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A HANDBOOK

CANE-SUGAR

MANUFACTURERS
IMD THKUI

CHEMISTS.

GUILFORD
7AiV
Chemui
in

l:
of

JPENCEE,

D.So.,
Sugar

Chargt

The Manujjaeluret

Cuban-Ameriean

Company

(Chaparra^DHicias, Tinffuaro, Conataneia, MercedUat and Vniaadt CardenoB Oramercy Refineries); Formerly
Chief of Suffor Laboratory^ U. S. Department if AgriaUturt, WaahingUm, etc.

SIXTH SECOND
TOTAL

EDITION,

ENLARGED,

IMPRESSION,
ISSUE,
TEN

CORRECTED.
THOUSAND

NEW

YORK:

JOHN
London:

WILEY
CHAPMAN

"
"

SONS,
HALL,

Inc.
Limited

Copyright,

1889,

1905.

1916.

1917,

BT

JOHN

WILEY

"

SONS,

Inc.

PRfeM

OF

"RAUNWORTH

CO.

sM

BOOK

MANUFAOTURCBe

"ROOKLVN,

N.

V.

"
I

DEDICATED
IN

BONOB

AND
TO

GRATTTUDB

M.

CH.

GALLOIS AND

M.

FBAN9OIB
PAST

DUPONT

PRESIDENTS
OF THE

ABSOaATION BT

DES THE

CHIMISTES AUTHOR

DE

FBANCB

411603

/"

PREFACE

TO

THE

SIXTH

EDITION.*

This and

edition is enlargedto include


Juice

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 departments of Purdue and Tulane Universities, engineering
has

eminently fitted him


my

for the

of preparation

this article.

I extend

thanks

to him.

few

errors typographical

have been
to

corrected and

some

slightchanges have been made clearly. more descriptions


Cambbidob,

bring out certain

process

G. L. Spsnceb.

Mass., 1917.

PREFACE

TO

THE

FIFTH

EDITION.

The

manufacture section devoted to ijie


this edition.
raw,

has been greatly


use

in enlarged of described.

The

processes

in

in the

facture manuare

plantationwhite

and

refined

sugar

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 rewritten. largely The

chemical

tion sec-

has been revised to meet factories and


now

in

operation.
ones

the conditions of the very large Additional tables are included have

several of the older

("eenreplaced by

recent

tables. G. L. Spenceb.

Washington, D. C, 1915.
"",

vii

'

PREFAC3E

TO

THE

FOURTH

EDITION.

The

first

edition

of

this

book

was

written

at

time

when
little

few

cane-sugar

factories

employed English,
are

chemists

and

but

had

been

written,

in

concerning
now

this

branch,

of

sugar-work. industry
in

Many
with

chemists

engaged
much

in

the

cane-

sugar available

the

result

that

more

material

is

the

preparation
control of
a

of

this

book.

The

proper

sugar-factory
methods of

by

the

chemist

requires
addition

knowledge
a

of

the

manufacture,
brief

in

to

chemical

training.
processes

For

this

reason

scription de-

of

manufacturing

is

included

in

this

edition.

With

the

large
few

increase
the

in

the

scale

of

manufacture

ing dur-

the

past

years, toward

greater
the

complexity production
the of

of

processes,

and

the

tendency
whether
raw

one

grade

of

sugar,

or

refined,
the

necessity
is

of

having
generally

competent

chemist

in

factory

becoming

recognized.
G. L. Spencer.

WAsmNOTOir,

D.

C,

1005.

CONTENTS,

MANUFACTURE

OF

CANE-SUGAR
FAcn

R"w

Material
of the and Raw of Juice Fuel
:

1
0 32

Extraction Steam Outline


Plant of

Sugar
the and

Manufacture

36 38
in

Purification Defecation
Defecation

Juice Clarification Closed Closed


of

Open
and and

Tanks

39 Settlers Settlers 43 45 47 49
'.

using using

Heaters Heaters Louisiana

Open
Closed

Defecation

Sulphitation Sulphitation
Carbonation
Harloff's Acid

Process after

Liming

Processes

50

Thin-juice
and

Process

55
58 60 61

Sulphur
Carbonation Lime Filtration Chemical

Stoves

Sulphitors

Tanks

Kilns Processes and used Juice and

Machinery
in

63 the

Reagents
of of the Juice

Purifying

Juice

72 77

Evaporation
Preservation

Sirup

83 85 86

Crystallization
Boiling Sugar

of the

Sugar

Crystallization
Purging
and

in

Motion
the

94 99
.'

Curing
of of of of

Sugar Sugars Sugars

Classification Classification Deterioration

Raw

102 103 103

White

Sugars
Raw

Warehousing Sugar
Raw

Sugars

103 106

Refining
Materials

107 109

Defecation Filtration Char Revivification


of the

112

115

Crystallization Drying
Technical
and

Sugar
the

118

Finishing
and Chemical

Products Control
XI

120

123

XU

CONTENTS.

SUGAR

ANALYSIS
PAQB

Sugars
Optical
Chemical

and

other

Constituents
of

of

the

Cane

and

Its

Products

134 141

Methods Methods Determinations

Sugar
of

Analysis Analysis

^
"

Sugar

187 191

Density
General

Analytical
and
of of of of of of the the

Work

109 199
:

Sampling Analysis Analysis Analysis Analyras Analysis

Averaging Sugar-cane
Juice

214 221

Sirup,
Sugars

Massecuites

and

Molasses
;

259 274 280

Filter-press Bagasse Factory


Molasses and Wastes

Cake Exhausted

Analysis
Analysis Analysis
Definitions Chemical

Chips

282 294

of
of

Cattle

Food
of

298

and Control

Applications
of

Expressions
Work

used

in

Sugar

Work.

301 310 340

Sugar-house

Sugar-house Evaporating
Purchase of of

Calculations and Cane Juice


on a

Heating
,

350 of its

Basis

Analysis
and

382

Analysis Lubricating Analysis

Limestone,
Oils

Lime,

Sulphur

Sulphurous

Acid

386 390 403

of of

Flue-gases
the Water

Quality
Fermentation

Supply,

Treatment

of

Impure

Water ".

407 409 410 423

Special
Reference

Reagents
Tables

LIST

OF

ILLUSTRATIONS.

VlGTTRa

PAGB

Central
1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20. 21. 22. 23. 24. 25. 26. 27. 28. 29. 30. 31. 32. 33. 34.
.

Delicias,

Cuba

ProntUpiece
10

Cane-shredder

Krajewski Krajewski
Fulton Fulton Puunene Fulton

Crusher

11 11 12

Crusher-roll

Crusher Crusher-rolls

12
13
\

Housing Housing
Juice

14 16 18

Meiaschaert's
Mill

Grooves

Settings
of

Diagram
Draw-down

Compound

Saturation for Defecators


^

20 44

Pipes
of
Tube

Diagram
Vivien

Deming's

Closed

Settling-tank

46 56 59 68 69 121 141

Sulphur
KeUy

Stove
Filter

Press.'!
Filter Press

Sweetland

Hersey
Nicol

Granulator Prism

(diagram) Single

Half-shadow Double

Compensating Polariscope
(Josef (Julius

Polariscope (Schmidt
"

143

Compensating Polariscope
Polariscope

Haensch)
,.,...

144 146 147 148

Half-shadow Half-shadow

Jan-Fric) Peters)

Triple-field Polariscope
Arrangement
Laurent of

Prisms

in

Triple-field

Polariscope
Polariscope.

(diagram)
. ..

149 150

Polariscope
Attachment Tint for Laurent

Compensating
Transition

151 152

Polariscope
Ventske
Scale
^

Cane-sugar
Control
Tube

Scale,
for

154

Polariscopes Ordinary
with Tube with Side

158 Forms End


158

Polariscope Polariscope
Bates'

Tubes,
Tube

Enlarged

159
159

Polariscope
Tube

Polariscope
Pellet's Pellet's Landolt's

Tubule Tube
Form
._

160 160 161 162


,.

Continuous Continuous Inversion


Desiccator

Polariscope
Tube,
Tube

35. 36.

Modified

37.

Wiley's

Caps

for

Landolt's

Tube
^
" " "

162
,

XIV

LIST

OF

ILLUSTRATIONS.

flOUBB

PAGS

38. 39. 40. 41. 42. 43. 44. 45. 46. 47. 48. 49. 60.

Sugar

Capsule FilteringDevices Sugar Flasks, Diagram


Flasks

166
166
^

of

Types

167 168 170


,

Pellet's Conical

Sugar Balance
Decimal Balance Norma Brix Balance for Rough Alcohol
."

171 172 173 193


,

Weighings

Stove

Hydrometer Reading the Hydrometer Westphal Balance Pyknometers


Calumet

Scale
,

193 195 197 203 205 206 209 212 213


,

Sampler '51. Coombs* Drip Sampler 52. Horsin-Dton's Sampler 63. Press-cake Sampler 54. Sample Box for Sugar
66. 66. 57. 58. 69. 60. 61. 62. 63. 64. 65. 66. 67. 68. 69.

Sugar

Trier

Hyatt Cane-reducer
Extractor

214 in Fiber

for Use

Tests

218 223 224 227 228 229 231

Vacuum Vacuum Abbe

Drying

Apparatus
or

Drying

Distilling Apparatus

Refractometer
Refractometer

Immersion

Sugar
Sucrose

Refractometer

Pipette
Holder for Alundum

Funnel

Crucibles
Holder

238 238 239 241

Sargent's Alundum Filtering Apparatus.


Alcohol Current Soxhlefs
Burner

Crucible

Regulator

for

ElectrolyticWork

243 244

Filter Tube
Burette Filter Knorr

70. Squibb's Automatic


71.

248 248 255 255 255 Volume 262 269 Content of Massecuite 271 281

Wiley
Muffle Muffle Muffle

and

Tubes

72. 73. 74.


75. 76. 77. 78. 79.

for Incinerations

for Incinerations
for Incinerations for

Apparatus
Inversion
Karcs's

Weighing a'Unit
."

Flask

Apparatus
Flask

for

Crystal
"

Kohlrausch

Bagasse Bagasse Bagasse Bagasse

Chopper, Boot
Chopper,
Oven Athol

Krantz

283 283

80. Bagasse
81. 82.

with

Induced

Draft

285 288 290 291

Oven

83. Bagasse
84. 85. 86.

Digester Digester, Norris


Extraction Control

Knorr-Soxhlet Hors6n-D6on's

Apparatus
Device

298
318

LIST

OP

ILLUSTRATIONS.
m

XV

FIOVBB

PAOB

87. 88. 89.

Lftboratory
Massecuite

CeHtrifugals
Funnel
for for

326

Separating

the

Molasses

326 347 355 356

Diagram Diagram
Vacuum

(CobensI)
of
"

Calculating
Effect

Mixtures

90.
91. 92. 93. 94. 95. 96. 97.

Multiple

Evaporator

Pan Distribution
of in

Vapor
Elevation Knorr's

Multiple

Effect

358 359 392 393 400

Horisontal

T3ri)e

of

Evaporator

CO2

Apparatus
Alkalimeter

Schroetter's

Engler's
Orsat's

Viscosimeter

Gas

Apparatus
.
.

404
.

THE

MANUFACTURE

OF

CANE-SUGAR.

RAW

MATERIAL.

1.
genus

Sugar-cane.
Saccharum.

"

Cane The

is
mode

large grass, belongingto


of its

the with

growth

varies Until

variety, climate, soil and comparatively


sterile. the
arrows

cultural

conditions.
were

within
to

recent

years

its flowers
or

believed

be

The

plant "arrows"
then noted
not

blossoms

usually only in
year.

Tropics and
have been

freely every
in

very

few

in Louisiana

exceptionallymild
in

years.

Large numbers
stations
new

of

seedlingsare
seedUngs
are

now

produced
in the other with

ment experifor

in various The

parts of the world


crossed
to

search

varieties. with

seedUngs

and

existingvarieties in order
These

teristics. develop certain characin several varieties


new

experiments have
now

resulted The

which selected
sucrose,

are

in broad

culture.

varieties
as

are

for

some

particular qualities such


to

richness

in

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

resistance

of

seedling varieties
are now

is in

Java.

There

few

old varieties

cultivated. in Cuba that


^*ery
sucrose sucrose a

It is
cane

generally believed freely is


not very

year

in which

the Such

arrows

usually
rich
in

productive.
content

cane, sugar

however, is often
content.

an?l of low invertfor several

It increases

in its
as

months

after
as

flowering, and, regards


the

is true when
may

with the be

other

canes,
season

deteriorates

sugar

rainy

begins. plant

The

yield of

cane,

however,
heavier

grows

littletaller and

after

small,since flowering.

the

RAW

MATERIAL.

"

Sugar-Ksanevaries greatlyin richness in differentcountries


and
even even

in the
a

same

country.
content

It does

not

often exceed in A

or

attain

sucrose

of 17 per

cent

Cuba, but this


cane

is sometimes

surpassed in other countries.


12 per cent

iana in Louisvery

containing
rich.

of

sucrose

is considered

Sugar-cane is propagated by
located
at

means
or

of the buds

that
cane

are are

the
a

nodes.
very

Pieces shallow

cuttingsof the
or

planted with
localities
are are

covering of soil

in certain

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

these

several
canes.

shoots The

or

suckers. under

These

form

clump
climatic

stool of conditions

cane

suitable soil and

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

and

so

on.

Fiscal
to

or

soil and

climatic
or

conditions

times someone

limit the crop


or

"plant-cane"
are

to

plant-caneand

two

ratoons.

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.
varieties
Normal
sugar-canes
are never

Dark-colored

hollow

or

partially so.

They
and

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.
that
ar"

contain

Canes
other of such The

abnormal
are

on

account

of

some

climatic

or

conditions
cane

sometimes

hollow, but

the

proportion

is usually very

small.

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 irrigated the distribution of water district, is suspended a few weeks before the cane is to be harvested,
to

promote
and

ripening. The
the

sucrose

content

of
as

the the

stalks

increases

reducing approaches maturity.


The stalks
are

sugars

decrease

plant

cut

off close

to

the

ground

in harvest^

HAVf

MATERIAL.
"

by burning, but it must


loss The

be harvested

very

promptly

to avoid

which through deterioration,


rate of deterioration

is accelerated

ing. by the burnshould


agrees
cane

is greatlyincreased The
to

rain in
to

fall upon the burned cane. Cuban most contracts cane and but The

manufacturer burned from it at

receive

up

includingfive days
in the
event

without

deduction
may

the
any

price,
time.

of rainfall he

refuse

of the juice is purification with of the burned


as

not

with

sound
sooner.

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

evaporator

foul

The

fine

of particles and
a

carbon

sometimes

finally appear
of sound

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


and

ture mixcane

burned

cane more

rather

than

burned

alone, since the mixed


The with their method local
cane

juicesare
Small small

purified. readily
cane

of transport of the conditions.

to the

factory varies

factories
cars.

in

carts

or

usually transport Portable railways are


in

largelyused in the Hawaiian


not

Islands
cane

and

Java, but almost


to

at

all in Cuba.

The

is

brought
It is

the

factory

or

railway in Cuba
in the Island

in bullock and
use

carts.

of Hawaii The

in British of flumes

the factories fiumedj" ported transGuiaiJS^|nisually and

in punts. 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 Sugar-cane is usually sold
to

complicates ptu^is mills. jui3B|^the

necessary. to

the factories without

regard
cane

its richness
to devise

in sugar
an

or

the

cult purity of its juice. It is diffifor the

equitablemethod

purchase of

upon

The of

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

basis of its

Louisiana

at

the

time

of

harvesting, Novembercourtesy
of Dr. C. A.

December,

is inserted

through the

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

LOUISIANA

SUGAR-CANE.

Wa""r.

74.60%
SiUca.

74.60%

Si02. Potash. KjO


CaO

0.25 0.12
0.01

Soda"Na^
Lime.
Ash. O.fiO

Magnesia, ACgO Iron, FeaOa Phosphoric acid, P^" Sulphuric acid, SOs.
Chlorine, Q.
Cellulose Pentosans.

0.02 0.01
Trace 0.07

0.02 Trace 6.60


2 .00 60

Fiber.

10.00

(Cane-gum) Lignin bodies, etc

i Xylan fAiaban

"

2.00 12. 60
90 60

Siiears

14.00

Sucrose Dextrose
Levulose

Nitrogenous bodies 06%) (Total N-.

0.40

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

0^ 12
0.07
.

0
.

20

0.01

T^ace
Trace 0.20
0.20

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


. ..
..

0.20
0.20 0.08

0.12

(Malic, succinic,etc.) ) "


*" "* ""

0.08
0.12

Total

100.00%

100.00%

The that
are

juice of
more

the
or

cane

contains

nitrogenous substances

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

broken

up

in the manufacture

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 molasses-makers. positive 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, of amount not sugar of the juice. The these organic impuritiesdepends upon the age and variety of
tic and the
cane

the result that asparin the molasses along with

and

also

upon

the

pressure

of

the

mill-rollers.

Their and
* s

percentage is much
third mills than

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

Eighth

Int. Congress

App.

8, 103. Browne,
La.

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

Planter,

1904, 3S, 49.

RAW

MATERIAL.

relative percentage is also than in

sion-batter from the diffuhigher in the juice


wax,

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

the greater

of the

juiceare

content

of the

cane

and

also the coefficient of

purityof
The

the

juicevary
that of

greatly in different parts of the stalk.


is of lower the
sucrose

juice of the nodes


the lower has

content

and

lower

purity than
exists between NoSl Deerr

intemodes.

similar

difference

"Uid upper

halves of the stalk.


canes,

analyzed whole
the
sucrose

the

pith, rind and


to that

node, and
whole the In
cane

has referred
on a

in each His

part

in the

percentage basis. ^
for three

figuresare
of Hawaiian

given in
canes.

following table

varieties

it should be considered that the separausing these figures tion into pith,rind and node can be made approximately only:

The

cane

contains

coloring matters
'

such

as

chlorophyll,

anthocyanin and saccharetin


insoluble in water and

of Steuerwald.

Chlorophyllis

in the readily removed of the juice. Anthocyanin is precipitatedin the purification 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. Sacis present in the fiber of the
cane.

is therefore

According

to

Steuerwald
lime and and

it turns

yellow and

is soluble

oliier alkalis and

is not

in the presence of altered in the carbonation unites with iron to

processes. sulphitation
an

Saccharetin

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

form

Bui.

30, Haw.

Sugar

Planters'
53.

Exp't Sta.,
de

36.

" *

Int. Sugar C.

Journ.,

14,

Mftller, Bull.

Assoc,

des

Chimistes

France,

31, 849*

MANUFACTURING

SEASON.

manufacture
charetin

and
be

finally appears

in

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

matures

the levulose

content

decreases
appears, to

and

sometimes

iisappears. Levulose
molasses. the dextrose salts of the This when

again always
is due
are

reappearance

however, in the isomeric changes in


in the presence of

its solutions

heated

earths, notably potassium of Cuban salts. The content cane-juice, reducing sugar termed the "glucose" in the cane levulose and dextrose,
alkalis and 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 mineral The 0.25 of the ash is quitevariable. cane-juice tween 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
or

ash content

of the

K3O,
about The
year
unms

25

to 45 per

cent

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":
"

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

This The

is true
season

in

Peru

and

in parts of the Hawaiian

Islands.

of manufacture

in Louisiana
1

begins in October and November and lasts through December and often into Jancane

Pellet been

reported raffinose in
confirmed

molasses,

but

its des

presence

has de*

not

by

other Deut.

chemists

(Bull. Assoc,

Chimistes

France,

14, 139;

see

also

Zuckerind., 9(3, 1439).

RAW

MATERIAL.

ANALYSES

OF

THE

ASH

OF

CUBAN

CANE

JUICES

(Percentages

of

the

Ash)

Factory Silica,
Iron

and

Crop

Year
. .

(1912)
SiOs and
6.46

Alumina,

FesOs^
3.00 4.70

AliOj

Lime, Potash, Soda,

CaO

Magnesia,
KsO Na"0..

MgO

5.01 46.28 1.36

Phosphoric

Add, Acid,
CI

PiOt.
. . .

4.21 4.08 12.90

Sudphuiic
Chlorine, Carbonic

SOt

Acid,

COt

10.53

uary.

The in Porto

season

begins
The

in

December

in

Cuba

and

in of

uary Janthe

Rico, is from into

usual

manufacturing
until
or even

period
though
in

West
may

Indies continue

December

June, longer

grinding
of
on

September Cuba,
and in climatic with the

parts

the
count ac-

northeast of
season

coast

of in

frequent following
and in

interruption
months. continues
many

rains

May

The

ian Hawaisix
of the

begins though permit


a

November conditions much

about

months,
Islands of from the

parts
The

very

longer during

season.

factories
or

Dutch about with

East

Indies into

grind
November.
season.

the This

dry

monsoon, very

May
the

corresponds

nearly
The the

Argentine
of the

advent

rainy
in

season

determines
The
cane,

the rains but

close
not

of

manufactunng
with the

period

the

Tropics.
of of the

only
it
to

interfere
renew

transportation
at

cause

its growth

the

expense

its

sucrose

content.

EXTRACTION

OF

THE

JUICE.

3.

Milling

Processes. from the


cars

"

Unloading
carts

the

Cane.

"

^The

cane

is unloaded in the

and

by

mechanical

devices of such

well-equipped
are

modem

factory.

