

No.

(Kohlrausch.

Store-house

VIII.

570.

(Riedel,

Artificial Zeolite

566).

Z., 28, 216).

Substancbs.

Elbctbolttic

(Kugler, Chz.. 32; R., 454). Chs., 24, 825).

(Schollmeyer,

Iodine. Fluorine

(Spillem-Spitxer. Z.. 53, 244).

571.

Chlorine, Bromine,

572.

Sulphurous

573.

675.

Acid or Sulphites with Lead, Zinc, Aluminum, Z., 50, 625). (Baudry and Charitonenko, Hydrosulphurous Acid (Ranson, Oe., 26, 737). Coal (Despeissis,Battut, Z., 46, 624).

576.

Wood

577.

Alkaline

Earths

578.

Calcium

Carbonate

579.

Barium

Salts (Bonillaut. S. ind., 50, 189).

580.

Barium

Aluminate

(Lallement,

S. ind., 53, 301).

Tin

(Hlavati, Z., 53, 258).

Charcoal

(Gin and

Leleux, Z., 53, 627).

(Schwerin,

D.

Magnesium

(Urbain, Bl. Ass., 16, 719).

Magnalium

(Murphy,

583.

Magnesium

Hydroxide

(Schwerin,

584.

Magnesium

Carbonate

(Schwerin,

585.

Zinc Zinc

587.

Basic

J. Fabr., 44, 18).

Chz.. 28. 626). D.

(Schollmeyer, Z., 46, 624). Antimony or Alloy with Calcium Zinc

588.

Cadmium

589.

Lead

Salts

(Wohl

and

KoUrepp,

Z., 29, 451).

(Hlavati, Z., 53, 258). D.

Z., 27. 1280).

(Urbain, Bl. Ass., 16, 719).

(Javaux, Gallois, Dupont,

Lead-Antimonj* Nodon.

i

Bl. Ass., 20, 966).

(Rembcrt,

581.

586.

*

Z., 29, 451).

582.

590.

Iron,

Sulphurous or

574.

Acid

D.

Alloy

also

Z., 27. 1211).

with

Z., 46, 626). Manganese

Sulphaite(Piettre and

591.

Leftd

Ondefl

592.

Lead

Peroxide

593.'Xead

(Z., 46. 626).

Basic

595.

Aluminum

Lead

and

(Piettre

Saccharate

594.

549

SUBSTANCES.

OF

INDEX

Salts

BI.

Nodon,

(Wohl

and

KoUrepp,

(Wohl

and

Kollreppt

19, 1351).

Ass.,

D.

Z.. 27. No.

see

1280).

593).

(Z.. 46. 626).

596.

Aluminum-Masneaium

597.

Aluminum

Z., 53,

598.

Alumina

599.

Iron

600.

Iron

601.

Manganese-Silieon

602.

Manganese

Dioxide

603.

Hydrated

Manganese

Zino

with

Manganate

(Delavierre,

Z.

(Browne,

174).

1908,

ang.,

Hydroxide

Iron

or

Hydroxide

1106).

(Z., 46, 626).

(Jennings,

Clement.

1846,

in

1848.

Woodcroft,

89

and

Bl.

Ass.,

103;

Z.. 46, 625).

Maigrot,

Bisulphide

Chi..

(Aschermann,

(Hlavati.

Alloy

26; 683).

Z.. 53, 258.) '

Z., 53, 626).

(Hlavati, Peroxide

and

(Piettre

Nodon.

19,

1351). 604.

of

Manganates

Chromium

Alkalies

Peroxide

Nickel

607.

Nickel

608.

Copper

609.

Iron

Oe., 28,

(G5ri,

Bl.

(Horsin-D^on,

Ass.,

and

611.

Antimony

Peroxide

612.

Mercury

(Polaciek.

Bl.

613.

Mercury

Amalgams

(Polaosek*

6|4.

Mercury

Peroxide

615.

Easily-Fluid

616.

Silver

(Hor8tn-D6on,

617.

Silver

with

Platinum

No.

see

603).

162).

Sulphites

or

Nodon.

(Piettre

619.

and

(Bfiudry

and

Chari-

16, 729).

Antimony

Platinum

(LavoUay

Z.. 46. 624).

610.

618.

Earths

Z., 50, 625).

tonenko,

nenko.

Nodon,

Acid

Sulphurous

with

Alkaline

and

(Piettre

(Horsin-D6on,

606.

and

Z., 25, 330)"

D.

Bourgoin, "605.

the

(Piettre

and

Ass.,

(PieUre

Oe.,

No.

see

Ass.,

19. 1351). Z.. 54. 1030).

612). Bl.

Nodon. (Palms,

1211). Bl.

Gurwitsch.

16, 720;

Bl.

Ass..

Ass..

19. 1351).

17. 274).

28, 162).

Acid

Sulphurous

Nodon.

and

Alloys

Mercury

Z., 27,

D.

Sulphites

or

(Baudry

and

Charito-

Z., 50, 625).

(Collette, Z.. 46, 623;

Thomas

and

Howe,

S.

ind.. 66,

624).

and

620.

Alloy

Antimony D.

Nodon,

Platinised

Z.. 27,

Copper

Additions

621.

622.

Sebonaft Straw-Meal

-"Solid

(Lense.

also

with

S.

Pboov

dubimq

D.

Sulphate

(Piettre

1211).

(Charitonenko,

Mineral

Manganese

Oil"

ind., 53. 272).

Cobrbctionb.

(Nowakowski,

Z., 33, 937).

C.

Z.. 17, 277),

B5Q

ABBREVIAVIONS

OF

REFEaENCES.

ABBREVUTIONS

OF

REFERENCES.

Reference. CUaaaen-Barti's

Bftrii

^'Zuokerfabrikation**

(Leipsig,

1905). B

Beriehta

der

deutacben

ohenuBchem

Geaellichftft

(R"R"ferat6). Bl.

Bulleuin

BUneh"tte

''Manuel

ZoefE

de

(Paria, Bley's

Bley

Sooi6t6

U

da

ehimique.

fabrieant

du

et

raffinear

de

sucre'*

1833).

"Zuckerbereitung

RunkelrOben"

aua

(Halle,

1836). Bl.

Bulletin

Asi.

de

raMoeiation

Chf.

Che'miker-Zeitung

C.

r.

Comptee

C.

Z.

Centralblatt

fdr

die

Zuckerindustrie. Journal.

Zuckerinduatrie. "Gesohiohte

lippmann'a

Gesch.

(ReReperiorium).

polsrtechniaches

Deutsche

Die

Z.

D.

cbimistes.

rendus

Dingler'a

D.

des

dM

Zuckera"

(Leipaig,

1890). des

J. fabr.

Journal

Ling-Roth

Ling-Roth's

f abricanta

"Guide

"Traits

de

f dr

und

Ansichten*'

la

fabrication

d"

sucre*'

Rabensuckerindustrie.

Oesterreichisch-Ungarische

Oe.

Sugar"

1878).

Zeitschrift

Neue

Z.

of

1871).

Maumen6's

(Paris. N.

Literature

Erfihdungen

10,000

(NQmberg, Maumen6

the

1890). "

Leuchs

tu""e.

"^

(London, Leucha

de to

Zeitschrift

fQr

Zucker-

industrie.

Prager

Marktb.

Marktberieht.

Prager The

S. ind.

La

St. J.

Stammer's

Weber

Weber's

Wooderoft

Woodcroft's

sucrerie

indigene "

et

coloniale. der

Jahresbericht

"Zeitblatt

to

Z.

Cane.

Sugar

S.C.

fQr

Gewerbetreibende." of

"Abridgments (London,

Sugar"

SSeitschrift

des

Zuckerfabrikation.*'

Specifioations

ing relat-

1871). der

Vereins

Deutaohen

Zueker-

industrie.

Z. ang.

Zeitschrift

f ilr

angewandte

Z.B.