Many

forms

devices
Where little These
carts
or

in the

use,

especially in Cuban
is cool in and the-

factories.
cane

climate
as

deteriorates
are

but used.
cars or

in
are

storage,

Louisiana,
to

derricks
cane

often the

usually arranged deposit it


upon

lift the

from

and

endless their

conveyors,
or

termed

carriers

elevators

according
or

to

form,

in

large piles for the


cart
are or

night work,
service. in In
up

to

prevent
latter
cane

interruption
the in in
same

in the

railway

the the

case^

derricks
upon

again used
carrier. and
or

picking Raking

and used for

placing it
many

the

devices
extent onto

are

Louisiana
cane

factories from the


cars

to
a

some

in Java the

pulling the

platform
Hoists

carrier.

and in

dumping unloading
to

devices
cars a

are

very carts.

generally
The
of
a

employed
usually
of
cane

in have
at to
a

Cuba
a

and
or a

hoists car-load

capacity
and

lift

half the

third

time

drop it into by
elevators.
at

hopper
These with
are

from

which
are

it is carried

the

mills

elevators
arms

heavy drag the


the

less endcane

chains,
with them.
a

fitted

intervals
or are

which under

Chains

cables attached

passed
to
a

load, in
with
a

using

hoist, and
device. time in

yoke,

provided
often the
use

tripping
loss of

The
this

breakage
method.

of

bundles

occasions of hoists in

However,
of the

greatly
factories

simplifies the using three


devices
cane

arrangement

railway

tracks

milling plants.
are

Dumping
the there

in

great
with
cane

favor
a

in

Cuba.

They

charge disther, Fur-

quickly and
of

minimum transit. In the

of labor. There
one,
are

is little loss of

in

two
car

general types
run

dumping
which

devices. is then
a

the the the 9

is is

upon

platform,

tilted door

and into

load

discharged

endwise

through

swinging

hopper

10

"

EXTRACTION

OF

THE

TOICB.

of an

elevator. The

In the second
or

type the platform is tilted sidecar

wise. and when

stakes
at

sides of the
with

aie

hinged

at
are

the

top

fastened

the bottom the


load.

latches, which

released
ployed em-

dumping
in

Hydraulic-power
The

is usually

tilting the
that

platform.

platform

is hinged

at

such when

points
the

the weight of the load itself is released


very

causes

it to tilt

wat"r

from

the

hydrauhe
pressure level

cylinders.
is required It is

With
to

this arrangement
the that

little water
car

return

platform
mechanical

and

to
were

position.
tor

probable
cane

devices

first used

handling
The

in the
cane

sorghum-sOgar
should

industry.
delivered
to the

The

be promptly

mills.

loss of sugar the fields and

due
cars

to the

exposure

of the cut

cane

to the

sun

in

is very
"

large. Multiple-mills
are

Mating
in

Machinery.
the of
cane a

used
its

exclusively
These
more

crushing

and crusher crusher

in
or

expressing
shredder shredder

juice.
three
or

usually consist
3-roller mills.
prepare
structure

and
arc

The

and

designed
the

to

the and

cane

for milling
case

by

breaking

down

hard
of

in the

of the crusher,

extra.ctinga part
for

the

juice.
first successful
National machine for preparing
cane

The
was

milling
Samuel coosista

the

cane-shredder, Fig. 1, invented


in Louisiana.
This

by

Fiske

and

first used

machine

tACnOH

OF

TKB

TUICI!.

MILUKG

FBOCEBSES.

13

A This from

fie"tond type

of crusher
or

ia the

Fulton, shown
The

in Fig. 4.

differs in its cutting

crushiog surface quite radically


crusher.

that

of the

Krajewski
from

cutting

teeth

ue

V-sbaped
fihown
in

and

are

luranged spirally,1.75 inches opposite ends


are are

pitch, vith
is well

the spiralsworking

of the

rolls, as

Fig.

5.

There
scnqiers

also grooves

separating the teeth prevent clogging the


the
cane

into groups, teeth. This

and

provided
crushes

to

machine
a

not

only

but also expresses

considerable

pt^

thoroughly, of the juice.

Fig.

8,

In

some

in atr^tgthening old mill' installations, especially


at

ing plants,
Btead mill.
a

moderate

cost,
or

crusher

is not

used, but
as

in its

special corrugated
Such

blunt-tooth

top roll in the first "excelsior

rolls, especially a
very

type

known

rolls,
Fig. 1.

"

are

generally used in Java.


mills have

PresentKlay
The

always three rolls, ae


the
cane or

is shown

in the
'

bottom that

where roll,

enters, is termed

"cane-roll," and
roll." The
two

opposite the "bagasse"


rolls
are

"dischargein

bottom

usually rigidly fixed

pod-

14

EXTRACTION

OF

THE

JTHCB.

tion and is
so

the top roll is controIIe4 rise and


cane.

by

an

hydrai'.ljc ram
"float"' with
presatire

uid tions varia-

arranged that it may


in the feed of the

fall or

Hydraulic
builders, The crushed

is

applied
in called

to

the bagasse-roU by

certain

ram

is shown
now

in the

top-roll cap
is

in

Fig.
from

7.
one

cane,

"b^asse,"
curved turner,

passed

pair
a

of rolls to

the

next

by

plate, variously termed

turnplate, knife, dumbto

trash-turner, etc., according

the country

in which

Fw.

7.

the mill la used.

This

is

supported by

heavy

steel turn-

plate-bar.
The mill-rolls
or are

supported
The
2 and

in massive older types

castings
of models bottom The in

termed
are

housings
shown

mill-cheeks.

housings

in Figs. 1 and
7.

more

recent

Figs.
rolls
are

and

The from

crown

wheels
are

by

which

the

driven

the top roll

shown flexible

in Fig. 1,

drivinggearing

engine
with The

is connected

through

couplings and

the top roll of the mill.

Fuupene housing, probably

the

original of the inclined

MILLING

PROCBS8ES.

16

type,is shown
shown which in
one

in

Fig.6.
This
note

A recent Fulton
latter

inclined housing is

Fig. 7.
may

dispenses with the king-bolts above. the top-rollcaps of projecting


6.

other types in

Figs. 1, 2, and
promote
Since the

The

the object in inclining of the top roll. which the The ing' housthe the and

housing is
cane

to

"flotation"

enters

the mill from

the side toward

is inclined.

the

greatest
and that

stress

is between
so

bagasse and

by incliningthe housing top rolls,


between the

that
Cane

/resultant of this pressure

the

the top-roll angle of inclination, 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


"

**

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

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 an

Mill-rolls

cast of

iron mixtiure that will remain

the

bagasse. A

return

to small

grooves

and with

even

tively compara-

smooth-bottom
t

rolls is

probable

the introduction

of the

described below. deep juice-grooves 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
1 J inches

be

in rolls 34 inches rolls. The

to 36

inches

in diameter

and

less in smaller in

method

of

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

16

EXTEACTION

OF

THE

JUICE.

vibrftUona. be The
used

An

unlimited

quantity
or

of saturation of

water

may

without

Blipping

reduction

grinding capacity.

mill inlets and


some

ai"e, in
all tend

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

to

an

juice extraction
further
the
more

and

also

grinding

capacity.
Messchaert is obtained These
the
grooves
'

states

that

improTement
discharge
numerous or

in extraction

by also grooving
are

bagasse roll.
than
those
1

smaller
are

and

in

feed"rotl and

1 inch
these

wide, 1
the

inch roll

deep
may

and

inch

pitch.
The

Except
must

for

grooves

be

smooth.

top loU

always bear

the usual

grooves,

preferably

about

three

per

inch.

The

moisture

content the

of the

bagasse

is materially
Another

reduced

by

grooving

discharge roll.

Hawaiian been tor the

invention in
over a

is the Hind-Renton

grooving.
an

This
average

has

tried out
crop

milling plant that obtained


97
per cent,

of

extraction

(sucrose

extracted
per

inch

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

of about the
lower

that

the juice flows that the

out

through
wedges

part it

the boot

groove

and

bagasse

itself above
that

in

"boot-jack,"
with this

It is also claimed

steel roll-shells may


pressure
on

be used

grooving. by
meana

The
of

the top roll is usually regulated except


not

hydraulic
few

rams,

generally

in

Java,

paratively Com-

mills in Java

have

most hydraulic regulation,, MMbinery


for

Mauutacturing

191^

MILLING

PROCESSfiS.

17-

of the mill

engineers preferringvery

slow

roll

speed and

rigid

setting.

applied on the top roll varies with the strength of the mill and the quanthe length of the roll, tity 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,
The

hydraulicpressure

''

pressure

on

the

crusher,425
tons to
on

to

500

tons

on

the first mill, and These

from

300

to 450

the other

mills of the train.


very

numbers
pressure

apply
cane

top rolls 7 feet long. The


the crusher and

high

applied to

crushed

to receive

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

the last mill. The

hydraulicregulationof
the viz.,

the top roll has

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
between the rolls to suit variations

in the quantity of
The

cane

or

bagasse
now

passing through

them.
a

hydraulic

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 of metal

springs
instead The has

are

used

en

many

of

Watson Mirrless,

Co.'s

mills

of
use

hydraulic rams.
of very

strong cast-steel housings


to

or

mill-cheeks

enabled

manufacturers

dispense with

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
'^

king-bolts. only part way

between

the

rolls and

the

relation

of the

tum-plate

to

the
.

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

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
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
in Java

the rolls.
to
as

This
as

ranges
over

from
30

as

low

as

12 feet

or

less

high

feet per

minute

in certain

SrdliiiU

Hawaiian

plants. The

Cuban

is practice

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
and each

conveyor
cane

results in greater the Crusher and

delivery of the

to

uniformity thus by giving


it promotes

the crusher

mill full work

at all times

the extraction of the

juice.
now

Milling-plants are
many
as

in

operation using from

to

as

21 rolls in addition

to those of the crusher.

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

EXTRACTION

OP

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 the manufacture.
to meet

The

application
tions combina-

of the water

is modified

the needs

of other

Paia

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

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

is

applied

to the upper

the from

lower

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 do
so

is sometimes

above

just as the bagasse emerges

from

between

IV

"0i"""^
To Defecation

^^
this way

Fio.

10.

the rollsso that it will absorb it in


it acts The
as a

expanding. In

sponge

that has been

compressed.

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
cost

are

used. and

The

usual

Cuban

high

of labor

cheapness of the

product, is

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,
to

MILLING

PROCESSES.

21

causes

the

rolls to

These

conditions

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

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. Tests

by

many

lead investigators is practically the


same

to

the

l^onclusion the

that

the mill extraction be used of the water of


warm

whether
matter

tion-water macera-

Ipt or

cold.

The

of the

quality

and

water.

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

sugar

manufacture. of return

The

hot

water

is derived

from

the

plus sur-

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


water, from
Those into distilled water. saturation
water

the
pure

of the heat the

units
are

that

pass

with

the

largely economized. is also a slightlyincreased There evaporation of moisture the bagasse in transit to the fires, from as compared with with cold saturation. With that obtained properly fitted rolls th"*e is Uttle danger of looseningthe shell from the shaft by expansion in the
The saturation Neither
use

juice

of

warm never

water.

bagasse.
the time

completely penetrates the the physical condition of the bagasse nor


water

the duration of the contact with the element, i.e., water, permits complete penetration. Manifestly the nearer we approach this ideal condition,complete penetration, the better the and the the extraction of the sugar. Modem mill

practice is

reverse

of the older methods

in which found
up

the strongest mills in the last mill of

the heaviest series. The

were roll-pressures cane

is

now

broken

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

thoroughly in the of the juiceas possible,

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 clearly recognized that the bagasse be thoroughly prepared for saturation. these Under must

conditions,moderate
mills.

pftessures only

are

requiredin the

sequent sub-

22

EXTRACTION

OF

THE

JUICE.

If all the
or

of the plant are ruptured juice-cells


process

in the shredding

crushing
be

and

the first grinding,it is evident


to the

that

when

the water

is

applied

bagasse, if the time

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

only
The

cells escape the superficial portions of the juice are

short, and
author

so

many

of the

rupture, that
diluted.

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
has
to
near were

demonstrated

45

parts of water, and


the then
one boiling-point

the

maintained temperature was The and bagasse water hour.


and the dilute

juicewas strained The residual juice was off, expredsed using moderate- pressure. 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. in millingto dilute all of the juicein the it is not practicable and that a factor depending bagasse with the saturation-water, the time element and the efficiency of the mills must upon in estimates of the water be applied actuallyutilized. The followingfiguresare from records of actual milling:
COMPARISON OF

thoroughlymixed

MILL-JUICES.

MILLING

PHdCBSSES.

23

Water
the second

was

sprayed upon
mill. The
upper
ones

the

bagasse as it emerged
were

from well

layers of the bagasse


received much

but the lower saturated, latter


was

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

bagasse. Influence of the Structure' of the Cane


structure very

on

MiUing.

"

^The With

has

marked

influence

on

the mill results.

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,
45 per cent

efficient

of fiber and been and

60

per

cent

of moisture. when

These

conditions

have 247

observed 100. Influence Deerr

in Java

grinding the
of the Cane

varieties Nos. In his


on

study of "The
Work
"

of the Structure
says:

Mill

Noel

"It

not

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
a

decrease

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
overcome

extraction. this influence.

Increased

saturation

is necessary

to

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

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

in the

that is extracted

in the

the

relation between
1

the fiber and


Sugar

sucrose

in this material.
Expt. Sta., 41.

Bui.

30, Hawaiian

Planter's

24

EXTRACTION

OF

THE

JUICB.

Straining the MiUrjuiee. ^Three types of Juioe-strainers


"

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-brass plates surfaces are whose of flights k^t clean by means or slats, The similar to a squeegee. attached less endto flights are an
are

in use,

viz.:

(1) Hand

strainers

in which

the

link-belt.
surface of the

They brush

the

of bagasse from particles

the

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

perforatedwith
holes and
are are

about

324 the

round

holes be

per

square

inch.

If the thinner that

smaller

plates must
This

correspondingly

liable to break.

is the type of strainer

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

(see

page

102).
is

In

this

the modification,

bottom

of

the

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

roimd under '^cush-

is discharged at the end of English factories, in a thoroughly drained the strainer, state, and is returned by an elevator to the mills for regrinding. cush'' of the The modern first type of strainer is not factories. The second
to be
or

considered

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
of the ihick sheets perforated sheets be the is very The
a

great, and
be link-belt
source

in order

to

use

perforations must

larger than
soon

would
very

otherwise

necessary.

becomes

foul,and
escapes

undoubtedly this is

since the consideration, be frequently must the strained juice. The belt and flights and tanks under The juice-canal 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. The third the type of strainer,

of sugar losses which chemical control begins with

"grasshopper,"so

far

as

DIFFUSION

PROCESS.

25

the
very

writer is aware,
marked

is

as

yet untried

outside

of Java.

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
may

be

used.

There of
cane

is very

little

wear

on

the

sheets.

strainingsurface
for 1000
tons

approximately 2X16
per
raw

feet is sufficient The

of

24

hours.

thoroughly straining the


manufacture
4.

juice and
6.
'

importance of its bearing on the


tlie

is stated of the
reason

on

page

Extraction
"

the

Juice

by
a

Diffusion
was

Process.

When
was

first edition of this book


to

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, howexpect
do their work due
to the increased

in 1889, there

with

marked

expense

fuel economy. It is largely the large water requirefor fuel, ments

and
or

the

in disposing of the residual ''chips" difficulty diffusion has of been almost doned. entirelyabanthe

bagasse, that
The results of

convenience

milling, with mills, has


also view much of these
space to

attendant
to

excellent the

by modem
In
so

contributed conditions
a

decline

diffusion.

the

writer hesitates in
as

devoting

process

that,

regards the
In

cane

industry,is
the
cane

almost

only

of historical

interest.

the diffusion process

is cut

into small

chips

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

strainers

at

the top and

bottom,
as

with

with suitable 27. The

pipe connections
a

indicated

in

juice-heater the diagram,

diffusers are

is called
are

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


with
warm

systematicallyextracted
The
water
are

water

in

these

diffusers.

enters

the first cell in the

filled series,

with
from

chips that

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

26

EXTRACTION

OF

THE

'JUICE.

fillsthat containing fresh canepredecessor,UDtil it finally from cuttings. A measured quantityof juiceis now drawn oflF is pumped defecation-tanks. to the the last diffuser and The the first diffuser exhausted is
now

disconnected
are

from

the

series and The with

chips it contains

containingthe least sugar are weakest juiceand the richest in


The which

discharged. always in contact


sugar

chips
the

with

dense

juice.
solution,of

diffusion process
a

in

theory

is based

upon

that property in

certain

class of substances
a

possesses,
a

passing through
Certain classes and which colloids.
accoimt

membrane substances

into
pass not at

of

contiguous solution. through a membrane


all. The former stances, sub-

readily

others

slowly

or

include
process

The

sugar, are is termed the


or

the' direction
"osmosis"

and the latter, crystalloids "dialysis," or, taking into moves through the crystalloid
The process
a

membrane,
for the
cane

"exosmosis."

ideal

tion condithe

of this highest efficiency into slices little more than

is that

in thickness plant-rell rupturing 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 residue. This condition can in the exhausted impurities 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 that the various in place, and that are ti?;ht, signal-bells
The
"

all mechanical attention. One of the

details essential to

good work

have

received

several

methods

of

arranging the valves


27. cell No.
1 with

of

battery is shown, in the diagram, page


For convenience of reference
we

will suppose

4 is

the first to be filled with when this cell is filled turn


two

chips. Fill cell No.


the water
3 in the

water;

into No.
same

2, passing it

through
the water

heaters; fillNo.
about
of hot

manner,
assures an

heating
dant abun-

to

203** F.
water

This (95" C.).^ first round

supply
heater No. No.

for the

of the

battery.

Fill cell No. 4 with


3 and

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

4 at the

bottom, drivingthe air

of this cell

through

28

EXTRACTION

OF

THE

JUICE.

with

chips. It is
For

now

time

to
us

make draw
as

the first draw


from the

of diffusion-juice.

example, let
same

No.

II.

Having
the

filled this cell in the


next at

manner

precedingones,

manipulation, the
the

pressure

top, is
the the

to

open

the

valve and of

being already established connecting the juice-main


draw
a

with drawn

measuring-tank
requisiteamount
open

charge.

Having
the the with

juice and
as

having
No.
12

closed

tank-valve,

that

connecting heater
12

juice-main and
is draw filled,

fiU cell No. its

usual, this cell having


cell No.
12

previouslyreceived

charge of chips. When

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 another closed and also that
5.

connecting heater
cell No.
out 5

No.

4 with

the

top

of cell No. main. of the in

Connect

with directly

the

water-

Cell No. 4 is now

of the circuit, and If compressed is usual

the firstround

battery is completed.

air were time

employed
a

forcingthe circulation, as
very

each of the The

cell of

juice is drawn
will have
to open

(except the first round


little water
on

left in it.

battery),No. 4 next operation is

air;
and

or

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

the air-vent

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 permit the
to escape of

the

bottom
remove

which

comes

in contact

with

the
a

hydraulic
leak.

jointto
The the

adhering chips,which
of the
commences.

might

cause

first "round"

battery having been


Three
one

completed, always

regularroutine
open
"

cells should

remain

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
one

and filling

series, i.e., the


the

one

which

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-

DIFFUSION

PROCESS.

29

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

juiceshould
at
were

be heated. which the

The United

table following States


at

shows

temperature

Government

experiments

conducted

in the work

tion. Magnolia Planta-

OeUnumber

1
.

(234667)
168"-176"

8
203"

10 203"

11

12

Temp.,

Fahr.

.'.140*

203"

186"

160"

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

juice was
but

no

greater than
cent,

with
was

millingand
diffusers

saturation,

and

0.07 pep

of sugar

left in the exhausted

chips.
was

The

high temperature
by the
which

of the

in this work

necessitated

coarseness

of the
cane was

chips. In the earlier


sliced, not
with

experiments, in
much lower

the

shredded,
a

temperatures
batteries the

were
,

maintained

factory satis-

extraction.

juice is heated into the circulating pipes. This method


In many
the

steam by injecting of heating modifies

of

and manipulations slightly, sugar through leaky heaters.


* advises Prinsen-Geerligs

eliminates

the

risk of loss
^

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
same

temperature

they had
maximum

when

entering it, so
with
a

that

in the
In
coarse

chips no

heat

becomes
a

lost." extraction time


a

order to obtain

moderately
maximum

chips and

at

the

same

juice of

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
""..
" "

J-

"

Cane

Susar

and

the

Process

of its Manufacture

in Java, p. 26.

30

EXTRACTION

OF

THE

JUICE.

the

extraction

in this

cell,and
that

consequently the
enter

less work this cell. in the

for the It is the


a

subsequent portions of thin juice which


well known of the fact thin the

greater the

difference

densities

juice bathing the


the
more

chips 'and
be the

heavier

juice contained place.

in them Due

sion rapidly the diffushould upon ever, had, how-

will take for the the

consideration

effect of high t^nperatures


a

quality of
normal

juice in de";idingupon
a

maximum. of
sucrose

With

constant

percentage draw,
and
a

in

the

juice, a
the

uniform

perfectly regular extraction,


per
cent
sucrose

dilution, and
to

consequently the
vary

in the is

will diffusion-juice, due


seasons

considerably.
per cent

This
cane.

variation In

the

variable

juice-content of the
the in stubble

(in Louisiana)
about the with

juice in

ordinary plant-cane will

average

91, and
same

if we
as we

draw do

amount

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


dilution
vary, cents

stubble, the
two

will
even

be

lower

and

the

analyses of the juices contained


to
commence on

juices wilt
same

though the normal


sucrose.

the work
an

per
a

of of

It is safe 23
per

with

dilution
per

about
of

cent,
cane.

estimating
If the

average

of 90

cent

juice in the
of 90
a

Extraction
too

is

satisfactorybut
cane

the

density
until and cent, there

the
per

sion-juice diffucent

low, the
the draw

contains

less than

of

juice,and
is dilution
to

should With reduced

be decreased thin
to

density
the safe

obtained.
may

chips
18
per

satisfactory regular work


but is it is not
a

be

go

below control With


to

this limit
to

except

when

careful
poor

chemical extraction. economical rather in the

promptly detect and remedy a the best multiple effect evaporation


more

it is

bum

coal to
or

evaporate
tenths been
per

additional
cent

water,
sucrose a

than

leave which

two

three have

of

chips

might

obtained

by

little

hieher The the based and

dilution.

following table, designed


for

for

preliminary work, gives


of

dilution
on

different

quantities
16" Brix

juice drawn.
cane

It
per

is

an an

assumed
average

juice-content in the

of 90

cent,
1.0656

of

density of

(9" Baiun^,

or

specific gravity).

BT-PROBUCT

OF

MILLING

AND

DIFFUSION.

31

5.