Zeitschrift

fdr

Zuckerindustrie

Zerbaa

Zerban's

Rouge,

"Louisiana

1908).

Chemie.

Bulletin

in

Bdhmen. No.

103

(Baton

INDEX.

A. "

Bach's

refraetomeier, 226.

Abbe

fermentation,

Acetio

of molaases,

fiber determination,

products,

Acids Acid

thin-Juice

cane

fuel value, 34.

138.

HarlofF,

process,

6.

Anthocyanin, Alcoholic Aoohol

fermentation, of

in

409.

products, 139.

cane

cream,

Alundum Ammoniacal

Bateile's

holders, 238. 141.

187.

methods,

based

Ash, calculations

upon,

normal,

error

Available

sugar,

weight

a

cane

199.

Char),

113.

purchase,

131.

power,

per

for cubic

analysis, 127. foot, 131.

and Books records, 337. Briz, degree, 191.

by

383.

Averaging,

305. of

"e"

109.

preparation

182.

basis

(aho

in analysis, 183.

paste,

acid, 182.

Aspartic

grain, 86, 119.

efficiency number^,

decolorising

254.

Asparagin, 5,

to

sugar

in analysis, 183.

254.

sulphated,

alarm, 296.

Bone-black

270.

277.

in sugars,

sugar

308.

270.

in massecuites,

294.

feed-water,

Boiling

254.

in molasses,

Boiler

Boiling-house

coefficient, 304. determination,

tube, 159.

analysis, 294. 348.

254.

carbonated,

39.

process,

observation

Blaclc-paste, analysis, 127.

79.

Analysis, optical methods, chemical

Bates'

Briz.

"ee

sirup, 120, 122.

Barrel

in limestone, 388.

gases,

288... 291.

171.

Balances, Balling,

crucible

282.

filters,63. 111.

414.

"determination

method,

Norris'

Bag

of molasses, 270.

samples,

determination,

sucrose

Alkalinity of massecuites, 270. Alumina

of

201.

sampling,

66. clarification,

284.

determination,

preparation

nitrogen, 250.

process

Alcohols

as

furnaces, 33. moisture

55.

Albuminoid

292.

filters,65.*

270.

in

283.

choppers,

270.

of maasecuites,

31, 302.

analysis, 282.

409.

Juice, 257.

of the

Acidity

40.

sulphitation prooen,

Bagasse,

juice, 301.

Absolute

"

dilution

and

spindling,

260, 262. 551

552

INDEX.

Brix. by spindlins* 193. hydrometer,

Brix-Dupont

Cellulan, 138.

102.

of milling and

By-products

430.

Cattle-food, analysis, 208.

101.

hydrometer,

Brix- Vivien

CBleuIation of volume^

Cask,

sion, diffu-

Centrifugals, 00. capacity, 100.

31.

dischargers, 100.

self-discharging,100.

C.

66.

separators,

Filter-press cake.

Cachaia,

"ee

Calcium,

carbonate

determination,

sulphide Calumet

Cane,

Char,

in limestone, 389.

sulphate in char, 128. in ohar,

sampler,

202.

influence

Charcoal,

cutting,

of sucrose,

of structure

control

6.

in milling,

matter,

purchase

7.

analysis,382.

or

National,

6.

Circle,

etc., 420.

of

Colloidal

water,

chemical

Cone,

double, 54.

area,

Copper,

50.

301.

estimation

Corallin Coral

53.

acid, determination

in

Wedderbum's

""foduction

240.

solution, 413. 73.

sand, composition,

Cross's

sucrose

method,

235.

Crystallisation in motion,

limestone, 391. acid, production carbonation,. 61.

434.

lime, 73.

tanks, 51, 60.

for

of

etc., 430.

method,

single, 50. Haan's,

quantity,

and

physical properties, 458.

268, 260.

formulae, 443.

Condenser-water,

Carbohydrates,

268:

solution, 413.

Concentration

140.

102.

sugars,

(Hersfeld), 266.

(Steuerwald),

fuel value, 35.

Carbonation,

raw

heating surfaces, 46.

Cochineal

inferential, 314.

tanks, 30. 47.

sugars,

method

4.

303.

in open

Clerget's constant,

weights, 313.

Carbonic

area,

of white

unloaders, 9.

Cane-trash,

defecation, 75.

Chlorophyll,

Cleaning

2.

in, 7.

transport,

Carbonic

for the

Classification

10.

content,

work,

310.

Clarification

Fiske's

analysis,

sugai^house

Circulating water,

200.

seedlings, 1. shredder,

of

Chitine, 138.

2.

on

sampling,

de

of

Chemicals

propagation,

113.

methods

187.

2.

23. mineral

for analysis, 127.

animal,

Chemical

after

distribution

115.

of efficiency, 130.

test

id.

11.

deterioration

alteration, 116. 114.

112,

preparation

5.

Krajewski,

solutions,

revivification, 115.

crusher, Fulton,

process,

and

washing,

composition,

sugar

covering, 113.

indirect, 216.

Caramel,

on

118.

filtrat on,

128.

analysis, direct, 214.

sugars

action

composition

1.

sucrose

circulators, 78.

Chapman's

in char, 130.

laboratory

04.

control, 06, 325.

in refining, 118.

553

INDEX.

CrystollitatioBof wiign, 85.

Excelsior

Crystalliser, 96.

Extraction

capacity, calculation. 345.

322.

F.

411.

paper,

Curing

by mills, calculations,

95.

masseouites, Curcuma

filters,64.

99.

sugar,

and

Cylinder, volume

area,

Feed-water,

430.

analysis, 294.

automatic

Tehling's

solution, 415.

Ferment, Deming's

Defecation,

process,

46.

tanks, 39, 43.

in open

Fiber,

Deming's

of

process

116.

defecation,

determination,

determination, 217. crude, in cattle-food,299.

Filter-press,66. washing,

137.

of

influence

on

exhausted,

206.

Worthington,

Filters, various

Flasks, cdso analysis, 294.

water,

Flue

Dupont Dry Dutch

412.

standards,

103, 278.

Sugar"fiasks,167.

83.

dry milling, 341. commercial

Formulas,

and

Ellipse,

area,

308.

glucose

Evaporation

for

303, 312.

Freeiing '*

Fuel,

juice heating,350.

juice,77.

mixtures, 470. fermentation,"

32.

vidue

of the

of bagasse, 34.

of cane-trash, 35. of molasses,

35.

calculation, 342. Evaporator,

a.

77.

cleaning, 81. tubes,

corrosion, 07.

calculations,

340.

Froth

429.

and

evaporation,

sugar-house

241.

Esters, 139.

Evaporating

342.

dihition, 340, 841, 448. in

42, 45, 46.

Entrainment,

sugar,

342, 443.

methods

determinations, Eliminator,

analysis, 395.

and

concentration

Electrolytic

65.

analysis, 294.

Formula,

E.

EflBciency number,

53.

types,

"ee

Folmaldehyde,

milling, calculations, 323. color

gases,

Foam,

341, 443.

paper,

67.

393.

sampling

Dilution, 305. formule,

67.

Filtration, 63.

25.

process,

68.

in carbonation,

(cachaaa), 70.

scums

juice, sampling,

68.

double, Filter-pressing,

201.

sampling,

disposal of

KeUy,

Sweetland.

chips, analysis, 282.

Diffusion

waste

subaeetate

lead 181.

rotation,

67.

juice, reclarification,70.

135.

Dextrose,

302.

cake, analysis, 280.

juice, 221. Deztran,

determination,

filters,65.

191.

spindling,260.

and

by dilution

bagasse,

cane,

45.

Denmty,

409.

292.

Weinrioh,

Desarboniser,

409.

Fermentation,

in refining, 109.

alarm, 296.

sugar

Glucose,

136.

in cattle

food, 300.

98.

554

IN]""X"

Invert

304. Glucose, coefficient,

electroljrticmethods

lead

of

sugar,

of analysis,

rotation, 181.

on

Meissl-Wein's

241.

methods,

gravimetric

Meissl-Hiller's methods

235.

table, 189.

preparation,^415 245.

calculation.