By-Product
of the

of

Milling
is

and
or

Diffusion."
megasse

The

product by-

milling cane woody


from

bagasse
cane

nies), colo(EInglish

fiber of the

with

the residual This

juice and
material

moisture

derived
a

the saturation-water. in many

supplies

very

large part and

instances

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.
It has in

frequently been
paper

urged

that Two

these
or

materials mills short


wee

be

utilized built it
was

manufacture. but
were

three
a

for this purpose,

operated only
of exhausted of the diffusion

time,

hoped that such


to the commercial
*

utilization
success

chips would
process.

lead

Havik East

was

commissioned
to
a

by

the Government

of the Dutch and He the other

Indies with
cent

investigate the fibers of Java


view
to

islands
32 per

paper

manufacture.

obtained

of the

weight of dry bagasse in dry unbleached


was

paper.

The stated

bagasse yield of

from per
cent

Cheribon of paper

cane.

The

quently fre-

52

is

disproved by

Havik's

experiments.
*

Int.

Sugar

Journ.,

14, 52.

STEAM

PLANT

AND

FUEL

6,

Steam
in
a

Boilers
cane-sugar

and

Fuel."

-The with

boiler the

capacity

quired re-

factory varies
cane,

manufacturing
of saturation-

equipment,
water

the the

quality of the grade of


sugar

the

quantity
More and

and

produced.
for rich
cane,

boiler for

capacity
facture manu-

is necessary
of

for

poor

than

the

plantation white-sugar than


includes in

for raw-sugar.

If the of the

factory
vapors

equipment generated

multiple
the

application
in the It
a

evaporating
fis

juice, in juice-heating
beet

and its
state

for other boiler the

purposes,

is customary lessened.

industry,
to

requirements
boiler

are

is

customary

capacity required by
per
cane

factory in nominal

boiler
A
a

horse-power large Cuban

capacity-ton. good
not

factory, having
but the in
to

equipment,
other
or

including
of the

quadruple-effect evaporator, utilizing the


vapors

using pre-evaporators
or

or

from

first

pans

multiple-effect evaporator sirup, requires from


per 1 1.25
or

juice-heating
nominal
to

evaporating horse-power
feet

1.50

boiler
square

capacity-ton,

about

12.5

15

boiler
of the

heating-surface.
vapors

Good

mill-work

and

the

utilization
may of

of the these

multiple-effect in juice-heating
numbers. increase The in manufacture

reduce
with

materially white-sugar
for evaporating

its attendant

steam-consumption
increase the
steam

wash-waters,
15 per
cent
or

etc., may

requirements
used

more.

Both
sugar

fire-tube factories.
on

and

water-tube
Cuban their
to

boilers factories

are

in

cane-

Many
of

select The
over

water-tube

boilers boiler

account

greater
an

safety.

fire-tube
the other

is often
on

considered of its

have water

advantage
the

type
meet

account very

large

capacity, which
of

fits it to

the

irregular demands
fuel the of
cane

The residue

usual from
as

the

cane-sugar

factory for steam. factory is the woody Many


instances
The

itself, bagasse.
in many

factories

use

bagasse
is

their only fuel, and in


excess

this material modern


dency ten-

produced
of

of the

requirements.
in

applying

heavy

saturation

milling has

increJtsed'
32

8TEAM

BOILERS

AND

FUEL.

33

the

demand

for steam, with


also be burned.
very

the result that


Where and
cane

coal,wood
is of moderate

or

oil must

often

cost, labor and fuel


low

dear

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. extra fuel is often elimiquantity of saturation-water, This condition frequently exists in Cuba, hence few factories have adopted pre-heaters or use a part of the
cane

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

the sugar sells for a very sometimes bring in larger net less

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
vapors

from

the

cane-shredder.
Cuba

It

was

first used

in Louisiana

and

then

in

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

at ''Soledad"

with the

but

two.

In of the

the

latter

case

the

furnace
was

under in the

front

end

boilers.

Forced-draft

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 after

used

using it in Louisiana.
on a

In in

this
an

type
oven

of

furnace

the

bagasse is burned
two

hearth Air

placed between
into the

water-tube

boilers.

is forced
to

burning
of in

bagasse
the Fiske

through
and

tuyeres.
bumiers

Prior all

the

introduction
was

Cook

bagasse

sun-dried

burning it. The inventions of Fiske and Cook had a profound influence upon sugar-manufacture in Cuba forcing the factories to operate through enabling,and, in fact, 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 fiunace
most recent
were

formerly

ployed em-

(3) The

step-grate grates

type.

In this type there


axe

is usually a

in front

of each

boiler. The

34

STEAM

PLANT

AND

FUEL.

inclined

and

resemble

and in fact step-ladder,

are

often

"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.

Modem

installations of all three types of furnaces is most flat-grate


very

are

very

efficient. The

step-gratesare
those Forced draft is in and often

used in Cuba. The generally efficient with very dry bagasse and are in the Hawaiian

usually used
now

Islands

and

Java.

littleused, since with the vast

ments improveper
cent

the milling,
very

bagasse

usually contains
and

50

much

less moisture

givesgood
"

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. In combustion
tests made

by the results of
in various of

many

parts of the

consideringthe
upon

actual

fuel value be taken absorbed

bagasse

as

it is burned that
a

the grates, it must of heat units


are

into account in ing evaporatto the tem-

certain number and

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 the grates and

quantity
Norris
^

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

additional
Dr. R. S.

for the following figures published

bagasse

of various

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

Moisture Per Cent in the Bagasse.

42

3129 3057 2982 2909 2835 .2762 2687 2614 2540 2468
"

43
44

45
46 47 48 49

60 51
'
"

"

Bui. 40, Hawaiian

Sugar

Planters*

Expt. Sta.

an

outline

of

the

customary raw

method cane-sugar.

op

manup;acturing
The

Introductory.
the define
many

"

purpose

of

this

outline

is to

imize min-

repetitions in future
of the with States described of technical

descriptions and
at

especially to
time ing illustratthan The in

terms,
Terms in

the

same

them the United


are

examples.
are

used

elsewhere

included
a

parenthesis.
part
"

esses proc-

in full in the

subsequent

of the

book.

7.

Outline
"

Manufacture.
or

Purification of the juice is


plished accom-

Juice,

^The

defecation of lime

clarification and heat.

of the The

by
is neutralized
to

means

acidity of the
is then

juice
raised

by milk

of

lime, its temperature


or scum

the

"cracking"

point,

usually

little below "brushed" "clarified" number

200** off

F. the

In

Louisiana

practice the
the

is often is then

juice after heatinij and


and continued

latter

ing by boilof tories fac-

brushing.
defecation and decant

The

greater
settle the the

using the
tanks after

process

juice in specisd liquid


or

heating,
from The the mud is mixed in the

clear
or

fied "clari-

juice"
cachaza).

"mud,"
is with
press,

"sciun"

"slops"
the

(Cuba="
filtrate
or

filter-pressed and
the clarified

"press-juice"
retained

juice.

The
are

tates precipiused in

"filter-press cake,"

fertilizingthe fields. Evaporation,


vacuo
"

^The

clarified

juice is evaporated
mdadura

in

partial
=

to

"sirup"

(Cuba,"

^;
per

beet
cent

industry
of water.

thick

juice), containing approximately 45


"

Crystallization, ^The single-effect


vacuum-pans

crystallization is
under reduced with in

accomplished
pressure. sugar.

in The

sirup
point
The
water upon

is

evaporated
or

imtil

saturated

At

this
mass.

crystals
pan

"grains"
with the

separate

the
to

boihng time,

is

"charged"
and

sirup from
it contains

time is

as

the

evaporates,
the

sugar

largely deposited
of additional form

grain present
Should
^

without

the. formation

crystals.

additional
Pronounce
**

crystals, "false-grain,"
May-lah-ddw-rah.'!

36

OUTLINE

OP

THE

MANUFACTURE.

37

through carelessness
prevent
mterference

or

otherwise
a

they must

be remelted

to

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

dense
the
^^

mass,

"massecuite/^ (beet industry


=

and fill-mass) This

strike'^ is then
a

dischargedfrom
"

the pan.

latter is often termed

^'strike'' pan.

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

velocity. The
may

are sugar-crystals

retained

by the liningand
The mother

be

washed

upon

it with

water

if desired.

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

is "cut

down," crystals before,


This "final

ready for another leaving the centrifugal


The and molasses the is reboiled
to

charge of massecuite.
second
crop

obtain is

of

"second "second

massecuite"

centrifugaled as
molasses."

yielding
molasses

sugar"
and
or

and

"second

is also reboiled

yields"third sugars" and


"third molasses."
modem At
a

molasses," "black
The
processes

strap"
followed is here

in the

factory
certain
pan

are

more

complicated
the of

than

indicated. is

stage of
instead and it

"pan-boiling" molasses sirup or is said


increases the
to be

injected into the


or

"boiled-in^'

"boiled-back"
In

thus modern and

output of high-grcidesugar.
one

fact ths
sugar

factory usually produces but


Construction.
^A

grade of

final molasses.
"

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

Factory Design and

large Cuban

"

"

MANUFACTURING

PROCESSES.

PURIFICATION

OF

THG

JUICE.

8*

Pariflcation
"

of the

Juice.

General

Consideraas

ttons.
beeu
upon
are

The

juice is first thoroughly strained


on

has

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

described

dependent
and

heat

in raw-sugar facture. manuexclusively 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 almost and heat is then

appliedto

temperature

littlebelow

94"

C.

(201" F.). A
scum

matters

is thrown down and thick heavy precipitate rises to the surface of the juice. The albuminoid and coagulated largelyrise to the surface,and are with the lime to form
wax

the acids combine salts. in the and


in
scum.

soluble and

ble insolu-

The

fat and The

clean This

included part of the gums are juice b separated by subsidence the defecation
process,
or

and

decantation.

is termed

some

localities the ''clarification''of the

juice.
of

A sugar

modification

of the

carbonation

process

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
An 1886

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
from the usual
one

in the addition the

viz.: to the juice and


"

stages, sirup (concentrated juice),each


Bureau of

of the lime at two

See

report of the

Cbemiatry. 38

CLARIFICATION

WITH

OPEN

TANKS.

39

addition
and

of lime

Both juice being followed by sulphitation.


or

be filtered sirup may by decantation. above used


recent

the

precipitates may

be

rated sepa-

The those A

of them processes and slightmodifications almost exclusively in the cane-industry.

are

patented
power

differs from

prpcess for white sugar, by Wijnberg, all others in Rising carbon of great a decolorizing called ''Norit." The carbon is then is added
to

bleaching
the

acid slightly

defecated carbon
cent

juice,which
solution
a

boiled and

The filter-pressed.

(press-cake) is revivified
of caustic The soda and kiln.

by

boiling with
with A

5 per

sionally occa-

by rebuming

it in

sirup is filter-pressed
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
the the Steffen
sugar

kieselguhr. differingradically from process,

saccharate-of-lime the molasses.

process

in the

recovery

of
as

from

The

saccharate

is used

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

Lippman's is given on
In the
none

list of
page

these, comprising

more

than

600

entries,

532. of the juice is purification long enough to destroy to avoid decomposition at

high

of the processes for the maintained temperature


care

spores,

hence

is necessary

later stages of the manufacture.


9.
"

DeTecatton

and

Clariflcatioii

with

Open

Tanks.

^ThiB is the process


the

in general use
of the
cane-sugar
.

and

has been

practbed
little

since

early days

industry,with
mill-tanks The
outer to

improvement
The bottomed of the As
soon raw

until recent

juice is pumped
vessels termed

years. from

the

doublebottom iron. with acids

''defecators.'* and the

inner

defecator, is of copper
as

shell of

the

bottom

of

the
to

defecator it to

is covered the

juice,milk
and
steam

of lime is turned

is added Into the

neutralize between the

space

bottoms.

40
The time workman the

MANUFACTURING

PROCESSES.

regulates the
its

steam-

defecator

is filled with

pressure juice the

so

that

by

the
have

latter

will the

nearly reached
scum

boiling-point.The
surface
'*

moment

thick is shut
of

that the

covers

the

cracks"

the

steam

of! and

juice is left undisturbed


lime

for the

subsidence

impurities.
If the
as

quantity of
be

required has been


on,
a

properly gauged,

will

described
surface
to

farther the

part of the

inapurities
''blanket,"
and acids

rise to. the and


a

with

sciun,

forming the

part settle
action forms

the bottona heat

of the defecator.

The the
of

of the

coagulates the
and soluble

albiuninoids
the

lune the

insoluble

salts with

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 bottom of the of the

defecator,

blanket

of

sciun

at

the

surface

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

and

breaks, in the efforts of the air and


"crack."
are

gases

to

escape,

it is said to defecators

Several
are

usually arranged in

series

and

filled with time after

juice in
the the
bottom

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

drawn

off from

and the

sent

to

the

the filter-presses,

clear

juice is

into

evaporator
scum

charge-tanks
to

or

into

and clarifiers,

the finally

is sent

the The

presses. proper

skill. liming of the juice requires considerable is used, the impurities settle slowly, the If too little lime and the subsequent clarified juice lacks brilliancy, 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
raw

sugar

the

lime
no

should
more

be

added

so

long
In lime

as

it produces certain than

precipitate,but
dark-colored

should

be used.
more

making
is used

sugars,

however,

is

required for the clarification of the juice. This to the yield of sugars. prejudicial
In the manufacture
of

is undoubtedly

white

or

yellow clarified sugar

CLARIFICATION

WITH

OPEN

TANKS.

41
ft

using sulphurous acid, the


to neutrality to litmus

juice should

be

limed

nearly
and the

paper.

The motion tube


man. are

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

glas^test-

usuallysufficient guides for an experienced defecator The of suspended matter should move particles
the surface of the

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

solution

or

other

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 indicates
tors may
to

methods

be

approximately correct;
been
eye

two

or

three the

defeca-

have

filled before

he

can

heat lime

first and others.

from

it, by the
means

only,
paper,

gauge

the

for the

he can test the juice daylight, 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. visible by artificial light. color reaction is plainly The in raw-sugar In liming juiceto alkalinity, work, samples of

By

of litmus

in

defecated time
to

filtered through juice, time If


a

paper,

should

be tested of

from
a

with

solution

of

saccharate

lime, in

test-tube.
more

precipitate is produced by the saccharate, lime should be used in the defecation,and, vice versa,
is
no

if there

It is the

the lime should be reduced. precipitate, usual practice in Louisiana to use the same tank, coils and The

fitted with
and

darifier. that the

steam-jacket, as both defecation is accomplished as


not
a

defecator above the


cept ex-

blanket

is

immediately removed
at the
same

and time

juice

is then

boiled

the workman briskly,


scum

ing'^ "brush-

off the

that

rises.

This

latter part of the process

42

liANUFACTURIMO

PROCESSES.

is

properly termed
is

the

''clarification/' though in Louisiana


the

this word

applied to
eliminators

entire process.
process
as

In addition to the defecation clarifiers


or a are

already described,
and

frequentlyused.
steam-coils the defecators and is then

darifier is The where tanks. clear

tank

fitted with from skimmed

juiceis drawn

ordinary a mud-gutter. into the clarifier,


run

The

it is boiled and

into

settling-

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

is

usually sufficient.
It sometimes
occurs

clarification will not


or

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


that

the

subsiders.

but with
upper

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

This

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

or

usually cause
is
scum more

spraying of the surface with cold water, will Cold water the impurities to promptly settle.
of the juice. The stirring rise of the is

effective than
to the surface

probably due

A the

modification

of the defecation

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

In

oonneetion

with

the

diffusion process
the diffusers.
to the

the
The

defecation

is sometimes

in accomplished is added

requisite
to

quantity of lime
the

cane-chips on
at
a

their way

battery, and
to

the diffusion is conducted

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

44

UANUFACTUBING

PB0CBS8B8.

juic" entering the


toward about
4

tank

at the

rear

t^nds

to cany

the mud
of copper

ward forand

the outlet.
in

The

coila should

be

inchcfl

diamel^ feet
of

and

should

provide
per tank. tank
to

imately approx-

25

Bquare actual

heating surface
in of the

1000
Hie

U.

8,

gallons
should
the

of be

juice capacity
the

coils

well above
of the mud.

bottom

the

facilitate

removal
writer

The

prefers

rectangular

drfecating

tank, with

Fid.

11.

rounded
below.
now

comers

and
tanks
a

the draw-down
may

arrangen^ent

described

These
use

be of very
in

large capacity.
excess

Many
gallons.

in

have

woriiing capacity
requires
of
a

of 6000 time for

While it has In
so

deep

tank

rather

long

settling,
of mud.
cot^

the advantage tar


as

yielding a small proportion


through
is shown

possible, it is preferable that the juice be


the

veyed
The nde

from

ddecators

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

than

draw-down

arrangem"it with
a

AtAiaa, the

outlet'^lbow.

above ventilating pipe,F, lekdiug

CLOSED

HEATEBS

AND

CLOSED

SETTLERS.

45

drawing down, the juice flows through the nipple,the elbow, A, and the cross valve,B, into the small and thence to the trunk line,D7~ The anglecollecting-box
In before drawing down the valve, C, is opened for a moment that may have settled in the juice,for the removal of mud that may be near the outlet-nipple. The valves, or pipe-line

top of the tank.

B, C,

are

controlled in

from

the

working-platform H,
into the main

The

valve
scum

G is used

washing the mud

line to the

It will be noted that the pipe is ventilated to tanks, E. prevent sjrphoning and that the juice therefore stops flowing when its level reaches
no

that

of the bottom down. from


or

of the draw-down elbow the and


scum.

pipe and
advisable each

mud

can

be drawn

The below

nipple
It is

insure that
to

juice shall be drawn


locate about three

four

draw-down
4

with difference of level of about defecator, between


centers.

pipes in inches,measured

The

inches should of
4000

above

the bottom 3.5 inches

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


in internal diameter in
a

lowest

be about

defecator

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
"

and
is

made

it available

adaptable to The juice is limed

practicalwork. factories of all capacities.


in the cold in

in

This

method

Deming's
lime is

process,

in

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

flows

into

the

thoroughly mixed
The limed is then

and

in transit to the heaters. F. and the cold

approximately 235"
it parts with the

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

eliminator,where concentrated, and warms

gases,

passed is slightly

46

BfANUFACtURING

FROCBSSBS.

through the tubes and condenses the


hot

steam

set free when A the

the
tial par-

juice enters
vacuum

the lower

section

of the eliminator.

'Is
gases

produced by
are

this condensation from the hot


a

and

air

and
upper
vacuiun

other

withdrawn

juice. The
pump
or

part of the eliminator system. temperature


of the F. in the eliminator.

is connected

with

the

The 210"

juice should be reduced here it is pumped From


compartment,
or

to about

into the

outer

A, of the closed

ii

settler

pressure-separator, shown

A
^

I
^

diagrammatically in
mud is drawn the conical and the bottom

Fig. 12. The oflfcontinuously from


of the tank
at

the clear central

juiceis discharged from


cone,

B,

In

many

tories fac-

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


212" In
to 218"

F.

his first

experience with
of their noted that

these in the

^^
W

j_.

tanks, the earUest Cuba, the writer


mud drawn

type

//
^/

ofiF after several

hours'

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

in the tanks

to

prevent the
the and conical thus

mud bottom

from of

settling on
the

separator
resist the

nearly
Fig. 12.

eliminated
spores

decomposition.

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. and defecators usually The heating-smfaces of juice-heaters incrusted with scale,impairing their efficiency. become soon

Certain

The
are

of copper-surfaces

the

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

SULPHITATION

PROCESS

OF

LOUISIANA.

47

localities that the laborers


with brushes. with In
water

are

unwillingto clean the defecators


copper

this ev"nt, the

bottom

should be

.covered and

acid strongly acidulated with hydrochloric the solution boiled. Five to six pounds of the commercial
are

muriatic acid

for use usually'sufficient

in

cleaninga

1000-

gallon defecator. of coiMefecators "The heating-surfaces


with whole

used Those

in combination in which the

juice-heaters foul
defecation
process

but is

little.

conducted is used

require frequent
in
as cleaning,

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

muriatic

acid

in

defecator.
may

When

the

coils

be

cleaned

by drawing
usual method

lightchain

over

the surface.

Juice-heaters usually foul very


of the

quickly. The
and
may

cleaning is
tubes and muriatic

to

circulate hot

caustic-soda

solution then be

through
with hot returned

follow acid.

this first with water


The soda solution

dilute
to
a

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. 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.
DEFECATION
IN

WHITE-SUGAR

PROCESSES.

12.

Sulphitation

Process

of Loulsiana.-^This

is

one

of the

and when fully skillsimplest of the sulphitation processes conducted good, though irregular, produces a very "near-white"
or

qualityof
The cold

"off-white"

sugar.

raw-juice is pumped
to

box, in opposite direction


acid gas
as

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


absorb
as

gas.

The

juice should

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 is

48

MANUFACTURING

PROCESSES.

is

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

wasteful

process,

since

it entails

phited.
This is
a

very

old process,

and
It

English or French colonies. has always been the custom


sensitive condition acid litmus
to

possibly originatedin the is interesting to note that it


the

to work

juicefaintlyacid* to
of

prevent

coloration
one

the

sugar.

This Java

corresponds to the essential


(Louisiana) White-Sugar
with
of

of the recent

thin-juice process.
Process.
"

Reserve is very

The

raw
a

juice
tical ver-

strongly impregnated cast-iron sulphuring-box


3 feet cylindrical,

sulphurous acid in
the cascade
26

type.

The

box box

is

in diameter

by

feet

high. This

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
The

has sufficient

juice is

next

heated

in

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, neutral to htmus. and is then strictly Phosphate of soda at the to the juice flowing into the settling-tanks 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 flows

mild

The filtrate from the filter-pressing. 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

to

acidityis raised
The clarified

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
in

white-sugar manufacture.

SULPHITATION

AFTER

LIMING.

49

The

high acidityof the juice as


work is

compared with that


As

in

Harloff*s

quite noticeable. practice.


"

previously stated,

this is usual in Louisiana


13.

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

Sulphitation

after

gallons of milk of lime of 26.5** Brix is used, with the sulphurous thus producing a very heavy precipitate 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

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

sulphitationis continued

An

acidity equivalent to that required in


25
to

10

cc.

of
a

sirup

to

neutralize
amount.

30

cc.

of 100th

normal

alkali is

suitable

Bachused Lime in

Sulphitation Process.
under and is

"

This of its

process

is

extensively
H. Bach.

Java,

the patents

A. inventor,

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 settled and the clear juice decanted in the to full boiling, as The clear juice is evaporated to the ordinary defecation. density,approximately 55" Brix. customary
The cooler

is added

sirup obtained
and

as

above

described
to

is

passed through
that

its temperature

is reduced
16 to

about

of the
of

factory's water
lime
per to

supply. From 1000 gallons are now

17
to

gallonsof the toilk


it and it is then

added

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. the total volume of milk juice, per cent of that of the original 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^

50

MANUFACTURING

PROCESSES.

C.) and (90**


water

is

The press-cakeis washed filter-pressed.

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 well formed. The filtered heated

sirup contains
to about

some
**

bisulphiteof lime and

is

therefore

195

F. to

decompose

this and

other

bi-sulphites. The tanks, and liquoris decanted

sirup is usually run into settlingafter the deposition of the precipitates the clear
and cooled
as

heated

and previously,
to

is then

sulis

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


Bach's all of the
process

phenolphthalein and

is sometimes

modified slightly

precipitates by decantation and pressingthem together. This process requiresapproximately 0.055


on

by separating mixing and filterper cent


are

phur of sulof

the

weight of the

cane.

The

sugars

good

quality.
CARBONATION

PROCESSES.

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

processes
even

has in S.

retarded

an

extension it has

of the carbonation its

ess, proc-

Java, where

largest application.

The

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 U.

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

of carbonation

temperatures

well below

60"

There

are

two

distinct

carbonation lime

processes,

viz.:
one

the

in which single, and twice lime

all the added

is saturated the

in

tion, opera-

the double the


gas.

carbonation,in which
In and the double removed carbonation

juiceis treated
a

with

process,

part

of

the is

is carbonated

by filtration and
in which the

this

followed

by

second

remaining

52

MANtlFACTURING

PROCESSES.

forming the
lime that and

carbonate the

and

then

forms

sucrocarbonates It is at the

of

renders

juice very
is

viscous.

this stage increase of

foaming begins and


There

it increases

with

always danger of forming darkcolored decomposition products with the glucose when steam
sucrocarbonates. is used excessive be
very
to

beat

down

this

foam. which

Further

there

may

be
to

rise of temperature,

will later be acid

shown

objectionable. The
the lime. The

carbonic sound made

bines 4;raduallycom-

gas
to

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

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

is

gradually raised
(Dupont
C. break
to 70" to

to 65" C.

lein paper heated order

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

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

filtration of the

juice. The

attendant

may

note

approac"ing

the appearance of the neutralityby the "spoon test," i.e., 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

as

often

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

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 to this paper is reached. (Dupont paper) until neutrality paper The bonated juice is then heated to nearly 70" C. and is over-carand sodium

during
the
on

very

few lime

seconds that has

to

neutralize been

the

slight by

alkalinityarising from
carbonic acid. In

not

attacked

practicingthe
must

carbonation for

process

beet-juicesallowance
due
to

than

lime,

to

avoid

alkalinityother over-carbonating. This is not

be

made

SINGLE

CABBONATION.

53

usuallynecessary
occasional for it. The next
tests

in
for

cane

work, but it is advisable

to make to
rect cor-

potash alkalinityto be prepared


is the

stage of the process


with Thin

The filter-pressing.
as

dressed are filter-presses defecation


over

heavy

cotton-cloths
are

in the

process.

cotton-cloths

usually placed

Three suits of heavy cloth to protect it from wear. heavy cloth are usually consumed per five suits of the thin. the Steam is turned into the
press

before the

use

and

is not

shut

off until it escapes of this

freely from

juice-cocks. The

object

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
up to

steaming

is to

about

45

lbs. and
very

should

filter very

rapidly.

The

juice should

flow

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
of the filter presses is the best indication of correctness of the in

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

manipulations.
the press
page
to
a

The

filter press-cake is
content.

usually washed

low

sucrose

(See under

filter presses,

67.)
filtered

The

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


Single Carbonation
Process.
process
use

sulphitationprocess.
De Haan's
"

This
to

important
J. S. de

modification

of the

carbonation

is due

Haan,
This

Klaten, Java, and. is in


direction. reduces the
process

in several

factories under

his technical

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

of milk

of lime into

and it.
as

the The

carbonic-acid flow of the


an

gas

are

taneously simulgas

turned

lime

and

is

carefully regulated so to very closely


has 35.7" been Brix

to maintain per cent

0.25

alkalinityapproximating until all the lime required


of the

added.
is from

The
4 to

usual
5 per

total
cent

quantity of milk of lime of


of the volume

juice.

54
*

MANUFACTURING

PROCESSES.

Approximately
are

20 tons
tons

of lime-stone and
of
cane

1.8 tons

of

gas-coke
to

used

p6r

1000 gas.

in

producing the lime and


is
now

carbonic-acid

The
paper gas

carbonation and the

continued

neutralityto Dupont The injectionof the


is reached.
to

juice is heated
one

to 70" C.
trality neu-

is continued

rainute after

The

object of this over-carbonation


that have
not

is

prevent particlesof lime


the carbonate from

been

converted and

into

r^idering the juice alkaline

it. discoloring The juice is

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
are

Carbonatioii based upon the

Process.

"

^All carbonation
process
as

methods in in

original French
double the
process

used

treating beet-juices. The


cane

applied
method

factories

differs from

modem

beet

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 which is warmed to the juice, 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 alkalinity than 0.04 per cent. With this alkalinity there is no danger of redissolving parts of the the juice filters very precipitates, freely and sufldcient lime
is left for the second Lime the
may
or

carbonation
not

or

saturation.
to

may

be added

the filtered the

juice from
This

first carbonation

preliminary pushed

to

saturation.

juice usually contains


error, the

sufficient lime
too

except
far.

when, through
The second
car-

gassing has been

harlopf's
.

acid

thin-juice

process.

55

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 of caustic lime that may particles precipitates. The saturated of the condition of the juice,on account is precipitates, filtered under
very
are

low

pressure.

Gravity

filters or
purpose

shallow with
a

frame-presses
of but

pressure

to

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


is the
more

The
means

filter press of

with

gravity pressure

economical

The

filtering. object in conducting the

process

in two

stages and

the stronglyalkaline juicefrom the firstis the removal filtering that are in neutral solution. of substances or soluble; slightly so Among these substances are magnesia, usually largely

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

derived

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 carbonates the potassium sulphites and especially 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.
summer

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.
of 1913,

56

MANUFACTURING

PROCESSES.

Of most darken

do not importance, Harloff ^ found that sulphites clarified juice containing glucose on heating and that do.
as

carbonates in
BO

This be

led

to

the

natural be

conclusion converted

that into

far

may

all the

salts should

them. He sulphites,since it is impracticable to remove accomplishes this by sulphitingto neutralityto litmus,which corresponds to slightacidity to phenolphthalein. Further, iron if present in the salts, These salts
raw

or

carbonated

are juice,

in

the ferric state. in


so

are

reduced
are

to the ferrous

state

juicesby the sulphurous acid and


in acid solution. from be The ferrous the sugar
cannot

colorless and

remain

salts do not

out crystallize

with

acid solution.

Litmus

conveniently used
poor,

at

night

or

when strument in-

the

lightis

and

therefore,is an
of
a

uncertain

in recommends which work. is

the the

hands
use

laborer.

Harloff

of the Vivien

employed largelyin France


tube is filled to the

tube. Fig. 13, in beet-sugar


mark with

The

zero

25

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
is 10 of the scale
on

the Vivien

tube and

smaller

20

"

15=

10

"

5 =

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 is tube, Harloff the

0==^

recommends
not

that

the

juicemixed
to
a

with
perature tem-

be precipitates than 90"

heated

higher

C. (194" F.) in closed

heaters

Fig.

13.
on

account

of

ing foulingthe heating-surfaces.Heatshould


a

above

this temperature the custom


an

be in open
many

tanks. in Louisiana this condition


Manufacture,"
a

It has been
to

for

great

years

work
"W. H.

with
Th.

acid
Harloff'8

juicesimply because
"Plantation should be White consulted
cane

with
Sugar
for

Norman

Rodger,
of carbon

London,
and

very

thorough

study

ation

sulphitation in the

industry.

WIJNBERG^S

NORIT

PROCESS.

57

and the color of the sugar is better,


idea
very
as

apparentlywith

no

definite

Harloff's investigations show why this is true. clearly why the sugar is better.
to

HarloiT

calls attention
on

to

the. corrosion

of the tubes

of the

evaporators,
to

the

vapor

side, when
that the

the
return

juice is left acid


waters
are

litmus.

He

also states and

acid ers. boil-

under

this condition The

damage the tubes of the


water

steam

boiler-feed

should

be

rendered

slightly

alkaline with soda when


18.
as

Wljnberg's
the

is practiced. sulphitation * Norit Process. The juiceis defecated


"

ordinary raw-sugar except that lime is process, short of neutrality. Ten per cent or more added to slightly 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 filterin

pressed. The
boiled with
a

cake
5 per

is sweetened
cent

off

as

is usual

and

is then

caustic

washed washed, and is finally norit is then ready for The norit with then is rebumed in
a

solution,filtered and with diluted hydrochloric acid.


After several
uses,

soda

re-use.

the

kiln.

norit is filtered with

sirup from juice treated the addition of kieselguhr and is


sugar.

The

ready for boilingto white


is
a

Norit

carbon

of very

manufactured

color,but
19.

by a secret large part of the


upon

high decolorizingpower It not only process.


gums.

and
removes

is

Remarks

White

Sugar
sugar,

Processes. with few

"

Factories

producing plantation white


make
a

ceptions, ex-

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
or

"near"

"off"

white

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.
.

Sugar
to

Journ., 1912, 720;

1913, 248

and

404;

1914, 488, all

relative

patents.

58

MANUFACTURING

PROCESSES.

sulphitation processes.
processes.

The

latter are

usuallythe cheapei
purity of the

There

is

marked

rise in the coefficient of

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 and more than justifies the increased sulphitation over processes
cost.

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

is considerable 'difference of

in the

carbonation

and

Bach
sugars

processes.
are

It is very produced from the attention manufacture. A

probable that the canes. light-colored

best white

Great
sugar
or

to detail is essential to successful white-

Uttle carelessness in the carbonation

and filtration will result in a poor product. sulphitation Double reduces purging of the sugars in the centrifugals the risk of staining the sugar through the necessarily imperfect removal of the molasses. Thorough cleanliness from not only from the point of start to finish is very essential; view of color, but also of yieldof sugar.
SPECIAL APPARATUS USED IN THE SULPHITATION AND ATION CARBON-

PROCESSES.

20.

Sulphur
stoves
are

Stoves of two

or

Ovens

and

Sulphitors.
"

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 sulphurouaacid gas under
pressure.

These

These

are

used

with

all types

of

sulphitors. 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 from shelf to shelf in the box. The surplus air and falling
k

In the first type the draft is

60

MANUFACTURING

PROCESSES.

The with
many

usual the

Louisiana

is described sulphitor
stove.
one

in connection
are

induced-draft

Sulphitation tanks
is
a

of

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 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 test.. It and tank overflows and
enters

forms, but the usual provided with a cover

the

second

tank

at

the bottom the second

ife sulphited to the required acidity. From


the

filtersto
21.

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


"

Carbonation-tanks. should be
more

The
20

carbonation-tanks
feet in

are

of

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

iron and

than

requireabout
for the

ten

minutes

and

second

about

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

three to five minutes

Continuous of the process.

carbonation The
a

is advisable

for

the

second

stage
is very

quantity of lime
suitable device

to be saturated

email

and

with

the

outflowing juice is

LIME-KILNS.

61

readilycarbonated
continuous

to the demred
on

point.
in many

There

are

several

carbonators

the market

d"signed for beet work"


works
on

Descriptions of them
sugar.

will be found

beet-

If intermittent
may 22.

second

carbonation
as

be

comparatively shallow,
Ume-kllns.
"

practiced,the tanks there is littlefoaming.


acid
a

is

^The

carbonic
in

is obtained

from

lime-stone This

calcined by coke-fires
also the all other identical

specialcontinuous
and
are

kiln.

kiln, as
are

carbonation devices that

sulphHation
used in beet-

machinery
sugar

manufacture.

The
a cone

kiln proper of
narrow

is 25

to 30

feet

angle with
and
coke

high and is the frustum end the small upward.


is fed into the kiln at
zones

of
A

mixture

of lime-stone
a

the

top through
are

conical

maintained

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

stone

and
and

unignited coke; (2)


dissociation
zone;

the

middle the

is the

combustion is
'

(3) below

combustion-zone drawn off.

that in which Kilns


are

the resultant

lime is cooled and

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
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 firing and the lime is produced this stone As progresses is removed from its place is tak^i time to time and finally
upon
a

concrete

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,
-

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

is located

the The

pump gas

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


have but
one

which

The the

kiln must is

inlet for air,and

that

where

lime

discharged. The
pump.

quantity of air drawn


that this pump

and, in,"
of the must

therefore,the combustion, is regulatedby the speed


carbonic-acid
It is evident
must

be

kept in thorough order and

work

with

great regularity.

62

MANUPACTUBING

PROCESSES.

since the
zone

sucoeas

of the
must

carbonation

depends

upon

it.

The

of dissociation

be maintained
are

in its proper
gas

place.
ing contain-

The

essential conditions

the

deUvery of rich
acid and

above
lime.. The 276* The
gas

30 pet should

cent

of carbonic

properly burned
described
in 275,

be

frequentlytested
stone

as
^

The

qualityof the coke and

must

be controlled. will assist

of kiln conditions following brief summary in the interpretation of analyses:

(1) The
is indicated

gas

oontainB
a a

large excess
the

of

oxygen,

little

bonic car-

oxide, and
at

low

percentage
between is white
coarse.

of carbonic
gas-pump

acid: and

Leakage
the kiln.

point
zone

If the combustion
too

fast

or

the coke is too

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

increased.

(2) The
carbonic of lime

gas

contains, too
nor

little carbonic add is excessive: Smaller

and

neither

oxide should

oxygen

quantities

be drawn and coke

and should

at

of stone

The mixture longer intervals. be investigated, the proporas tion

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

acid is

be

running
an

too
excess

slowly

and

fluctuating: irregularly.
oxide of the and
mal nor-

(4) The

contains
oxygen:

of carbonic combustion is converted other the pump

quantity of incomplete and


on

The acid

coke

is

carbonic

into

monoxide

account

of

deficiencyof
too
coarse

oxygeu;

conditions

normal, the coke is


fast.

and

being is running too


oxide in

(5) The
excess:

gas

contains

both

oxygen

and

carbonic and the

The
some

circulation air.

of the gas is slow

sampler is high-grade
coke
gas-

drawing
The

American

beet-sugar factories usually


in their kilns. The

use

metallurgicalcoke
has coke forced and the

high

cost of such

Java

factories to substitute The residuum Coke

the

cheaper

oil-still residuum.

is used is used

in the in ratio

ratio of 1 to 12 of stone of 1 to 9.6-11


^

by the weight.

of stone.
Book for for

See

"

Hand
p.

Chemists

o"

Beet

Sugar
and
a

Houses,'*
discussion

G.

L.

Spencer,

211,
Also

qualities.

analyses of analysis of lime-stone,

lime-stones this

of their

work,

p.

386.

FILTRATION

PROCESSES
"

AND

MACHINERY

23.

Filtratiop.
the that the

"

In

the

usual

processes

of
not

cane-sugar

manufacture but

entire

clarified contained With

juice is
in the

filter-pressed,
and

only
from

portion

scums

tates precipiprocess

defecation.
may

the

carbonation

all

of

the

juice
The fine

be

readily filtered by
the
which

through
defecation
soon

ordinary
process

presses.

juice

clarified
matter

contains
pores

flocculent cloth.

obstructs
upon

the the

of

the
of

Several

processes,

depending
to

addition

sawdust,
to

lignite,charcoal, etc.,
filtration,have
In
may

the

clarified
none

juice preparatory
has been

been the be
a

devised, but
Bach

practically successful.
both
the

sulphitation

process,

juice and
in the

sirup

filter-pressed. The filtering medium


as

precipitated calcium
does In

sulphite supplies
carbonation
filters mechanical

the

carbonate
years,
or

processes.

recent

of

many

types,
been used

using
with

sand,

cloth,
success.

other Sand filters but


were

filtering media
filters

have

varying
white

apparently
used

give good
in

results.

Bone-black
sugars,

formerly
have been

making

plantation
the

these

displaced by
be this

ous-acid sulphur-

processes.

The

scums

and

juice tank-bottoms
to

may

easily filtermaterial the in

pressed.
steam

It is advisable settle
to

thoroughly
the

heat and

"blowups,"
preparatory
and

mud,

decant is
a

clean in

juice
sugar

filtration.
filtration

There

gain

both

facility of

by

this

treatment.
to

There residual the


when

is mud

an

additional and

gain
The

of sugar and

by adding

water

the

again

heating
mud

settling it, and usually


"

decanting readily

thin

juice.

filter-presses more
should be Filters. Cloth the

alkaline,
24.

therefore

lime

added filters

to
are

it. of two is from

Mechanical
viz.
:

Cloth

kinds,
the

(1)
the

Bag bag
the

filters,in which outward;

filtration
or

inside

of

(2) mechanical
the outside

gravity
the

filters, in which
inside
of the

filtration

is from

toward

bag.
63

64

FILTRATION

PRQCESSES

AND

MACHINERY.

Bag
in
outer

filters are

used

largely by
The mud

refineries and

but

little of
an

Each sugar-factories. and in the


cent
or
an

element filtering

consists

inner
case more

bag.
of

collects inside the contains about

bag,
80

and
per

of

sugar-factory work

juice. Unless
a

this mud

is washed
sugar

in with

the

bag it is evident that there is


filters
are

large loss of

these filters. Mechanical


of not very

tion satisfactoryin the filtra-

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 second

carbonation, but
low
pressure
are

presses
more

using shallow
economical.
of
a

frames

ing work-

under
The

mechanical

filter consists

large niunber

of rectangular

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

the

inside

of it.

metal

distender

prevents
into and

the

bags
filter

collapsing. The clarified juice flows by gravity,under a low head, fillsthe box,
bags.
time is not The
to

the

filters into

the
from

mud

collects falls off.

on

the

outside is

of the
so

bags and
that the cloths mud is

time

The

pressure

low

mud
become
sent

to

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

the the

25.

Sand

Several
As

types
the
name

of

sand

filters

for

juiceand sirup are


the
may medium filtering

use.

of the filter implies, Pulverized


must
soon

is fine, sharp sand. The material filtering the filter will


is

coke

also be

used.

be

of

grains juice

of uniform

size,otherwise
the

dog.
mud sand the is then

When

it contains

medium filtering is displaced with

clogged with
and the

water

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

filter is

again ready for service.


been used with

These the have

filters have

moderate
a

success

in
ago

cane-industry. Many
been converted
26.

of those

installed

few

years

into the

excelsior filtersdescribed

below.
"

Excelsior
"

Filters, Bagasse
excelsior filter was

Filters, etc.
devised

sior Excel-

Filters.

The

in the Hawaiian

EXCELSIOR

FILTERS,

BAGASSE

FILTERS,

ETC.

65

Islands
2.5

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

2 inches

above

its bottom.

for bringing clarified pipe-line

jiice to the filter is connected


tank's bottom
to break

with

it at the
a

center

of the

and

over

this inlet is placed

the force of the current

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

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

small

approximately
1000
tons

150

cubic

feet of excelsior

is necessary

per

of

cane.

materially improve cloudy juice If the juice caused by defective Uming and defecation. has been properly limed and heated, but carries suspended
These
not
matter

filters will

and

the filterswill greatlyimprove it. cane-fiber,


of

An

advantage
or

the

excelsior

filter is its freedom

from

fenrentation excelsior may

serious

be washed and used


"

over

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


filters are constructed in

clogging with

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 This material the has
a

Fillers.

These

the filterand

put upon
ferment For than used

the mill-

great tendency

to

and this

thus
reason

contaminate
it is
a

much

juices during filtration. less desirable filtering medium


"

excelsior.
to
a

Fiber extent

Filters y etc. in
a

Various

fibers

are

limited

way

similar to
a

excelsior.

Thin

sheets

of paper-

pulp
used

have

found

small and

Granulated applicationin sirup-filters.


many

cork, asbestos
and with little

other

materials

have

been

success.

defecation
treatment gums.

process

cannot process

sirup by the be readily filtered, except after


that will

Cane-juiceand

by

some

largely remove

the

66

FILTRATION

PROCESSES

AND

MACHINERY.

In ft very in

old French

process, alcohol

was

used

as

tant precipiculty. diffi-

sorghum-juice. Filtration
The U. S.

followed

without
^

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 the basket. in having no perforations The defecated of the mud juice without previous removal juice or even
"

(cachaza) is
basket. the The

run

into

the

machine
to

near

the

bottom

of

the

mud

is thrown

the

wall

of the
over

basket the rim.

by

force and centrifugal


cost

the clean and

juiceflows

The

of the

heat, oil, etc., are

plant possiblythe

the expense
reasons

for power, loss of for the small extension

is good and the separaIf the defecation of this process. tion therefore sharp, the centrifugals of the precipitates will

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

clean clarified

plates and

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
or

frames

recessed

and

side-feed

or

frame

presses.
are

The

center-feed
a

presses

made

up

of
a

heavy
The

recessed

with plates, hole


in

round
to

opening in each
form the of these
in the

and

corresponding
cloth is

the
to

cloth the
no

inlet channel.

clamped
There

plate at each
in the

openings.
frame-press. A

is

hole

cloth

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

PROCESSES

AND

MACHINERY.

capacity
claimed.

of

400

gallons

of

cachaia

per

pr"es

per

hour

is

KeUy
These

FUtcr-presa.
filters
are
a

"

SweetUmd
of
hs

Sdf-dvmping
the the

FUter.