Meissl-Hiller

using

subaoetate

lodate Iron

determination, 129. limestone, determination

in

factors, 236. tions. solu-

precipitation in clarifying

413.

paper,

in char,

sulphide

181. 253.

,

388.eolorknetrio

method,

277.

ratio, 304. method,

volumetric

Sideraky's 251.

J.

Soldalni's

method,

solution, Soxhlet's

247.

416.

Juice 250.

method,

Violette's

method,

volumetric

method,

247.

in

grooves

weight,

mill-rolls,

Renton,

240.

347.

mixed

or

15.

315.

measurement. 120.

Hind-

16.

Messchaert.

5.

Granulators,

of the

extraction, 10.

reduction

Wedderburn's

Glutamin,

calculation

247.

methods,

analysis, 221.

diluted. 302.

purification, 38. preservation

H,

with

hyde, formalde-

83. of

study

Hasewinkle's

solidified

07.

molasses,

in

grooves

mill-rolls, 16.

undiluted. 301. weight. 315. 319.

lead

dry

Home's

201.

strainers, 24.

juice

Hind-Renton

sampling,

method

Jot

170.

sucrose,

Hydraulic

regulators

pressure

K.

for

mill-rolls,14, 16. acid, standard

Hydrochloric

tions, solu-

Kieselguhr,

417.

Hydrometers,

Kelly filter press,

68.

76.

102.

L.

corrections, 104,

temperature 480. 400.

for

Hydrosulphites

bleaching,

76.

Laboratory Lactic

fermentation,

Landolt's

I.

inversion

Immersion

gases.

sugar,

influence

227.

182.

see

of acids

method

subacetate, influence

*

Glucose, on

of

175. inating, elim-

170.

327.

tube, 162. also

Home's

70.

calculation,

observation Invert

dry, 235. acetate, precipitate^ volume error,

324.

refractometer,

Incondensible

Inversion,

Lead

10.

calculation,

400.

tube* 162.

polariscope, 148.

Laurent

Imbibition,

appliances, 171.

136.

rotation,

Home's on

preparation, 414. Levan,

138.

Levulose,

136.

dry, 170.

rotation, 170.

41

T!'

"Mtiinr

t

t.

.^.^".

*""-

s

Ur

557

INDEX.

Retention

number,

308.

Rheostat

for

in

uae

methods,

electrolytic

solution, 416. Solids

by drying. 264.

by refractometer,

331.

reports,

Soxhlet's 8.

Saccharetin,

iron, 6.

Specific gravity,

see

Saccharimetrio

analysis, limits

Folariscope. of

Sucrose.

"ee

Samplers,

automatic,

202.

Samples,

Stock-taking, Strainers

and

compositing

serving, pre-

207.

Sampling,

332.

Sucrose, 134. nitrate

contraction

'

200.

chips, 201.

contraction

of

211.

in

filters,64. in milling, 19.

of dilution, 347.

in sugars,

or

influence the

Silica in limestone, soluble, 387.

total, 387. Sirup, analysis, 259.

of

141.

lead

294.

subaoetate

on

rotation, 179.

of salts

the

on

rotation, 180.

pipette, 231. retention

"

definition, 302.

or

recovery

number,

308.

and

sampling,

molasses,

274.

in waste-water,

Fiske's

cane,

and

optical methods,

10.

measurement

massecuite

264, 266.

Separators, Settling tanks, 44, 46. National,

in

work, 70.

centrifugal, 66.

for

oxalic acid method,235.

in juice, 231.

67. filter-pressing,

Shredder

288.

214, 216.

factory tests, 265.

calculation, 324. disposal in diffusion

version, in-

cattle-food, 300.

Cross's

calculation

on

187.

in bagasse,

in cane,

212.

double

solutions

chemical

methods,

molasses, 211. sirup, 211.

Soums,

on

454.

determination,

massecuito,

Saturation

solutions

dilution, 261.

juice, 201.