"

development
in
a was so

mechanical

type

of the

described filters,
outaidc

in 24, of

far

filtration is from

to the inside

bag.
the
first filter of this

TTie Kelly, used


over

Fig. 16,

type
are

to

be

in

cane-sugar

manufacture.
upon

Filter-bags
suitable Each

placed
and
are

frames in
an

suspended
inclined

pipe-rack
bag

enclosed

cylinder.

communicates is ad-

with

filtered juice-canal.

Muddy

juice (cachaza)

netted mud the

to

the

cylinder under
itself to the cloths

eonaiderable
and
to

pressure.

The

attaches

the the

juice flows
canal. the end

through
tion opera-

latter into
is

the
from

pipes leading
time
to

The
door

stopped
of

time

and

of and
may

the the be

cylindrical body

is opened mud.
sucrose

for the removal

of the rack

discharge
washed
to

the

The
content

mud in

or

press-cake
press.

low

the

The

cloths

require changing
The
press

at very press,

infrequent intervals.
Fig. 16,
its two
or

Sweetland takes its


name

"clam-shell"

type
and

of

from

parts

opening

closiiig

FILTER-PBBS8ES.

69

after The

the

manner

of

the

clam-shetl
2

Bteam-ehovel

bucket.

body

of the filter compriaes


with closed.
screens,

Bemi-cyUndricsil membera
to form
are
an

hinged together,

euitable The each

gasketa,

water-tight
of

cybnder
for and the

when

filter leaves

composed
outlet these

crimped-wire

provided

with

nipple
screens

filtrate. latter

Filter-cloth
are. so

is fastened that with

over

these in

arranged

they
the

may

be

clamped
in filter.

tightly
Variable

place in the filter body


with the is

outlet-nipplea
the

connection

delivery
for

fittings outside
the leaves
to

epacii^

provided

suit different

Fia.

IQ.

filtration ahut-off

conditions. cock,

Each

leaf

has
etc.

separate
The

delivery,
and the

glass delivery-tube,
press is easily and

opening
Several

closing of the

quickly
power.
one

accomplished,

lai^e ^le
may

of presses
at

using hydraulic
the
same

presses

be The

operated

time the
The

from

hydraulic
collects

valve.

Uquid is forced
submerges
and
process the the

into

filter. mud

It

displaces the air


upon

and cloths This

leaves.
passes

the

hiiuid
continues

through adjacent

them

to

the

outlets.
are

until

filter-cakes

but and

alightly separated.
the the wash-water
in the

The

cachaza-valve

is then The
water

closed

valve cake

is

opened.
a

displaces
sugar.

juice

and

removes

large part of the

^
70
FILTRATION PROCESSES AND MACHINERY.

dried by compressed washing, Uie cakes are partially if so desired, and the lower half of the body is swung air, open and they are discharged. Steam air be or compressed may After used inside the leaves to loosen the cakes from the cloths. A

coating of
of the

kieselguhron
This is

the cloths facilitates the

cakes.

applied

in water

discharge suspension before

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 containing skimmings, allowance must be If the skimmings are not made for their volume. 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-tanks may 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-cake be almost entirely may To what extent the advantages of this process are offset by
28.
"

the

and possible
not

even

probable return
of

of

to impurities

the

juicehas
29.

been

estimated.

Reclarification
the

Filter-press Juice.
the
presses

"

Many
to

sugar-makers return and others clarify defecators;

filtrate from

the

resettle this filtrate separately

RECLARIFICATION

OF

FILTER-PRESS

JUICE.

71

and the This the


to

then filtrate last

mix

it

with
to

the the

clarified

juice;
of

still the
matter

others

pump

directly
is
an

charge-tanks practice, especially


to
no

evaporators
how been Such clean added filtrates

objectionable
appear to

juice
the mud

may

be,

if

lime

has

(cachaza)
the

preparatory

filtering.
of

greatly

increase

scaling

of

the

tubes

the

evaporator.

CHEMICAL

REAGENTS

USED

IN
1

PURIFYING

THE

JUICE.

30.

Lime.
has
are

"

^The found

most

effective
treatment

agent

of

moderate

cost

that There
use

been

for the

of the

juice

is lime. for

several

methods

of

preparing this substance


as

in
is

the

defecation
to
a

of fine

cane-juice powder
the lime

follows:
must

lime (1) Quickbe slaked

ground

which

with
in

water

before

liming
slaked

juice. This
is

method

Cuba.
on

(2) Dry

prepared
powder

by
This
of to

is_used sprinkling
TvitK form Baum6 tors defecaof

water

heaps of lime.
to
use

The in

sifted
the

is mixed

juice preparatory
lime

defecation.
of

is also used
from

in Cuba.

(3) A milk
and

lime

15"

is

prepared
through

quicklime
in

is

pumped
it is

the

pipe-lines,
method and

which very

circulating. This
both slaked
the in
cane

is used

constantly generally throughout


(4) The
settle and linae form The is
a

kept

beet-sugar
and then

industries. allowed
water to

large tanks
The

heavy

paste.

supernatant
use

is drawn

off.

paste is weighed for


The

in the defecators. lime is of great


sugar.

preparation

of the

importance, especially
Essential be
not

in the in

manufacture

of white

conditions allowed
for thus be

properly slaking
reaction the
as

lime
too

are

that much The

full time
water

the

and

that

be

added,
should
and

reducing
large
the When the
season.
so

temperature.
retain the heat

slaking-tanks
reaction

to

of the

promote

slaking.
the factories
to

of Louisiana the lime


in

were

very of

small the
to

it

was

custom

slake
milk
water

advance
after

grinding
a

The

was

reduced,
then

slaking,
through

low

density

with

and

passed

fine

screens

list of

several for
use

hundred in sugar

substances

and

combinations
on

that
532

been

proposed

manufacture,

is given

page

72

LIME.

73

into

second
After

tank

and
a

so

on

until all the

containers

were

filled.
to

allowing

few

settle out, the supernatant

days for the hydrated lime drawn off and fresh liquidwas
added
to

portions of the strained milk


in the tank. The

were

the paste

already

alternate
were

drainage and
filled with

repeated until
paste.
further been The

all the tanks has


two
or

settling were the heavy limeindications


of

author

frequently noted
three weeks
to

slaking even
This

after the tanks

had the

filled.

description is given

emphasize

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

form
on

However,
of lime

is made

farther

scale in the evaj- orators. of the satisfactory use

of magnesia. containinglargequantities

The

to

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, resulting in
an

almost and

impervious filter-cake.
on

amples Ex-

of lime-stones
are

comments

their characteristics for Chemists


of Beet-

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


Lime Hawaiian this
source

"Handbook

from

coral beach-sand The

is used

to

some
^

extent

in the

factories. shows
per

cent;
made

lime 91.7 for the

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

author

Cuban
of 6.6

coral sands and


4.5
per

(dry) gave
cent.

magnesia
first of 92.5 and
per

carbonate these
cent cent

The

Cuban calcium

sands

would

oxide, 6.0

containing per-cent magnesium oxide


to

produce lime

1.6 per

The the

etc. silica, following information

relative

coral

sand

is from sand is

Paia

factory, Island
in

of

Maui, H.

T. *:

"Coral control.

burned
sand is

rotary kilns

with

temperature

Danp

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

sand

contains

considerable
Sta. Haw.

magnesia
Sugar
Planters*

which
Ass'n.

is

Spec. Report,

July, 1913, Expt. (Hawaiian),

"Planters'

Monthly

Nov., 1909, 444.

74

CHEMICAL

REAGENTS

USED.

usually presumed
to

to be

depositing,upon portion of the magnesia


increase The the molasses

its

objectionablein the defecation owing the heating-surfaces. Further, a remaining in the molasses
consequent loss of
would
sucrose.

output with
Maui

experience
a

of the

showed The the


5.45

large elimination defecation was good, the yield of


output
per
saw

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


sugar

satisfactoryand
lime contained in 1913 The elim-

of of

molasses

was

small. The

The

cent

magnesia."
lime in
use

writer visited Paia defecation carbonation


process. process

and

coral

in the double the


"

alkaline
"

filtration in the

inates
30a.

the

magnesia Sulphurous
sugar

from

Acid.

juice. ^The production is described


58.

in

the used

white-sugar chapter,
in
raw

page

This

reagent
"

is little

manufacture

except in Louisiana.

Aside
a

from

its

heavy

bleaching effects the sulphurous acid precipitatewith the lime which assists
clarification. thus reduces It also
the

duces prochanically me-

in the the lime salts and massecuites.


more

breaks

up

some

of

viscosityof the sirup and


massecuites those made boil much than without

Sulphured sirups and


vacuum-pan

freely in the
31.

this reagent. Carbonate of Soda,


ferment
as

Caustic better

Soda.

"

^Juices which with

have

begun
than
are

to

are

neutralized

soda,
salts useful has

rather that
in
a

with

very

lime, objectionable. The


The taken

the

latter

produces soluble
salts
are

soda

also

neutralizing molasses.
beneficial effect when

carbonate

apparently
in

into the pan

boiling stringlime

sugars.

Carbonate
from

of soda

is

an

incomplete precipitant of
In
a

its salts in sugar

solutions. the

series of experiments
of

de
to

Grobert
a

found

that

addition
of

carbonate
of

of

soda
cipitated pre-

sirup in the proportion


about
52 per
cent

its equivalent The


per

lime

of the lime.

addition
cent of

of two

equivalentsmore
A
wa,s

of soda

81 precipitated

the lune.

part

of the soda

remained

in

free state

and

neutralized that

by the organic non-sugar.


of soda

the remainder M. de Grobert etc.

states

if carbonate

is used

in

juices, sirups
21.

"

Eighth

Cong.

App.

Chem., 8,

76

CHEMICAL

REAGENTS

USED.

facture.

Among
acid zinc

these

substances

are

barytes,
of of

hyposulacid and
of

phurous
with'

(made
tin

by dust),
etc.

the

reduction

sulphurous
sodium

or

hydrosulphites

calcium,

clay,

alumina,
acid

Hyposulphurous
tin

is tin.

used The

in last

bleaching
named

molasses,
is also used

also in

salt,

or

muriate washes is for used


to

of

centrifugal Kieselguhr
of

yellow
as a

sugars.

filtering sirup

medium.

The

addition filtration.

this

material

juice

or

greatly

facilitates

EVAPORATION

OF

THE

JUICE.*

34.

Multiple-effect
of

Evaporation.
the

"

In

the

old

esses procto
a

sugar-manufacture,
the
a

juice

was

evaporated

sirup and
kettles
over

sirup
fire
or

to

the
pans

point of crystallization, in
in which the have

open

in

liquor

was

boiled

by live steam-coils.
and these is very
The
are

These
in very where

processes

nearly disappeared
and
sugar

only used
in
or

small the

factories

by but
or

few

of

except

places
where is in
to

price of

molasses

high,

local

conditions

pennit.
modem

evaporation being
type
in of
made

multiple effect in the


do

factory,

the
to

steam

duty

two

or

more

times, according
is
ducted con-

the

the

evaporator.
of
vacuum

The

evaporation
of

various "standard''

forms

apparatus,
the
most

which

the

so-called
In the

is triple-effect
a

generally used.
will
a

this

form

of

evaporator, book,

description of which liquor is boiled


in shallow few inches
to

answer

purposes 3 to

of this
4 feet

the

in and

deep layer,
tors evapora-

from

in

depth, whereas
from of the of the
a

film
a

the

depth
to

varies

but

thin

film,

according
The of

the

type type

evaporator.
evaporator,
in
consists triple-effect,

standard

three

vertical lower

cylindrical vessels, termed


part
or

'*pans"
with
a

or

''effects"; the
drum fitted with

of

each brass

is

provided

steam-

copper

tubes,

through by
In

which

the The of

juice circulates
steam-drum the
to

and termed is
a

which the

are

surrounded

steam.

is

"calandria." which
as

the the

center

calandria the lower This


space

large tube
of

carries it boils

juice back through


the

part

the

pans

up

tubes. The

large
above of pan,

tube the
a

is called

the

"down-take."
vapor-space,

calandria,

the

is

nected con-

by
of the the pan
^

means

large vapor-pipe
the
vapor-space

with of the

the

steam-space
pan

second

and the

second of

with third and

calandria is
See P.

of

third.
a

The

vapor-space the

the

connected
pp.

by
381,
"

large pipe with


and Juice

condenser
by
Prof.

350

Evaporatin*?

Heating,"

W.

H.

Creighton.

77

78

EVAPORATION

OF

THE

JUICE.

vacuum-pump. exhaust steam


water

The from

juicein
the flows

the

first pan
pumps
a

is boiled

by

the its

various

and

engines and

of condensation

through

trap

to the boiler-feed

water-tank. The
vapor

generatedin
that
pan.

in the second, and

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

sirup in the third


circulates thin
water

The

pan to pan juice being admitted and the removal

from

juiceis fed into the firstpan and reaches the third,the and finally, fast as the' evaporation of the as sirup permits. A
vacuum

of finished

is*producedin
in the
vapors
vacuum

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

in the calandrias in each


pan

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 pan. travels

depends somewhat

By

reason

of the
to

differences in the
and
are

vacuum,

the

juice
the

from

pan

pan

the hot

vapors

produced
to

in

evaporation in the first pan


in the the

enough
to
water

boil the

liquor

second, and
pan.

those

in the

second

boil the

sirup in
pan
or

third

The into
to

condensation the the calandria boiler-feed

of the third

second
pan,

is either

drawn

of the

is

directly pumped
third pan These
pumps

tanks, and
*'

that

of

the

is also removed
are

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
sweet-water

by a pump. usually termed


from the

The

is removed

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 are

like inverted of such


to

syphons connecting the liquor-spaces and


vacuum are

length that the


them.

in the pans

is not

sufl[ia

cient

empty
level of

They

arranged

to

maintain

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

first pan.

These

pipes

cause

the

liquor

to

circulate

very

rapidlythrough the tubes

of the calandria.

In

the operating

MULTIPLE-EFFECT

EVAPORATION.

79

apparatus

the workman

needs
on

only to regulatethe
vacuum

inflow

of

juice and steam-pressure


to

the first pan.

less It is perhaps needin the third pan circulators. is

state

that

very

uniform with

work to satisfactory requisite

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 baffleusuallyin a greatlyenlarged section of the vapor-pipe. plates, The enlargement of the pipe reduces the rate of the travel and of the vapors permits the deposition of the entrained Owing
to the

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

pans pans

etc. quadruple-effect,

The

principle upon
is the
same

which

all types of is that

this

apparatus
in the

are

based

for all and standard

outlined With

of descriprtion than

the

higher combinations
under
a

the

triple-effect. the first pan triple-effect,


it,instead
of
a

is worked and

pressure

within

vacuum,

is called the calandrias

"pressure-pan."
of

The

multiple effects
incondensible of these
gases

are

provided with pipes


A careful supervision
not

for the removal


of

of the

gases.

the

removal

is necessary,

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

because

only the heating-surfaces,

of the The

and partlyfrom juice, should be

other

nitrogenous constituents.
the upper and ruins them.
very

anunonia

removed, since- it attacks


in the steam-space the

ends of the copper


It is the the in largely
vapor

tubes

practice in

beetnsugar industry and


to

cane-factories of Java

utilize

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
or a

quadruple effect.
"extra steam"

When from

the

first vessel

is

"robbed,"
surface
is

is taken

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
etc.,is used in connection
with the

multiple-effect.

80

EVAPORATION

OP

THE

JUICE.

The
the

of the first effect heating-surface

is sometimes

double

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
even instances,

to

part of the massecuites.


are

Preheaters

(Pauly-Greiner)
their be due This

VCTy

little used

in

the is

cane-industry, though
extensive.
steam may

use

in

beet-sugar factories
to fear of

to the

large amount
or

of exhaust-

usually available in cane-factories


sugar
at

ing destroy-

the
a

Deerr
upon

made

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

cane-sugar

other

conclusions

he

arrived at the following: (1) "The

system

obtaining in
very

cane-

juices is
amounts

very

complex
a

one,

consisting of
weak

variable of free

of salts of both
Hence

strong and
that may with

acids,and
one

alkali.
may
cause

temperature
inversion local

be safe with With

juice

serious

another.

conditions

usually prevailing in juicesshould


with
to
no

factories

(Hawaiian
at

Islands),

suffer

half hour's

heating

120"

C. (248" F.) conservative

detectable

loss of sugar.

It would

be

adopt this temperature as the highest to which cane-juice should be subjected during evaporation, though under a
careful 125" C.

system

of control
or even

and

observation 130"
"

temperature

of

(257" F.),
be

C.

(266" F.) for shorter


sterilization almost of taneously instan-

periods, might
cane-sugar at

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


125" C." the

(3) "The

use

of of

high-temperature evaporation and products is possible


a

evaporation and
under After
a

preheater system

also the sterilization of all cane-sugar rational control." of the it is

house

the

concentration

juice

to

multiple-effect evaporators,
settling- and
im

pumped

sirup in the to combined

storage-tanks. A

considerable

quantity

of'

soluble in the thin juice are insoluble in that were plenties 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
*

Bui.

36, Expt.

Sta.

Hawaiian

Sugar

Planters'

Ass'n.

MXTLTIPLE-EFFBCT

EVAPORATION.

81

settling and
The

decantation

in

the

tanks

mentioned is very

above.

sediment

that collects in these tanks


cannot to

rich in sugar. it is

This material

be

therefore readily filter-pressed,


or

usually pumped
with

the defecators

to be diluted clarifiers,

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

and
same are

foam

that

rise to the surface of

have

the which

coefficient derived. that better

purity

as

the

approximately sirup from


of 3rield

they

It is probable
sugar

results, so
be realized

far

as

the

is concerned,

would

by rapidly heating
of the
as

the

sirup to its
scale
be

boiling-point.
forms
at
on

The
must

which

the

tubes

evaporators
a

removed of heat.
cane

frequent intervals
Its

it is

very

poor

conductor that

composition
some

varies

somewhat
very

with
much
*

of the

and

in The

localities forms of the first pan, with

faster than contains other

in others.

tubes

which those

always
of the the

thin

juice, scale little compared


The
most

pans.

third

pan

of

contains triple-effect

thickest The
in

and

obstinate

scale.

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

IstPan, Cent.
57.85 2.02 3.25 7.86

2d Pan, Per Cent.


56.98 1.92

3d

Pan,
Cent.

4thPan,
Per

Per

Cent.
7.49 1.65 9.93 7.02

Phoflphate Sulphate
Carbonate

of lime
of lime of lime

15.02 0.54 19.55 0.71 11.32

4.68
13.31

Silicate of lime
Oxalate Iron of lime

11.27 2.58 54.34 5.08

oxide

2.03 7.79 matter

1.53 7.43 13.41

2.31 39.26 11.04

Silica Combustible

20.37

The
water

tubes and

may

be

cleaned

by moistening the scale with


This is
a

scraping
method,

the

surfaces. the

very

laborious

and and

tedious

therefore

followingis usually used,


vacuum-pans.

applies also in cleaning the coils of the


"

Prinsen-Geerligs, Kobua

Ar chief, 1900, 694.

r
82
EVAPORATION OF THE JUICE.

The caustic of is into with is the

pans

are

filled solution cubic

to

above

the

level from

of

the
to

tubes
two

with

soda soda

containing
foot
hours of

one

pounds
solution
the
pans

per

solution. and is then The dilute The the


a

This

soda

boiled

during
iron
or

several

run

from
pans
are

an

lead-lined
then into boiled the acid
of

store-tank. with
sewer.

washed which

water

and
run

muriatic acid should

acid,
be
treatment

afterwards
to

strong
if the the the

enough repeated

be
at

very

to

taste.

This
will At

intervals in
Reason

about

week

usually
the end
to

keep
of

heating-surfaces

good
it

condition. is

manufacturing
tubes The
a

usually

necessary

give

thorough
alkali solution time
is to

scraping.
may

be
as

used becomes

repeatedly,
weakened.

adding
The pressure

caustic soda in

soda
solution

from

time boiled and

it

always

under

atmospheric

cleaning

evaporators

pans.

84

PRESERVATION

OF

JUICE

AND

SIRUP.

formaldehyde.
should fill the The be mixed

The
with

measured the

quantity
juice immediately

of

the

preservative
on

starting

to

defecator. of

use

formaldehyde
separators
tends
to

in is
not

preserving entirely
after

juices

held

in

DemThe tinae.

ing's juice
This the

closed

satisfactory.
a

always
may

decompose
due
to

standing
in The

short

possibly

be with

difficulty juice!
from
to
to

thoroughly formaldehyde

mixing
is

formaldehyde
added the in heaters

the

usually through

the

pump-tank,
and eliminator be due

which the

it

is

pumped
The

separators.
that

decomposition
the also The walls of

may

also tank

organisms
killed

lodge
heat.

upon

the

and

are

not

by

the

{See

11.)
writer's in

experiments
the presence due
of
to

indicated
of

slight

deterioration This tion deteriorathere

of

juice,
was

even

formaldehyde.
of sucrose, of

probably

inversion In
and

as

were

no

indications of labor
of the

fermentation.

view
of

the

very

large
event

saving
breakage juice,
The

and

fuel,

often the

sugar

in

the

of the

machinery,
with

slight
is

deterioration

of

preserved
cost

formaldehyde,
in

insignificant.
is
so

of

formaldehyde
be

barrels
it

small

that

it

would than the is

usually
indicated in the

advisable above.
It

to

employ

in

larger

quantities
from

practically

all

disappears

juice

evaporation.

CRYSTALLIZATION

OF

THE

SUGAR.

36.