Sand

test, 297.

of

filter-presscake, 208.

sugar,

268,

for juice, 24.

cobaltous

199.

diffusion

products^ 80.

cane

ct-naphthol test, 296.

bagasse, 201. cane,

of

269.

of, 207.

care

430.

Steuerwald-Clerget methods,

202.

Calumet,

determination,

boilers, 32.

Sterilisation

coefficient,304.

Saline

glucose

water, Landolt, 198. Sphere, surface and volume, Steam

134.

Saccharose,

for

197.

184.

Saccharon,

225.

tube

solution, 416.

Saccharimeter,

accuracy,

filter

tests, 244.

6.

with

reaction

247.

Solidified molasses, 97.

242.

acid solution, 413.

Rosalie Run

Soldalni's glucose method,

weight,

319.

Subacetate

211.

of

lead, Home's

dry,

179. .

Soda,

carbonate,

to

reduce

ing, scal-

influence

75. for neutralising, 74.

caustic, for neutralizing, 74.

Sugar

on

rotation, 179.

solution, 414. analysis, chemical 187.

methods,

558

INDEX.

analysiB, optical

Sugar

methods,

influence

Temperature,

141.

183. Tin

boiling, 86. methods, Sugar-cane,

salt

Total

90.

as

Cane.

*se

a

Carr-Sanbom

by 271.

by Josse's

flasks, calibration, 160.

by Pellet's

cleaning, 169.

notes

losses, calculations, 335. processes,

Trapetium, Trapesoid,

36.

101. of pure,

preparation rendment,

by

method,

222.

factory calculations, 340.

packing,

76.

drying. 222.

crystallised, estimation,

manufacture,

wash,

sugar

solids, determination

crystallisation, 118.

Sugar,

isations, polar-

on

382.

278:

method,

225.

method,

224.

methods,

on

428.

area,

428.

area,

Triangle,

area,

Turmeric

paper,

231.

etc., 428. 411.

Tyroein, 5.

refineries, classes, 106. V.

refining, 106. refractometer,

228.

Vacuum

212.

sampling,

pan,

solubility, 455, temperature

456.

control, 325. in

errors

ing, polaris-

184.

grades, 103.

trieffor sampling,

Viscous

Sugars, analysis, 274. Clerget's

fermentation,

409.

247.

solution, 416.

weights, 320.

fermentation, 409.

Vivien's for

coils,81.

Violette's glucose method,

212.

method

from

scale

Vinous

of low

treatment

224.

ovens,

85.

tube*for carbona-

control

tion, 56.

sucrose,

275. in the

134.

cane,

,

standard,

by Dutch

color

deterioration

Warehouse

278.

warehouses,

in

103. after

Louisiana

Water,

Wax,

Sulphur, analysis, 386, 397. acid,

in

Sulphurous in the Sweetland

and

solutions, 418.

char:

classification,103.

remarks,

47. 57.

fiber,determination,

Worthington following

for

balance, 194.

manufacture, Woody

Index.

decarbonizer

sugain

303.

List

customary

metric, 425.

White

filter-press,68.

"""

measures,

Westphal's

T.

Tables,

and

116.

acid, analysis, 386. defecation, 74.

Sweet-water,

diffumon, anidy-

5.

cane,

Weinrich's

limestone, 394. standard

in

feed, examination, 294.

Weights

58.

Sulphuric

of quality, 406.

waste,

boiler

Sulphitors, 58.

determination

diffusion,407.

for

sis,294.

47.

process,

105.

quality, 408.

liming, 49. 49.

process,

stoves,

Water-supply improvement

Sulphitation Bach's

for sugar,

67. filter-press, X.

this Xanthin

bodies,

140.

217.

TABLES

OF

LIST

AND

FORMULA..

CARBOHYDRATES. Chemical

and

Physical

Properties

of

the

Carbohydrates.

Principal

Ewell. 458.

CALIBRATION Calibration

of Flasks

Calibration

of Flasks

CorreclionB

for Use

OF

to

True

to

Mohr's

Solutions

Sugar Corrections

and

17|" C.

at

Cubic

or

True

451.