The

Vacuum-pan.
of

"

The

eirup obtained
45 per
water

in
cent

the
or

concentration
more

the This

juice still contains


content

of

water.

of

could
to

have

been

largely reduced

in the
sugar

but multiple-effect, further

facilitate the in

graining
a

of

the

evaporation is conducted usually


and vertical and
a

vacuum-pan,

in

single-effect.
is
a

The

modem
cast

vacuum-pan

cylindrical

vessel, of
a

with iron^,
copper

conical

bottom has

is fitted with

number

of
at
or

steam-coils

strike-valve The and


pump
to

the

bottom,
of the
a

for the

large door or discharge of the sugar.


with with
a a

roof

dome

pan

is connected and

save-all
vacuiun-

condenser

by

directlyby the
type
of the
pump.

large vapOT-pipe vapor-pipe or by a


The the
vapors

small

pipe,according
very

the

vapor-pipe is usually made


may

large, that
slow, thus
also

velocityof

be

comparatively
pan

reducing the

entrainment

of

sirup. Hhe

is

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

for

the

removal that the

of

test

samples.
can

The the

apparatus
temperature

is

so

arranged
the which is

panman

vary

of

boiling liquor by increasing or


produced by the
the ctmdensed
pump
"

decreasing the
condenser.
all of the The

vacuum

and when
are

pump

is said to be of the ''wet


water

system
vapors

condensingwhen

and
are

passed through it. The

vapors
a

condensed

in

special condenser,
and flow
or

using
to
a

pump

of the

''dry system,"
a

with

the

condenshot
as

ing-water through
well and thence

torricilian the

tube

"leg-pipe"
air is led

from

factory. The by the


These
pump..

off in

separate
The of
pan

pipe
as

and

removed

described
are

is of the

usual

form.

Various
extent

types
and

vacuum-pans

used.

vary

in the

85

86

CRYSTALLIZATION

OF

THE

SUGAR.

arrangement
devices special
37. the

of

the

heating Hurfaces,in
of the pan, and the circulation to

the

relation
use
or

of the of

height to the diameter Boiling

in the

absence

to promote

of the order

boilingmass.
to

Sugar

Grain.

"

In

facilitate

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

given.

beet, and

in expressionsdiffer somewhat branches of the industry. Only refining These will be

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 When
a

in cane-work

massecuite," and

each

boilingis
from

called

"strike." and the

portion of
is left
as

strike is removed
a

the pan

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 pan.
two
or

remainder

The
more

pirocess is termed
pans
are

"cutting." by side they by large pipes, with


from
one

Where
are

worked

side

often

connected

with

one

another
the

suitable another.
In

valves, for drawing


These
are

massecuite

to

called

"cut-over
a

modem

practice, when
it is said to be

pipes." grained strike


into the

reaches
pan

certain
of

stage, diluted molasses

is drawn

instead
in
on

sirup and
When

"boiled

in,"
been

or

"boiled

grain-sugar."
liquor in the certain density and is more
fs said or "weak"
to haVe
as

the

pan
or
"

has

concentrated with be

to

less saturated The

sugar,
' '

it
"

reached
the

"

proof.

proof may
or

strong
This

liquid is
the

of greater
as

less

density.

expression
connection
The

is still further with

modified,
of

will

be

explained

in

process
the
a

of

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


pump

pan

is

closed,
shows

vacuum

is started, and
20

when

the
tlie

gauge

vacuum

of 15 to

inches

of

mercury,

chargepan

valve
td
cover

is opened

and

sufficient Steam

sirup is drawn
into the

into the
coils ahd

the

coils.

is turned

tlie

BOILING

SUGAR

TO

GRAIN.

87

sirup is rapidlyconcentrated
used
or

depends
as

upon

low

in the pan. he

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

high,
room

needs

many

crystals and

comparatively little

As coils
more

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
are

for their

or

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. this

At The

stage there

are

two

methods until
as

of

procedure:

(1)

concentration

is continued with

the

ciently liquor is suffi-

supersaturated

sugar,

is indicated
watet

sample
into
on

drawn

by the proof-stick. The


is
now

of

by a injection

the

condenser

increased
th^ cooling

and

the

steam-pressure

the

the
sugar

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

coils reduced, thus

to

itself and described.

the

quality of
second

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 but of
sugar
are

in

(2) The

separate,
sufficient and of

and

when

the

there the
a

crystalshe

panman raises the

consider^

that of

temperature

pan

injectsmore
uniform

sugar

more

sirup. The first method grain than the second,


formed
at
once.

produces
since

all ol

the

required are crystals


After the

crystals are
to

formed, sirup is drawn


as

into

the. This

pan

from

time

time

the

water

evaporates.

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
mass

secure

the

best

results.

If

the sirup when surrounding the will


be

is too

concentrated, with
rich in
sugar,

injects the liquor

he

crystals too
and
must

fresh

formed -'false

be

remelted. formed

Th^se
at
a

crystals crystals are


late

termed

grain," and

where

stage

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

r
88
CRYSTALLIZATION OF THE SUGAR.

the the

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

is rich in sugar and sirupsurrounding the crystals of such densitythat it is supersaturated at 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 raising molasses. the temperature 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
pan

from

time is

to

time until the

strike is

kept very free, t.e., of c""nparauntil the crystals low density, are large or the pan is tively about two-thirds filled. At this stage it is gradually boiled the end of the operation,thus dryer ioid dryer until near and impoverishing the molasses surrounding the crystals, is evaporated to an apparent degree the massecuite finally Brix of about 93, and is then discharged from the pan. should be as cold as possible The massecuite at this stage. of estimating There are various methods the proper moment 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 crystals the sugar to deposititself upon already present
finished.
,

The

massecuite

and
causes

not
a

to
waste

form

new

ones,

concentration Unnecessfiry
steam.

of time of

and

sirup,employed with with all, but not applicable 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

charging a

pan

with

BOILING

SUGAR

TO

GRAIN.

89

of the

valve

is

adjusted sirup, etc.


of

from

time in

to

time

as

the

tration concen-

varies, with

variations This

the

steam-pres""ure, the
of
very

density of the
the first method
of sugar,

method

and

produce a graining, good yield from very


many

charging, with uniform quality


An

the

massecuite. false

irregulargrain, with
that from In has
not

minute

from crystals,
a

grain
sugar

been

melted, results in
so as

low

yield of
the

the massecuite.

boiling a
sugar

massecuite from
at

to

obtain of

maximum

yield of
moderate

it, the full number

should be formed
and
very

graining,and

crystalsrequired the crystalsshould be of

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 sufficient increases
to take crystal-surface up

the of

sugar,

and

besides

the

risk of the
on a

formation small

false

grain. When
or

boiling a strike
a

very

nucleus

of massecuite of
a

on

small

cut, there is also risk of false


molasses. be

grain or
in

partially

exhausted The

temperature

to

maintained

the

massecuite
whether,

during boilingvaries with the desired grade of


hard
or

sugar,

soft,white
from

or

raw.

American in

practice also differs


to

somewhat
The As hard with Java will be
sugars
no

that

of

Java

respect

temperatures.

low temperatures. prefersrelatively superintendent noted


are

in the boiled

chapter
at 180"

on

F. in the American but lower

sugar-refining, 119, page refineries,


temperatures
are

inversion.
in the
as

Similar

customary
Hard

white-sugar factories

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
sugars,

grained

at

temperatures

approximating

160"

F., and
the

the

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

until be

grain is
in the

lowered of the

strike to promote

reduction

purity

to

that surrounding the crystals. Massecuites either in motion be further crystallized (crystallizer
or as a

massecuite) temperature
In

at

rest

in tanks

should

be

boiled

at

as

low

possible.
very

making

soft sugar,

after

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 for soft-sugars. usually preferred are of Sugar-boiling. Methods Pan-room 38. tions. Definiture

of the

"

"

Raw

sugar

manufacturers

often

designate their
as

vacuum-pans
or

and by the letters "A," "B" "C," number them, to distinguishthe grade
not

in
cuite masse-

fineries, re-

of

and

the pans

themselves.
same

pan

is

usuallyalways
a

employed in boiling the of fts proximity account


but this is not With the

grade
a

of sugar

in

refinery on

to

certain mixer in
a

and

set of centrifugals,

usuallytrue

factory.

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

by

n"Un"3

rather

than

numbers.

Formerly
strikes
were

when

only
cuite masse-

were "straight-sugars"

boiled, the
"third." pure The

numbered

"first,""second"
was

and

first strike of

boiled' with and the


may

cane-sirup,the second
second in molasses.

with

first

molasses all the thfere is

third be

with

At

present
three

pahs
some

boiled
in

part with
nomenclature. of

molasses, hence
When

confusion
are

the

massecuites

boiled

with

return

molasses, the writer


(1) First
a

prefers the following designation for each: containing only sirup or sirup and
molasses. This is therefore
a

cuite, masse-

very

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
of

massecuite

In many
case

factories but
of

two

massecuites

are

boiled,in
"mixed"
or

which

that

the

second

boiling is termed
in this method

ond." ''secto

The about 75"

first massecuite

is reduced

purity with first molasses. the methods of pan-boiling Utilizingthese definitions, in raw-sugar with rich tropicalcane worl^ will be applicable methods described. These are rapidly extending in Cuba
and possibly elsewhere. The
of boiling-back molasses

"has been

practiced ih Louisi*

92

CRYSTALLIZATION

OF

THE

SUGAR.

diately after leavingthe vaeuum-pan^


the
same

and
of

should

produce

grade of

sugar

and

purities. The second or This after remaining three or four days in the crystallizers. 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-crystals and should be The molasses must
'*

widely different massecuite is purged crystallizer


molasses

warmer

than

the massecuite 54"

in the pan.
pan
"

It should

be reduced

to

density of about
Boiled

Brix, at
Islands formed
to

temperature.
In Java
a

MassecuUes

with

""Seed." and of

method

practiced

largelyin the
upon
a

Hawaiian
magma

the strike is started

footing of
A

string-sugar mingled with


in this way is

sirup. Grain
called ^^seed."

upon

which
sugar

build

popularly

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

method
in the

of
source

boilingwith seed
of the 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,
The but it may stored in without also be
a

used

in first massecuites.

The

magma

is

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


from

with motion, and crystallizer,

is

massecuite The
pan

another
a

pan.

following is
is boiled

convenient

pan

method:

The the

first

without

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


massecuite. The The molasses

molasses, except when second (mixed) massecuite


is boiled from this
on a

sirup
of

is boiled.

footing

first final.

massecuite

is

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

crystallizer sugar,

with

second

molasses.
very

This

method

produces
any

single

grade of product of

strong grain and

desired test.

METHODS

OP

SUGAR-BOILING.

93

'

BoUing MolasaeS'Sugara. In
"

many

for the process

in of crystallization

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 fitted molasses with is first heated 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. Many
to

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

carbonate

The in
some

carbonate

of soda

neutralizes
up

the the is

acidity and
lime

sufficient
extent.

quantity breaks
Carbonate the molasses
of

salts,at least
in the

soda
ently, appar-

frequentlydrawn
soda
In

into the pan author's

with

and

experience, with
to

advantage.

The

is.preferable to

lime.

boiling molasses
the
pan

string-proof,it is simply drawn


down
to

into

and

boiled

the

proper

density.
of
a

The

determination drawn
matter to
a

of this

density,by the usual


and

tests

sample
is The
a

the "string" between judgment requiring much the

finger and

thumb,

experience.

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

required proof varies with

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


formed
range

of the

car

or

tank,

in

polarizationfrom
of

80"

to

large. Such sugars 90", varying in test with


skill

the

quality pan-boiUng.
89"

the

molasses

and

the

displayedin
is

the

A suitable

densityfor
Brix.

the massecuite

mately approxi-

to

90*, apparent
from mixed

The

sugars

massecuite
are

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


"

not

"

molasses

sugars

in the

commercial from
rest.

acceptance'
massecuites Such
sugar

of

the

term.
to
"

Molasses

sugar

is obtained

boiled
has
a

stringtest
" "

"

and

at crystallized

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

first sugars

except in color.

94

CRYSTALLIZATION

OP

THE

SUGAR.

39.

Crystallizaiton in Motion.
in the

"

^This process

was

first

turers beet-industry. Cane-sugar manufacslow in abandoning string-sugarmethods, and were when the strikes were first introduced crystallizers were 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 cr3^8tal-

used

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

lization

far

as

is

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

massecuite

be

kept constantly in motion

and

be

temperature
is

to increase

the

supersaturation.

Manifestly it

device that will move each impossible to produce a stirring 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

separating it from
an

its neighbors is but The

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 in thickness.

stronger solutions

near

by

must

mix

with

the weakened

tion solu-

by diffusion.
uniform

The

motion

of the stirrers of the

lizer, crystala

by rocking the crystals, promotes


fall of temperature of temperature, the saturation the growth
of the of the

this diffusion and With the

in the massecuite.

fall

solution

resultingfrom

crystalsis
A
to

crystallizationcontinues.
the

changed to supersaturation and point is finallyreached when


This is due
to

crystal size

ceases

increase.

the

vis-

"

'"

Crystallizationof

sugar

in aftei-product

massecuites,"

H.

Classen

Int. Sug. J., 14, 284.

CRYSTALLIZATION

IN

MOTION.

95

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.
not
to
a

cosity of the medium

and

lack

of

as

diluent

since

it does

not

add

solids to the

massecuite.

From should into the

the above be boiled

remarks, it is evident
to

that the massecuite

very

high density before


should
not

discharging it
with molasses the that

and crystallizer

be diluted

in the

vacuum-pan.

Dilution has

should

fall of temperature the

increased

begin the moment the viscosityso much


With

no crystallization

longer progresses.
determined
in

practice this

condition massecuite
to

may

readilybe
in motion diffusion

while

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
promote
**

massecuite

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

used
A

to

limited

extent
as

on

account

of
a

local condition:

(1)
into

gKainstrike
the pan; and

is boiled

is usual and
of about

part of it is discharged
90"

from

hot molasses is mixed with

Brix

is drawn

the pan

into

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

the massecuite

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
a

and crystallizer

mixed

with

as

in the first method. Thare is

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
or

magma

in these processes. the

Among
the
older

advantages
are a

of crystallizationin motion

over

methods,

saving of

labor

and

floor space,

96

CRYSTALLIZATION

OF

THE

SUGAR.

the production of grain-sugars and the ability cleanliness, the factory at the close of the manufacturing promptly to liquidate
season.

No

massecuite

need

be

carried forward

to

avoiding loss by fermentation. ^The apin Motion. Laboratory Control of Crystallization 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,
"

the next

thus

immature.

Crystallizers.The
"

usual

are crystallizers

of three

the third of which Closed

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


a

types, works: (1)

stirrer. A water-jacket for control powerful spiral with 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. fitted with stirrers as in the of half-cylinder cross-section, These closed closed type. (3) Vacuum are crystallizers. vacuum-connections and provided with a crystallizers This is in fact crystallizer steam-jacket at the bottom. with forced circulation of the a slow-boiUng vacuum-pan fitted with massecuite. The

large extension of present-day factories has led


from

to the

discharge of the massecuite

through
in the pans

the pans into the crystallizers is applied air-pressure pipe-lines.Moderate

to force the massecuite

through the pipes. The


of not less than

should pipe-lines

have

an

internal diameter

_i

SOLIDIFIED

MOLASSES.

97

14

if the erystallizera are IncheB, especially

located far from

the pans.

CrystallizerBare
firstand mixed

used

to

some

extent
an

for the

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
the molasses.
40.

massecuites

pending

Solidified
this
to

Molasses."

So

far

as

the

formed, writer is inand


for

product is produced only in Java


for arrack manufacture. molasses of soUdified is first
**

ment ship-

British India

The

manufacture Molasses and

requires no
"

special
and

apparatus.
skimmed

blown-up

with

steam

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
have
a

is then

the characteristics
mass,

described into
on

below.

The

dried

molasses,
while it is

molten hot

is

run

closelywoven

baskets

very
are

and

solidifies

cooling.

The

tops of the baskets


short time after

covered The

with

vacuum-pump

burlap for shipment. should be operated for

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
to break

the pump

should

not

be

stopped until ready


are

the usual

vacuum.

The
as

commercial

for this product specifications shall break with


a

follows:

(1) The
the

solid molasses

clean hard

fracture; (2) it shall sink in water;


to

(3) it shall be

too

indent

with

fingernail.
^

J. J. Hazewinkel whether He and the calculated

examined

solidified molasses
occurs

to

mine deterfacture. manu-

dry substance analyzed the molasses


loss of the results to
a

during the
and the
a

before
of

after

drying,
of His loss

basis
to

ash

content

originalmaterial, assuming it
were as

be

constant.

conclusions
of

follows:

(1) There
extent

is considerable

dry substance.
upon

(2) The
the

dependent

temperature.

decomposition is (3) The reducing sugars


of the

Archief. 1912, 20, 181.

98

CRYSTALLIZATION

OF

THE

SUGAR.

in part pass that


to
some

over

to

organichoh-sugar.
loss of

(4) It is possible
is due
to

extent

dry substance

position decom-

of both About
In

reducingHBugar and

organic

non-sugar.

(5)

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

probable that' polymeiization of dextrose place during the long heating.


41.. Froth
boiled
at
**

levulose

takes

Fermentation/'

"

^Wh^

massecuites foam
may

are over

high temperatures
hours after
"

they often
The

and

run

the sides of the containers.


or some
"

foaming
froth
a

ately begin immedi-

striking. This
"

pheanomenon
It

is is

termed

fermentation
years of

or we

fermentation.''

only in
of

recent
cause

that foam.

have

fairlydefinite knowledge
due the
to

the

the

It is not

that

is, to
^

bacterial

activity, but
that

fermentation, decomposition of
to

certain salts. Herzf eld Lafar's


states
on

Kraisy

has

recently shown

that

results
e.g.,

the reaction

of the

invert-sugar with amino dioxide, is


(149** F.) is
carbon the The mation forcosity visalso is

acids,
the

glutamic acid, splitting off carbonic


of
a

cause

foaming.
temperature

Massecuites of about

(sugar-beet) foam
65" C.

suddenly when
reached. dioxide

Kraisy explains the


of sugar of the

phenomenon

by the
until

remaining in supersaturated solution


massecuite results in
foam.

crystals catalyzes its liberation.

Herzf eld

states, always referringto the beet industry, that foaming


rare

since the introduction

of

phenolphthalein for rosalic acid foaming.


in
a

in

alkalinitytests.
The usual method is to pour the

Lime
of

will stop the

stopping foaming
upon

cane-sii^ar

factory
This
gas.

water

the

surface

of the massecuite.
escape

reduces Cane

viscosity and
that

facilitates the have The


not
same are

of

the

massecuites
not

been

heated
as

above those
cause

156*^ F. do observed of

usually fpam.
md^ssecuites.
escape of

conditions

in

beet-sugar manufacture
cane

probably the

foaming

in

should crystallizer
gases
or

always

have

provision for

be uncovered

preferably should except while discharging by air-pressure.


.

the

^Zeit.

Ver.

ZuckeriDd.,

64, 543.

100

PURGING

AND

CURING

THE

SUGAR.

is directed
room

into the second

gutter and

is returned

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

purging as described farther on. Each sugar-drier ugals. or usually manipulates two centrifpurger 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
purge from 4000
to

4800

lbs. of 96" with the

polarization sugar
skill of the

per

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

the

against the

wall

of

sugar. cuts

The the

basket
sugar

is revolved and

slowlyagainstthe plow, which

down

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

spinele
the while

or

shaft
In

to

direct the massecuite other

toward
may

the be

wall of raised

basket. the

the

type,

the

valve

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
form

out

of

it without

assistance. valve should before be

In the

the
trifugal cen-

other

to lift the it is necessary machines is stopped. These

used

only

with The

freelypurging
manufacture

sugar

of strong
sugar

grain.
demands

in special care in the centrifugal with 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. is often added
to

of white

the

wash

water

to kill the

tinge

of the

sugar.

The

method

of

double

yellow purging gives

the best results in

washing plantation white

sugars

CENTRIFUGAL

WORK.

101

Two The
very

sets of

are centrifugals

necessary

for double

purging.

sugar

is

purged in the first set without


It is then into
a
**

little water. and formed

cut

down
smip

"

washing or with into a mingling


from the second

device

magma

with

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 sirup of the second. rich, light-colored 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

crystal against crystal promotes


film of molasses. Double

the

removal

of the

hering ad-

to

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

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
conveyor-screw

is lubricated

with

first molasses is also used

diluted

to

about
to

78**

Brix, and

this molasses

in the
a

mingler
The

form

magma

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


or

simply
mixer

mixer.

for immediate
as a

purging
or

to

to be storage crystallizer

used

footing

"seed"
Raw

in

massecuites. boiling
are

sugars

in

Cuba,

without

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

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 in clean dried
as are are

of also

used

in
test

the and

of

high

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 its tare White is

approximately 2.5 lbs.


may

sugars

be
steam

dried in

in the the

granulator

or

with

superheated

centrifugal.The

dryer or crystal^

102

PXJRGING

AND

CXJKING

THE

SUGAR.

lose with such

part of their glossin the granuiatorthrough friction


one

another. and

The

American

market

is accustomed

to

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

made
steam

in Java should

for the be heated

home
to

and about

East 200"

Indies C; in
a

markets.

The

separate

boiler. Various from the

types of

conveyors

are

used

in

transfixing

sugar

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

(1) Ribbonribbon it. The that

or

screw-conveyor.

This and

is

screw

or

spiral
with

revolves

in

trou^
the

carries the be
a

sugar

cross-section belt.
a

of

trough should
is often
a

parabola.
slats

(2) Endless
attached the
to

The

belt is of is
a

of

curved-steel

chain.

This

very

efficient

device,but has
hopper (3) Grassthat is

objectionable feature
conveyor.

leakage of
very

sugar.

This

efficient conveyor of Scotch

used

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
very very

generally in factories

quickly,leaving the
a

sugar.

Each

stroke

advances
are

the

sugar

certain distance.

All parts of the conveyor

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 centrifugal market 96*^. sugar polarizing
"

This

sugar

must sugar

be

grained in the
is of

vacuum-pan. test and


' *

The

responding cor-

in Java

higher
tedt

is there called
''

* *

muscovado,
market
may

''

and

in the American

market
upon

Javas.

Under

certain based

conditions 95"
or

the
of

which
next

be

instead

96".
was

The

price is grade is 89""

the

molasses

sugar

seconds.

This
now

crystallizedat rest, but


included. and Muscovado

sugar

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

in coolers crystallization

The

molaases

LOW-GRADE

SUGARS

INTO

HIGH

GRADES.

103

b removed

by simple drainage. The

bulk

of the

raw

sugar

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
very

dark

brown, numbered
25. These
are

7, to

an are

almost

pure

white

numbered Holland.
square sugar 44.

samples

prepared
sugar size.

sugar, annually in in small

They
bottles

supplied to
uniform No. of

the

trade

of the

glass and

Tropical 96**
The cation classifi-

usually fallsbelow
Classification
of the sugars
122.

16 of this standard.

White

Sugars."

given
order
n:ust 45.

on

page

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


or

Plantation
to

White
meet

Granulated.

Java

white

sugars

in

the

market No.

of the East specifications Standard.

Indies

grade above
Conversion
"

25 Dutch of

Low-grade
of

Sugars
a

into

High
sugar

Grades. without this

The

method

making
sugars

single grade of

remelting the low

is described

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

polarization. String-sugar must


or

be

used

to

"

seed

"

pan

be

remelted in
a

in

juice or

water

for

reboiling. Remelting

results

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

part of the

products that
46.

serious deterioration of

in storage. of

Deterioration

Sugars.

Warehousing

Raw

Sugar.

"

^The

of losses of much

through
study.^

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

Jhe

size and

hardness the

of the

the crystals,

cleanliness of the factory and


the moisture
content

process,

residual sirup on

of the sugar or the crystaland the

packing conditions, the composition of the


character of the
ware-

See R.

also

"

The

Deterioration

of

Sugars

on

Storage,"
Ass'n.

No6l
!

Deerr

and

S. Norris, Bui.

24, Ezpt. Sta. Haw.

Piantera'

104

PURGING

AND

CURING

THE

SUGAR.

house

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
on on

account

of the
^

dilution

of the

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 and to be usually due to bacteria by investigators

of molasses

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 activity of bacteria water A
sugar

and

yeasts.

large and

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

Cleanliness

the moisture
upon

content

the

keeping
will
must

of the sugar has a very is the consensus qualities


now

marked
of

ion opinfact

of many that in
very

observers.

It is

quite
its be

well-known

dry

sugar

usually hold
also

polarization' even
under

long storage.
The

It

stored

sanitary
is not
that

conditions. well

permissibleupper
very

limit of moisture
observed generally

but it has been established,

^Beet

Sugar

Manufacture

and

Refining, L. S. Ware,

II, 343.

WAREHOUSING

OF

RAW

SUGAR.

105

sugars per cent

polarizing
of

less

than when in

97^

and

containing
suffer without
even

less
very

than

moisture If stored of loss of is of


to

warehoused
a

little

deterioration.
to

dry
sugars

place,
may

exposure

damp

currents

air, such
of moisture. formula

gain

in

ization polar-

through
The

application Australia,

the

of in

the

Colonial

Sugar
a

pany, Comsugar

great

value its

judging

whether

may

be

expected
moisture

conserve

polarization: polarization)
not to
=

Per In in

cent

in

sugar

-4-

(100"
may

"0.333.

other

words,
the less be

that
of

sugar

suffer its

deterioration

storage,
be should of has

ratio than somewhat

its

moisture

non-polarization
that this

should ratio Gain


sugar

0.333.

Experience
smaller for

indicates
sugars.

Cuban
an

polarization
not
a

is
a

not

always
of
sucrose.

indication Such loss the

that
may sugar

suffered
one

loss of in
a

be
a
'

offset

by

greater

moisture,
the

thus

giving

polarization
of the The
to

higher
might

than
cause

original
rise

test.

Decomposition

levulose full

small
a

of test. warehouse should


to

specification
It is certain

of

suitable warehouse
as

is be

difficult

make. There

that
of

the

large and
it should

dry.
be

is difference

opinion during
should

whether
or

almost

hermetically
The

sealed

storage

open

for be

free

ventilation.
on

warehouse
account of

undoubtedly
of moisture The the

closed
on

damp

days
with that when

on

the

deposition

the

si^ar

the it

reduced is the

night
safer

temperature.
to

writer

believes

plan

close

warehouse

tightly

practicable.
6

Approximately

cubic

feet of

warehouse and 6.5

capacity
square

should feet of

be floor-

provided
Bpace.

per

325-lb.

bag

sugar

SUGAR

REFINING

"

47. in

Introductory.
"

The

practice. The working theory,but very complex the handling of the sweetup of the lower-grade materials, mous waters and the control of the char filtration involve an enoramount

process in actual

of

is refining

simple

much detail, in this chapter. of

of which

cannot

be

sidered fully con-

The
raw

narrow

"margin"
sugars

or

difference between tended


to
cause

the the

prices of

and

refined

has

concentrar

faciHties and

shipping industryinto largeunits. The matter the increasing number of fancy grades of refined sugar have also helped in bringing about this concentration. States all of the refined sugar used in the United Practically in situated the is now cipal prinproduced in a few largerefineries
tion of the

of

seaports.
48.

Definitions. the

"

Refineries
pure

are

of two

classes:
sugar

Those and its

producing only
modifications
sugar

white

granulated

and

those

which and

manufacture

both

granulated

purity. chapter as ''hardrefineries respectively. It must be sugar" and "soft-sugar" that the in borne soft-sugarrefinery also mind, however, The two hard types of refineries use produces sugars. however, the same essentially process, the soft-sugarrefineries, employing all expedients which will give fine color to their lower-grade liquors. to refer lo a sugar The term "liquor" is used in refining 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

the soft white

yellow sugars

of lower

These

refineries will be referred to in this

By

George
The

P.

Meade,
in the

Superintendent
here

of

the

Cardenas
to sugar

Refinery,
refining
*

Cuba.
as

methods

described American

apply especially

it is conducted

refineries.

106

l08

SUQAR

RBFININa.

The

raw

sugars

arrive at the

refineryin various
300 to* 330

kinds lbs.

of each

packages.
are

Jute-bags
from the
are

containing
West Indies.

received

Hawaiian

and

Central

American

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.
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

The

sugar

is

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
"sweet-water" is mixed
to
a

with

other thus and

similar
enters

solutions

and

is

evaporated
The

sirup and

the

manufacture. under the and

palm-baskets are steamed boilers in specially constructed


barrels
50.
are

then

burned

furnaces.

Hogsheads

steamed

and the

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

Washing

the

minglers, which are with mixing-flights, where vMed

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
sugar

type used
is washed

in raw-sugar

manufacture.

The

resulting
it with

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

in the

process

separates the

raw

material

into two

parts,

one

sugar

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

kinds

sugar,

e.gr., cane-

and

beet-sugar.

DEFECATION.

10^

The

''washed
water

sugar" is dissolved in about


in
a

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.
tank

weight of

provided with

''raw-sugar washings/' purged from the mash, have coefficient of purity of approximately 80" and constitute
14 to 18 per cent

The

from

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 with
In water
or

of the

dark reduce

sweet-waters

and

is sent

to the defecators.

order
too

to

sugar

losses

through material

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.
When
very

hand

small, soft-grainedlow-grade
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.

muscovadoes

concretes,

are

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

Defecation.

The

defecators

or

steam

may

be

blown

into

the

liquor. The
to

bottom

of the

blow-up
A for

is

usuallysUghtly conical
of defecants have

facilitate

drainage and

cleaning.
great number
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
are

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
milk of lime and This
sent

is called "black of available

paste," and contains

from The

10

to

12 per

phosphoric acid (PsO^)*

black

paste

110

SUGAR

REFINING.

co"taind
hence acid black found
are

chlorides and
the

these

are

not

absorbed

by the char,

increase

paste may
dust with

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

in the market to

commercial of

names.

They

sulphates which will be retained by the char in the filters, phate increasing the sullargely 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
apt
a

have

high

other

two

preparations named, is the


introduces is introduced
as a

most

satisfactoryof liquors.
Brix. The
20"

the three and The lime

less soluble salts into the milk and of about the

phosphoric acid
alkaline
a

is first added

lime
to

afterward, usually in sufficient quantity


reaction acid
to litmus. may

immediately give a faintly


to be

faint

reaction

If soft sugars be maintained lime-salts. The

are

made,
th^

to amount

prevent
of

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

formation

of dark-colored

refineryhandling
1000

sugars

of 95" from
for

average to 600

test

will

about

lbs. of lime

and

500

lbs. of

available
of
raw

phosphoric acid
sugar

(P2O6)

each of

million the

pounds

melted.

After

the addition coils and

defecants,

steam

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 being hydrometer.
The lime

is turned

into the

the

densities

as

determined

in

the

hot

liquor with

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
^ The

Fahrenheit

scale

is used

in all American

refineries

and

is therefore

Used

throughoat

this chapter.

BAG

FILTRATION.

Ill

albumins

and

pectins. The
entrains the
or

whole with

forms

heavy, flocculent
terials ma-

precipitatewhich
derived The defecated

it the

finelysuspended
and

from

raw

sugar,

jute, etc. bagasse-fiber,

liquor
over

washings
to

liquorsmay
be washed

either be sent the

low-grade sugar or they may separate bag-filters


have been used for
a

distributed

filters which

allowing sugar-liquors,

draining period after the

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

having

outside
6 inches

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
a

short

in

diameter, and

an

inside

bag of cotton-twill fabric


across.

which

is 6 feet

long and 24 inches


A

The

inside

bag

being loosely crumpled in the sheath


fluted filter of the laboratories.
may

gives the effect of the connection, which

bronze

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 precipitate The filtered washedbeing retained.
to the sugar matter

be screwed

Uquor is of a Ught-brown color,quite free of suspended filtered raw-washings are also clear or turbidity. The
darker the color. After mud from fifteen
to

but

of much
use

twenty
very

hours' slow.

bags fillwith

and

filtration becomes
now

The

liquorgoing on

to the filter is

shut off and

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

thin

alkaline is further

sweet-water

from in the

the
as

filter-

presses and hang in the each

the mud

washed

bags,

they
into

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


after which
a

jetof hot water

three to

five times

the

bags

are

taken
remove

out

of the filter and mud. The

washed

in

series of tubs

to

all the

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

cake

is discarded

or

sold for agricultural use,

and

the presa-

112

SUGAR

REFINING.

filtersas mentioned partly in flushing is evaporated to a sirup. above, and the remainder
is used water, filtrate,
53.

Char
utmost

Filtration.

"

^The char

or

bone-black

filters are

of

and importance in refining. The economy of the refining depend upon careful control efficiency process the close attention
on

and

to detail at

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 of the next, is termed the
to cycle will take from forty-eight the speed at which the rebumed upon

"cycle" of the filter. The ing seventy-two hours, dependchar is drawn from

the kilns. Two


or

systems

of

working char-filters prevail: The


the "continuous"
one

"set" the
a

"battery" and

systems.

In

set-

system, all the filters filled in

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

as day are w6rked class doing the same

group

of work

system,

each

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. 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 smaller char-filter installation for
a

at

the top and


20

and

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

termed the The


weave

the

Two

manholes of the

at

the

sides

near

bottom char

for the
on
a

removal

exhaust^ with
a a

black.
coarse-

rests

perforatedplate

covered with

cotton

blanket, and

this in turn

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, is carried up in a the perforated plate. The outlet-pipe

gooseneck
the top. The

on

the outside

of the filter to within

few

feet of

material filtering

is animal

charcoal

or

bone-black.

CHAR

FILTRATION.
.

113

This

is the

granular residue obtained


It is

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 melted
as

distillation of bones.

well.

The

ratio

of bone-black

used

to

sugar

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
proper;

varies

washing the Uquor


Char.

out

of the

char

with

hot

water;

and

the revivification of the char.


"

Filling the Filter mth


upon

^The time of
may

is dependent filling be drawn from of


a

the

speed with which


draw of char

the char

the
cam

kilns.

The

is controlled

by

means

arrangement
retorts.

The

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

of

the

proper

burning of the char

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 in many
to
secure

may

ways

and

there

are

several char with


a

patented
may

devices delivered bent

designed

this result.
means

The

be

into the filter by

of

funnel

slightly

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

stem, the funnel

being turned

intervals

have

man

enter

the

cistern from
a

time

to

time the
a

and

tribute dis-

the

material

with

shovel.

After
up

filter has in the

received
middle.

sufficient

char, this is drawn


with

into

cone

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
"

**

Covering^* the Bone-black

width

of the

filter at

the

bottom

and

rises, forcing the air

114

SUGAR

REFINING.

out

through the
covering.
the

cone

of

char, which

is kept dry throughout


to

the

When

the

liquor begins
is closed The head and is

flow

from
run on

the in the

goose-neck tiie outlet-valve


until filter is filled. the filter and

liquor is
now

put

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

hours. Considerable
on

heat

is

generated when
With the char

hot
at

liquor is first run


a

to well-burned to

char. the

temperature

of

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" 160" and

liquor will be scorched.


most

The the

char

should

be

cooled

to

at

and every precaution filters, should be observed to the flow of liquor to avoid interruptions during the covering period and until the temperature of the outflowing liquor is practicallythat of the liquor entering 150" before it enters the filter. The FiUration,
"

The

washed-sugar liquor from


on

the

bag-

filters (99" four hours

purity) is run
or

the filter at
rate

160" 150

F. for twentycubic feet per

longer

at

of about

sirups from granby dark-colored ulated this in turn strikes (90" purity) and by low-grade bag-filtered raw-sugar sugar-liquors, 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. This is followed

temperature
the filtration. In the

raised

with

each

reduction
one

of

purity.
a

Each in

grade of liquor follows the preceding


where soft-sugar refineries,
are

without

break

low-purity liquors of

all the liquors which essential, not used are to filtered. The produce granulated sugar are double or triple 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

second

and

third

re-filtration

removes

color, but

does

materiallyraise the

purity of the

liquors.

116

SUGAR

REFINING.

and

in

of general consist essentially


gases

casing through which


Deflec
of

the waste conduct The

from char

the kilns

are

drawn.

the wet

char enters and

slowly over the driers carrying about


with
a

the surface
20 per

ting-plates this casing.


of moisture

cent

leaves them

about

3 per

cent.

The

kilns consists of

furnace of

fired at both

ends and

flanked the

by double or char slow'y


cross-section and heat
10
to

triplerows
passes. 3 inches

pipe-retortsthrough which
are or

The

retorts

of cast
3
are

iron, of oval by
to

12 feet

by 9 inches long. The retorts

inches heated

12
a

inches

dull red

to

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

some

carbonates the washing the


pores

which in

This

carbon

remains

of the

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

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

The

char

is

to the filters.

cooled

through
screened is

its way the to cold water is circulated. which


to
remove

If necessary the char is further filters by passing it over pipes The bone-black before is it

the finer

and particles

the dust

again filled into the filter.


New char is added from time
to

time

to

compensate

for

the

loss in
in

is shown

screening. The char the next paragraph.


in the in
course

gradually deteriorates,as A refineryusually renews


of every two

all of its bone-black The dust is used


or

making

phosphoric acid
and

three years. for use in the


or

defecation
The

is sold for fertilizer manufacture. Its Alteration

Composition of Bone-black
new

by Use,

"

Analyses of
of

bone-black after

of American several months

manufacture of
use,
are

and here

the

same

black

given:

CHAR

FILTRATION.

117

New

Black.

After months'

six
use.

Carbon Insoluble Calcium Calcium Calcium


Iron

9.61

10.80

silica
. . . .

.59 .16 .06 8.92 .06 80.70

.67 .55
.24

sulphate. sulphide.
.
.

carbonate

4.48 .23 83.13


100

Undetermined.
.
.

100

Weight Weight
mesh

per per

foot,loose cubic foot,packed.


....

cubic

43.8 48.5
. .

lbs.

54.5 59.1

lbs-

Percentage

between

16

and

30

sieves

84.8

Bone-black

always contains some nitrogen, which is apparently The essential to its decolorizing properties. r61e
not

this black
must

plays in the filtration has


contains be
a

been

determined.

New

considerable since

amount

of ammonia

which salts,
a

removed,
must

they would

have

detrimental
reason,
use

efifect upon
new

the color of the filtered be

liquors. For this


and burned

char

throughly washed

before

for filtration. As with is shown


use.

by the analyses,the composition of char alters


carbon increases

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. The 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

to increase

as

the

around

5 per

cent.

The

iron increases

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

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

the sugars

boiled from

them.

bone-black

may

become

118

SUGAR

REFINING.

"

unfit for
cent. constant content

use

if the calcium

content exceeds sulphide


and

0.4 per

Thorough
addition from

washing
of
new

burning, together with the black, will prevent the sulphide

becoming abnormal.
on
"

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

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

while
extent.

the chlorides and

nitrates
or

are

not

absorbed

to any to
a

great
much

Invert-sugar
than
water.

"glucose'' is absorbed
but is

greater extent
with the hot

sucrose,

largely washed

out

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.
'

presupposes

correct

control

and

well-burned

char.

With

acid-liquorsor
inversion In from
may

burned insufficiently
occur

char, heavy losses by


will
40 60 per per

in the filters. absorb


cent
cent

actual 80 to 85

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


or

of of

the mineral the

matter

"ash," and

from

50

to

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
system
of

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 slightly yellow 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

CRYSTALLIZATION

OF

THE

SUGAR.

119

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

to make

granulated

sugar

Where filters of
same a

the "set"
set
are

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

system

fication. necessityfor a rigidclassiThe distribution on the pan-floor is made to suit the needs of the boiling-system. The vacuum-pans used in refining do 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 of boiling necessity as regards sugars to certain specifications hardness and of the The size the crystals. factory raw-sugar uniform aims make of size to and hardness a only usually sugars and other of grain. In boiling hard granulated sugars, is maintained a high pan-temperature (180"), while for which small low soft sugars, in a grain is desired, 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. "off-color" sugar which is disposed of by This is a slightly and slowlymixing it with the better grade of grangradually ulated time
"

and

there is not

the

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 with the washed raw purity)and are melted directly sugar. strikes boiled back these from The are on a sirups footing strikes of about 67" purity. These of fourth liquorto make The

See

page

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

factory.

I.J

120

SUGAR

REFINING.

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
magmas
are

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

and

washed

with

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, white to a deep brown from almost an pure sugar. varying The lower grades of liquorsfrom a set of char-filters are boiled
form

the residual

sirup or

"barrel

into

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
a

series of strikes of

successively lower

sirup.
55.

Drying

and

Finishing
the such
very

the

Product.

"

The

tion separa-

of the

from crystals

centrifugalmachines
The
to

sirup in the magmas used in the as are thoroughly washed

is effected factories

by
.

{42)

white
remove

sugars

are

in the machine
con*

all

veyed
The
for
one

from

are sirup. The moist sugars the centrifugals above to distributing-bins

adhering

the

granulators.
bulk of the white

drying. The
another, hence
The and
20

through the granulators granulator also separates the crystalsfrom


sugar

is sent

its
an

name.

granulator is
feet

iron drum

(Fig. 17) about

feet in

inclined to the horizontal long, slightly 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.

diameter

DRYING

AND

FINISHING

THE

PRODUCT,

121

means

of

steam-drum
or

extending through the middle


ot steam-pipes
at

of the

granulator
end of

by

large group
The air
an

the

dischai^
pipes
fan and also of
a

the the the

drum.

is drawn exhaust

over

the

through
removes

granulator by sugar-dust.
the usual
are

fan.

The

The

illustration American

(Fig. 17) is
in

Hersey
Two above lower

granulator,

type.

granulator-dnims
the other. with
a

usually operated
is fitted with
drum.
a

series,one
and the

The

upper
steam

heater

central

The

sugar

leaves
very

the little

upper-drum
steam

partly dried
t"

and

quite
the

hot,

hence

is required
sugar

complete
the

drying in the lower


drum

section.

The

should

leave
110". for

lower

comparatively
necessary to

cool,
make

preferably below special provision

It is sometimes
sugar.

cooling the

If sugar

is packed

Fia.

17.

while

hot it is very
the
to

liable to cake
to
a

in the of

packages.
which the

The

sugar

falls from

granulator
the size of

set

screens remove

classify it lumps
and

according
coarser

the

crystals,
the

dust,
The

and

deliver
sugar the

products
requires.

into

the

packingand
rest

bins. other

screened
as

is

paciied

in barrels,

bags

such
upon

containere

n.arkct

Barrels
are

"shakers"
with

while

filling. Certain

refineries

equipped
ot
sugars

lai^e storage-bins which


the day-time only.
machines
are

permit the packing


in filling, weighing
cut

during

Automatic
small

used and

and

ing clos-

packages.
The

Cubes

loaf-sugars

are

packed
or

in cartons.
cubes
or

European

practice of wrapping
paper,

two

three

"dominoes"

in moisture-proof into
or

for restaurant
States.
are

service, has been


The various
sugar

introduced
of lumpproper

the

United

kinds
oi

loaf-sugars
a

all made pure

by

mixing

the

grain with

heavy

sugar-

122

SUGAR

REFINING.

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

directlyor
closets. dried. sawed The

slabs

and
are

bars.

The

cubes

usually dried in hot ready for packing after they have been
are are

These

slabs and

bars

cut

or

sawed

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
same

way.

The

soft

sugars,

white
sugars

and
are

described. from the

These

yellow, have already been packed while moist, directly

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 as extra crystals 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. As

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."
"

has

been

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

55** Brix

and

reboiled

"smooth"

before

barreling.

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

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

This

upon

other

factors.
34
water

follows:

Polarization
6 per

per 22

cent; ash
16 per 57.

cent;
of

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

cent.

Yield

Refined

Sugar.
in

"

The

yield of
terms

sugar
raw

in

refinery is

expressed

percentage

of the

124

SUGAR

REFINING.

and a sampled and analyzed, as in the case of raw sugars, weighted average analysisis calculated for the period. The barrel-sirup is 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
"

"

volume
per

of the

material
as

in cubic

feet and

cubic

foot,

indicated

by the

pounds solids density. The solids

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. available To

compute

these

to available sirup and figures

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. Then:

Lbs. Per
cent

solid solid

impuritiesin stock

X 100

impuritiesin sirup produced


=

lbs. available

sirup in stock;
to

(1)
aa

loss

figure would
than the

not

be
as no

of

more now

practical value customarily


temperature

the

refinery,
This

such,
to
a

number

determined.

refers The
are

refinery

having
and

exceptional
of

conditions. data

complications prohibitive.
It is not would This
not

expense

securing
closer of

accurate scientifically

clear, however,
be desirable would
or

that in

approximation
excessive
a or

to

true

figures

locations

and of

irregular heat.
the

condition

necessitate of of
a,

either
more

control less

laboratory
Dr. shown

temperature
C. A. Browne corrections above The 96"

corrections

arbitrary
p.

nature.