Centimeters,

BAVUk,

Baum4,

and

453.

Centimeters,

Cubic

DRY

the

452.

SUBSTANCE.

Specific Gravity

Brix

Temperature,

Ger-

Hydrometer.

'^

lach, 489. for

Corrections at

Density

Variations

C,

20""

of

Temperature

at

Various

Temperatures.

Refractometer.

Dry

Substance

by

Dry

Substance

by Refractometer,

Specific Gravity

and

Brix

Degree

at 20%** C., 497. Specific Gravity of Water

at

DILUTION Dilution

of Sulphuric

Evaporation Formuls

Tables.

Standard

Hydrometers

of the

Corrections.

(Per Cent

Various

438.

Geerligs, 494.

Sucrose) of Sugar

Temperatures.

Solutions

Landolt,

Anthon,

472.

Concentration,

and

Weight

and

Volume

of

a

443.

Sirup

to

a

Basis

of

30*

Spencer, 440. "

EXPANSION Alteration Coefficients

of Glass

198.

CONCENTRATION.

AND Acid.

Thiesen,

Geerligs, 492.

Spencer, 431, 433.

for Dilution

Reduction

for

490.

of Water

Vessels

of expansion

AND

of

482.

Stammer,

of

Variations

for

to

AND

Brix

VESSELS.

Centimeters,

Units

BRIX

Degrees

of

Comparison

Cubic

in Calibrating

DEGREES

DENSITY.

GLASS

CONTRACTION.

by Heat, 447. of Glass, Cubical,

447.

559

Baum^.

660

LIST

Contraction

TABLES

Cane-sugar

of

FORMULiB.

AND

Solutions

on

Inversion.

Gallois

and

Du-

454.

pont,

of

Contraction

Dupont, Volume

OF

Invert-sugar

Dissolving it in Water.

on

Gallois

and

454.

Solutions

of Sugar

Vaiioiu

at

Temperatures.

Gerlach,

454.

REAGENTS.

Impurities in Reagents Special Reagents

and

of Solutions

Strength

for Sugar

in Analysis, 422.

for Use

410.

Work,

SOLUBILITIES. in Sugar

Baryta Lime

and

Salts

in Sugar

Solutions.

Sugar

Strontia

!^elletand

Solutions.

in Sugar

Sidersky, 466.

in Alcohol.

Sugar

in Water.

Flourens, 455.

Sugar

in Water.

Herzfeld, 455.

Shrofeld, 456.

STRENGTHS of Lead.

Ammonia. Calcium

OF

Gerlach,

475.

of Lime.

in Milk

Blatner, 473.

^

Nitric

Sodic

in

Oxide

Oxide

Oxide

of Lime.

Fresenius, 476. Fresenius, 476.

Hydroxide).

Hydroxide).

(Sodium

Sulphuric Add,

474.

474.

472.

(Potassium

Acid.

Matecaek,

Graham-Otto,

Kolb,

Acid.

Sulphuric

Milk

Acid.

Hydrochloric Potassic

ETC.

SOLUTIONS.

Carius, 475. Oxide

Calcium

467.

Jacobsthal,

Solutions.

Sugar

Acetate

Sencier, 467.

Solutions, 455.

Otto, 471. for Dilution.

Table

Anthon, 472.

THERMAL

DATA. "

Boiling-points of Sugar Solutions. of Thermometric

Comparison FormulsB

for

Converting

Gerlach,

454.

Scales, 444, 446. of

Degrees

One

Thermometer

to

Those

446.

Another, Melting-points

of

470.

Walker,

Freezing-Mixtures.

Metals,

Temperature

of Iron

SUCROSE,

REDUCING

as

447.

Indicated

by Its Color,

SUGARS

(GLUCOSE), OF

Clerget-Steuerwald

Constants.

446.

PURITY.

Steuerwald, 268, 270.

Coefficients

of Purity.

Kottmann,

Coefficients

of Purity.

Home,

526.

522.

AND

CIENTS COEFFI-

of

LIST

OF

Table

Meiasl-Hiller

Reducing

AND

Invert

for

Tables.

Sugar

Sucrose

Tables.

Sucrose

Factors.

Sugar.

Meiasl-Wein,

Sohmiti,

500,

Crampton,

Weights,

Available

of

506.

(Empty

Space)

Gallon

per

SoUdB

and

(Briz),

514. of

Condenser-water.

have

Norris,

Used

been

in

Treating

434.

Sugar-oontaining

532.

S.

and

Bureau and

Standards,

in

Cylindrical

Cubic

Tanks,

Foot

of

Sugar

408. also

Solutions,

Weight

of

405.

Gallon

per

U.

TABLES.

Lippmann,

Von

Mensuration,

Weight

180,

428.

Wantage

Weights

Weight that

Solutions.

Weight

Meissl-HlUer,

512.

Geerligs, the

Substances

of

Index

and

Hersfeld,

425.

Sugar.

Estimation

517.

Rice,

UNCLASSIFIED

Atomic

561

FORMULiB.

616.

276,

240,

TABLES

of

Measures, 425.

Cubic

Standards, Metric

Foot

of

Water

at

Various

Temperatures.

440.

and

Customary.

U.

S.

Bureau

of

n 's

5l "D

s

a n

P

is' as

"

"WESTON" Centrifugals BELT, ELECTRIC

-

and

WATER-DRIVEN

Catalogues our

to

new

particulars of Ball f!9.^ringSpindle, applicable

on

giving

request

all drives.

Specially designed Switch

Electric

Motors,

with

interlocked

Self-Dischargers

POTT,

_"

CASSELS MOTHERWELL,

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and

^^"

patent

brake. Unloaders

plants

Double-curing Btakera:"

and

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WILLIAMSON, SCOTLAND

BATES SUGAR AS

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ADOPTBD

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U.

S. CUSTOMS

8BSVICB

at

"Jt.T"*

No. Bates

18411

Suffar

to contain for use in

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Flasks true

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Sugar Flaska

(M actual

regularly furnished

are

metric

milliliter

at

20^

aiia) by

C,

adjusted

us

or

at

2i\i'* C.

the be within .04ml for the tolerance 100ml and for the 200ml d: db .06ml lOOml is the standard Flask U. 8. Customs capacity. The in paragraph flask described House "b," section yil" Bureau of Standards Circular No. 44, '*Folarimetry. (I

tropics.

They

Each,

adjusted

,

17H""C.

18414

without

Rriemm

UBORATORY Washintton

to

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chan^m

Squre

81

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81.80

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1.80

udthont

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CO.

THOMAS

APPARATUS

100

40

graduation.

ttaht^ct

ARTHUR

West

too

at 10""C.

1841S. "'

to

'.

Capacity, ml 18411.

guaranteed

are

AND

REAOGNfS

PHILADELPHIA,

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"

GUILD

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OF

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Filter Presses,

Water,

Melters, Lime, Magma, Hot Water, Injection,etc.

Spencer's Sugar Washers; Autoand delivery niatic measurement of the wash

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to

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'^Everythingfor

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Inc.

SONS,

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Calculations

0sed

Morse.

Hand 6

Second

tables.

30

Tables 6

Technical staedt Manual

97

Hand I..

binding, %i.oa

by

and

9.

C.J.

for

and

Gaston

grabados. for

Spencer.

de Alanzo

Ribete Chemists 475

117

pages.

C. A.

By

C. A.

By

888

pages.

de

Browne,

Otto

no

Mittel-

Cloth, Si.5onet.

pages.

flexible,(5.00

CaBa.

617

By Guilford L. paginas. 4 by 6j.

net.

ti Beet-Sugar

6i.

pages.

Browne.

Works.

Azucar

by

Irving H. 4 by 6J.

net.

Cuadrada.

4

By

net

Sugar

Bourbakis.

Fabiicantes

do

Book

189

Use. Laboratory Clotb, $1,25 net.

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Calculations

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