(Handbook
may

Sugar

Analysis, applied
to

260)

has

that

only
to

be

properly
of the

cane-sugars

polarizing give
are

and

beet-sugars.
statements

technical

refinery

are

designed
fluctuations Under with

to

tive comparasive exces-

control' figures and

where
very

temperature

not

they (G. L. S.)

accomplish
one

this

successfully.
is

average

ture tempera-

conditions,

report

comparable

its

predecessors.

INTRODUCTORY.

125

Lbs,

available sirupin stock X polarization of sirupproduced


100

=ibs. Total in

sucrose

in in

sirup in stock.
stock
=

(2)
lbs.

sucrose

stock"

sucrose

sirup in

available

granulatedin

stock.

Example:
Assume
a

stock

in process

of 1,180,000 lbs. solids

^50,000 lbs.

sucrose

330,000 lbs. solid impurities.


Assume
a

barrel-sirup produced

as

containing:
34.2%
,
.

Sucrose Water Solid

22.1% 43.7%
100

(ash,glucose,organic) impurities

330,000X100^
43.7
'

lbs. available

sirup; H,

(1) V /

778
"

032X34.2

^=258,261
100

lbs.

sucrose

in

in.stock: sirup y

(2) \ /

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


The stock
at

increase in process

or

decrease the end

in

the

available
as

at

of the

period

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.
the These of
raws

net

weights produced
to

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

melted

126

SUGAR

REFINING.

melt

can

be

totaled

to

give the analysis of the combined

output

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

of the

increase of

decrease

of each

constituent

during
of net

the

process

refining.
To illustrate let this,
us assume a

set

yields for

refinery period and calculate the loss in


Polarization Net of the melt.
. .

sucrose

for the

period:

.94.9** 84.

yield of granulated Soft sugars produced Net sirupproduction


Then,
Sucrose in melt

3% 8.9% 4.6%

at 88.8** at 34.1"

polarization polarization

94
.

90

84 Sucrose in

3X100
'""
"

granulated %

melt

"

84
.

30

9X88

8
=

Sucrose

in soft sugars

% melt

7 90
.

4.5X34.1 Sucrose Sucrose Sucrose


. "

or

sirup

1 melt

^ =
" " "

1
.

63 93
.

^"

in total lost in

product %

melt

73 17
.

refining% melt
same

Following this
loss of be traced. Rouiine

method

of and

the gain calculation,

or

invert-sugar,ash, water
Control. The

organic
control
of

non-sugar-

may

"

routine

depends largely upon


materials filterand in the

determinations

of the refinery the purity of the


The char-

successive
are

steps of the

process.

controlled on a basis of purity. entirely of these purity tests required day and night is The number in a separate so large that the work is usually conducted by boys trained floor, 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.

pan-work

SPECIAL

ANALYTICAL

METHODS.

127

The
work.
any

dilute
The

purity method
"

of Casamajor is used
"

in this
to

material

convenient the

or ^liquor, magma density,usually between

sirup is diluted
15" and A 20"

Brix,
tion solu-

and

corrected

Brix

is determined.

part of the
of

is clarified with

Home's

dry

subacetate

lead, if such

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
'-

are

computed
The

from

the

formula

Factor

-;

TTT**

figuringis simplified by the


use

use

Sp. gr.X degree


of Home's
on

Brix

table of

for purities

in

refinerycontrol,given
Black Paste. ^A

p"ge 526.
59.

Special

Analytical

Methods. for

"

"

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


convenient follows: with Make Titrate Wash
10 grams

method ri^tine

of the
up

paste into
the

200-cc.
a

flask rod. filter.

distilled water,
up 20 to the
cc.

breaking

mark, mix

lumps with thoroughly by shaking and


of the

of the filtrate (1 gram

normal paste) with tenthThis The

using methyl-orange as the indicator. alkali^ hydrochloric acid. gives the aciditydue to uncombined
number
X 0.365=

of

cc.

of
cent

N/10
free

with methyl-orange alkali,

indicator

hydrochloricacid (HCl). 20-cc. portion of the filtrate, Titrate a second using pheThis titration gives the total acidity indicator. nolphthalein the free acid. The culations caldue to the acid phosphates and
per
are

made

as

follows:

Number
cc.

of

cc.

N/10

alkali

with
orange

phenolphthalein indicator"
indicator X 0.35=
per cent

N/10

available

alkali,methylphosphoric acid

(P2O5). 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
"

Bone-black:

of particles and
a

iron'that

may

have
100

gotten into it from


grams

the retorts

filters.

Grind

about
to
a

of this

prepared char in
should
must pass

porcelain mortar
a a

powder, all of which


The

through kept in
moisture,

lOO-mesh

sieve.

ground
to

tightlystoppered bottle

be sample prevent absorption of

128

SUGAR

REFINING.

Bone4)lack:
the

Moisiwre

Determination.

"

^Heat

grams

of

unground
'

portion of the subsample


Carbon and
10

during four
^Treat

hours

at 110*' C.

Bone-black: of the acid

Insolvble
cc.

Moiter,

"

2 grains

ground char with


50
cc. a

of concentrated

hydrochloricthe residue

and

of water. tared Gooch

Boil

gently for fifteen minutes,


and wash

filter through with


water to

crucible

the

and

contents

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

weight
Loss

over

the flame

of

lamp.
cent per

on

Residue

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

carbon;
cent

insoluble

matter.

Bone^lack:
grams water

Determination

of Calcium

Sulphate. ^To 2,0


"

of the and
100

powdered char, in a 250-cc. flask,add 25 cc. concentrated hydrochloric acid, gradually. cc.
Add about. 100
cc.

Boil fifteen minutes.

water, and
with of

after

cooling to
mix and

room

temperature,

dilute to the mark


200
cc.

water,

filter.

Evaporate
150
cc.

the filtrate to described


as

about

Proceed

char) of with the analysis as is


20 grams

in page The

362, using the concentrated


barium

solution obtained

above.

washed

by
20

sulphate -5(CaSOO.
grams

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

Bone-black: of the

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

slowly.
described

Proceed above.

as

in the determination Great


care

of calcium in

sulphate,

must

be exercised

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

SPECIAL

ANALYTICAL

METHODS.

129

Bone-black:

Vclumelric

Determination

of the Iron,^
Dissolve
Check

"

^The

followingreagents are required: potassium permanganate: (1) Standard


grams

to

of the salt in 1000


an

cc.

of water. known of

this solution
aa

against
follows:

iron

solution
2.5 grams

of

strength, prepared
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 the conditions of the

Dissolve

piano-wire, or

analysis,as below,
solution: Dissolve

standardizing the permanganate. (2) Phosphoric acid and manganous


grams

50

water,
add 250 followed

of manganous with the addition


cc.

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

in order

by 150 sulphuric acid.

of water

and

100

cc.

of
may

centrated con-

The

phosphoric solution

be

prepared

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

grams

of pure

granulated tin
with few

in 125

cc.

of concentrated is

hydrochloric acid,
of
a

heating. Solution

promoted

by the addition

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.
(4)
Mercuric
cc.

chloride of water. the

solution:

Dissolve

50 grams

of the

salt in 1000 Proceed the

with

analysis as follows:
and

Ignite

10

grams 30

of
cc.

powdered

bone-black

digest the residue with

of concentrated fifteen minutes. and hot wash


water.

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

the

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 Heat

and

manganous

solution and

600

cc.

of water.

Adapted

from

Clowes

and

Coleman's

"

Quantitative

Analysis,"

5th ed., p. 206.

130

SUGAR

REFINING.

The

titration of the in the


may

material

prepared as
over
a

above

may

be

conducted the The and the

flask be

placed

solution

transferred

flask,in the
the

washings

latter case, added to the

background or a large porcelain dish. should be thoroughly washed


to

white

solution

in the
9,

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
permanganate
iron wire solution.
to

standard

solution

from

ascertain

the

iron

value

of the

permanganate
be

The

percentage of iron in the char may


the data obtained Calcium Carbonate in the two and

readily
"

calculated from Bone-black:

titrations.

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 are analysis Bone-black: ^The test Thoroughness of the Revivification, 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 (underin proportion burning), the depth of the color being directly 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 solution

when

the char is heated into

so

hot that Should

is converted remain

the oxide.

the

uncolored

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

SUGAR

REFINING.

the

colors

of

the

filtrates and

unfiltcred

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. bone-black
many

should
tests
are

be

kept

as

standard

of

comparison, if
ditions con-

such

to be made.

It is essential in all tests of this character of the

that all the

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
be chosen In
to
so

suit the

temperature, etc., should


The
means

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

be maintained.

decolorizing power
of
a

by

colorimeter. convenient

Stammer's

instrument

for this purpose

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

very

color

of

colunm

of

sugar

solution
so

with

standard

coloredthe
one

glass plates. An
of the of
a

eye-piece is
under

arranged that
appears upon

color half

solution

examination

disk, and

that
a

eye-piece and
lowered column

by
of

means

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

of the standard

solution
on
a

being varied
scale

at

the
of
a

same

time;

this

length is shown

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. by
means

the
as or

object is
the disk

to

equalize the intensities

of the

colors

seen

on

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

be made,
to
an

or

the

reading

on

the

scale may

easily be reduced
as

expression showing the


the standard.

depth of color

compared

with

SPECIAL

ANALYTICAL

METHODS.

133

This

instrument power
of
a

may

be in the

used

in

determining
manner;

the

izing decolor-

char

following
should used. be

standard-color
a

solution

prepared Duboscq Prepare

with recommends the

mel, cara-

definite
per

quantity
liter
pure

being

grams

for

his

instrument.
to

caramel until all

by
of

heating
it is the

cane-sugar

about

215"

C,

decomposed.
depth
of

In color in of certain

examining
the this standard solution
of

bone-black, solution,
with
a

mine deterthen

heat

measured
of

voliune char
a

weighed example,
of

portion
half color.
an

the

length

time,
the

for

hour,
The

filter,
difference

and

again
the

determine
of
of

intensity
to

in the

depth

color,
the

referred bone-black bone-black for

the in of

standard,

represents
In

efficiency
work is
a

decolorizing.
a

sugar-house

standard

known

decolorizing
results and

capacity
can

convenient be
to

comparison. by

Comparable
certain The the volume Fill certain take
the
a

only adhering
may
as

obtained them in all

adopting

conditions

experiments.
in

decolorizing
absence
of
a

power

be

roughly
Treat
as

determined,
a

of

colorimeter,

follows:

measured above.
to
a

standard-color similar
to

solution those used

described

cylinder, depth
same

in and

Nesslerizing,
filtered

\vith
volume add
same

the of
to

decolorized
the this
as

solution;
in
a

standard latter
of

solution
from
a

similar until solution


over
a a

cylinder, portion
shows white
of

and the
same

water

burette

depth

that
of color

the when

decolorized examined added


of

the

intensity
The the

background.
to

volume

of

water

is char.

inversely

proportional

decolorizing

power

the

SUGAR

ANALYSIS.

CHEMICAL

CONTROL

OF

THE

FACTORY.

SUGARS

AND

OTHER

CONSTITUENTS PRODUCTS.

OF

THE

CANE

AND

ITS

60. the

Sugars.
sugars

"

^In

the

manufacture in the

of

sugar

from
are

cane

of
and
or

importance
levulose.
cane-sugar,

analytical

work

sucrose,

dextrose,

Sucrose,
Dextrose

is the and them


are

most

important
other

of

these.

and

levulose,
with

possibly by
of

reducing-sugars,
chemists under of their The A table

usually grouped
the
"

cane-sugar
on

name

glucose,"

importance manufacturing
as

account

influence
sugars
are

in

anal3rtical and
classed
more

processes.

chemically important
is
sugars

carbohydrates.
and
page

showing
of the

the

chemical
on

physical properties
458. A
few
concern

carbohydrates
of
a

given

of

the the

properties
chemist of

those
cane-sugar

which

immediately
are

factory,

given

in

the

following

paragraphs.
01.

Sucrose,
"

Saccharose,
is very

Saccharon,
distributed refined
to

or

Cane-

sugar.

^This sugar and

widely
is the it its

in the

vegetable
conunevce.

kingdom
In
a

in its pure of the

state

sugar

of

classification of

sugars

belongs
formula
are

the is

disaccharides,
The the

derivatives commercial
sugarcane

hexoses,
of

and

CijHjjOn.
sugar-cane,

sources

cane-sugar

the

beet, the
is often the
a

maple-tree, and
very

certain

palms.

The

sorghumcane,
not

rich

in of

sucrose,

rivaling the
from
very

tropical

but been

manufacture commercial
are

sugar

this

plant

has

success,

though
made from

large quantities
all

of

table-sirup
of the United Sucrose hemihedral

annually
States.

it, in nearly

parts

crystallizes in anhydrous

the

monoclinic

system,
The

forming specific
134

transparent

crystals.

DEXTROSE.
.

135

1710

gravity
crose

of

the

crystalsat

prjs

C. is 1.58046 and

(Gerlach).
alcohol.

SuIt

is

readily soluble

in water in absolute

in diluted

is

practically insoluble
anhydrous

alcohol,ether, chloroform
or

and

glycerine.
free of raffinose of

Dry
heated it melts
at

sucrose,

other

to
at

temperature
a

120"-125"
of

be impurity, may C. without browning; Moist


sucrose

temperature
above

160" 100"
84.

C. C.

poses decomand

temperatures
sucrose

The

action

of acids

salts

on

is

given in

Sucrose many

is not

directly fermentable,
sugar.

but invert

is converted
sugar to

by

ferments

into invert

The in

promptly

ferments. is

Further
on

information
409.

regard
other

fermentation

given
Sucrose

page

in of

common

with

many

substances
a

has
ray

the of

property

rotating the
the This

plane of polarization of
to

light.

It

rotates

plane
property

the

right and

is termed shown for

dextrorotatory.
(see 67),
the
in

is utilized, as of

will be

the

construction

polariscopic apparatus

analysis of
62* Dextrose.

sugars.
"

^This sugar
where

is also

widely

distributed

in with

the other
to

vegetable kingdom,
sugars.

it is found is

in mixtures it

Its chemical

formula hexoses.

CgHiaOe and
is

belongs
ent pres-

the in

monosaccharides,
sugar-cane, in formed and

Dextrose
sucrose,

always
it and

on

inverting
rhombic the melt
at

levu-

lose

are

equal quantities.
forms

Anhydrous point
is

dextrose

crystalswhose
forms C. in 80P-90" and

melting
crusts
or

144"-146"

C,

and

hydrate

transparent
Dextrose

crystals which
is

readily soluble
the

in water

alcohol, the
and

solubility in the latter varying with


It rotates

its dilution

ture. temperato

plane of polarization of light


for the detection and

the

right.
The chemical
are

methods based
upon

estimation

of dextrose of
to

its property, and

in alkaline

solution,
oxides the

absorbing
lower of

combined The
to

oxygen

reducing
utilized in For

metallic

oxides.

reaction
cuprous

analysis is

reduction
of dextrose,

cupric

oxid. 458.

other

properties

refer to the table, page

136

CHEMICAL

CONTROL

OF

THE

FACTORY.

63.

Levulose.
and
sucrose

"

^This sugar in sugar-cane. fructose


or

is

dextrose and

usually associated with It is widely distributed,

is often

called

monosaccharide, hexose shining, needlenshaped crystals of


which
are

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

system,
tals crysof levulose alcohol. The

hygroscopic and
at

difficult to The chemical soluble

produce.
formula in water

melt
is

95"-105"
sugar

This CflHigOfl. the

is very

and

It rotates

is therefore

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

quantity of levulose is small


Both and these
sugars
are

compared with
present

the dextrose.

often

only

in faint

traces,
small

the levulose is absent. occasionally Even though levulose be absent or present in

in very

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

large proportion
of

increase
may
occur

levulose when
no

has direct

been

inverted.

Such
a

molasses
very

will often
true

have

low

polarization and
or

high,

sucrose-

number. The action


reappearance

increase

of levulose heat

is due
upon

to

the

of alkaUs
A

and of

salts of alkalis with dextrose

the dextrose. levulose. be isomeences refer-

part
under

the

is converted levulose There chemical

into
may
are

Likewise rized and


to

similar

conditions

converted this

into dextrose. in the

many

phenomenon
note

and

technical

journals.
It is direct
to interesting

that according to de Haan


of
a

the

polarization and
differ but Invert and

Clerget numbers
Uttle. When
sucrose

carbonation

cane-molasses
64.

Sugar.
other

"

is acted

upon

by
ture mix-

acids

certain

reagents

it is converted and
or

into The The

of is said

equal parts
to

of dextrose

levulose. inverted.

sucrose

have

been

hydrolized

mixture

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

"reducing-sugars" and
tories. cane-stigar labora-

"glucose"

are

used

synonymously

in the

Verbal

commtinication

and

Archief, about

1910

or

1911.

ABNORMAL

CONSTITUENTS.

137

65.
"

Abnormal There
are

Constituents
a

of

Sugar-cane

ucts.^ Prod-

while

not

of compounds large number occurring normally in the juice of the their appearance the in the
cane
or

which,
cane,

yet

make occasionally
ous

and

its

ntuner-

products, as
products

result of fermentation
process

of destructive These mal abnor:

influences

during the
may

of manufacture. classified
as

be

roughly

follows
same;

firsts

sugars

and

closelyrelated
A few

derivatives

of the and

second^

the
eous

gums;

thirdfacids; fourth^alcohols
of these
numerous

esters;

fifthgaa,

products.

compounds

may

be

briefly mentioned:
1st.

Sugars

and

closely related derivatives


^^" been
These upon

of the
'

same.

Mannose,

CJEl^fi^f^^^
two

non-fermentable Pellet
are

sugar-glucose
in cane-molasses

CcHjjOq
from action

have

reported by
dextrose and

Egypt.

products
amounts

produced They
when
an

by^ the
occur excess

of alkalies in been

levulose.

in

cane-molasses
of lime has

perceptible
used
in

only
is formed

the

clarification.

Mannite
amount

(C^Rifi^).
through
and the fermentations

This

body

in considerable and levulose in

reduction of ketoP in small

of dextrose

certain

juices and

sirups.
have been

Glycerol
reported

(CgHgOa)
in 2d. The Dextran troublesome of various

Dimethyl
molasses

(C^HgO^)
amounts.

fermented Gums.

(C"Hi()05)n. This
enemy

gum,

most

common

and

of

the

sugar-maker,
as

is

the

product

fermentations,

such

that

produced

by

the

Leuconostoc in
canes

(Froschlaich), and

is of
or

frequent
insect
soon

occurrence

injured by
of

freezing
gum

by
canes

ravages.

The them

formation wortliless three into

this

viscous

in

renders

for

milling. Its
that of
sucrose,

high specific rotation


introduces
a

(+200),
error

times
the

serious

polarization

of

cane-productS| unless
through
author's the

the

gum

is

This

article who of

(65, 66) is included prepared


the 5th it at the International

courtesy

of

Dr.

Charles

A.
*

Browne,

request. of

Report

Congress

Applied

Chemistry,

3. 383.
"

Browne,

La.

Planter, 1905,

p.

237,

vol.

31.

138

CHEMICAL

CONTROL

OF

THE

FACTORY.

first removed

b^ alcohol.
A found

Hydrolysis
by
and
was

of

dextran, with
Steel
in

acids,

gives dextrose.
Levan.
gum

Smith

and

cane sugar-

products in Australia
formans. in
raw

produced by the Bac. levanifound


to

This sugar;

organism
it
causes

be

very of
a

destructive
sucrose

rapid inversion
has

and

produces the slimy


of "40. Cellulan. A

gum,

levan, which

Hydrolysis
gum

of

levan, with by

rotation specific acids,yieldslevulose.


'

found

Browne

in

the

tanks

of

sugar-house
of

in Louisiana.

It is formed

in certain of

tions fermenta-

cane-juice and
treatment

sirup, and
alkali with reactions blue

consists

laige leathery dextran).


a

lumps
The

insoluble
on

in caustic

(distinctionfrom
of cellulose with

gum

boiling alkaH
coloration

yields

uct prod-

giving cuprammonium
and

all

the and
on

in (solubility zinc-chloride into

iodine), and
Mannan. A

hydrolysis with
found

acids is converted

dextrose.
gum

occasionallyin
sirups.
mannose.

the

sedementary
of

deposits of fermented
mannan,

juices and

Hydrolysis

with

acids, gives

Chitine

(C1SH30N2O12?). This

substance, which

strictly
*

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

by Browne
molasses

in

fungoid origin and

on

hydrolysis with

hydrochloric

5^elds

an

amine-sugar, glucose-amine

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

Formic, acetic,propionic, butyric, capric,and


acids of the

various
among In

other the tion addias

fatty series, have


of

all been

found

fermentation-products
to very

cane-juices and
acid in should be

sirups.
mentioned

the

above,

lactic

of

common

occurrence

juices, sirups, and


either

molasses. action of

The lime

latter
upon

acid the

may sugars

be

formed

by the
Oideum

of the

juice during clarification, or organisms,


"

through the
Bac.
^

agency

of various

as

lactis,
"

lacticus, etc.
'
" "

^ a

International
La.

Su^ar 1905,
p.

Journal,
238,
vol.

4, 430.
34.

Planter,

140

CHEMICAL

CONTROL

OF

THE

FACTORY.

Water.

20.00%
Silica.
Potash.

20.00% Si02
K2O CaO MgO acid, acid,
a 0.60
3
.

50 50
.

Lime,

1 0.

Magnesia^
Ash.
8.00

10

Phosphoric Sulphuric Chlorine, Soda,


etc

PjOs SOg.

0.20 1
.

60

0.40

iron,

etc.,

NajO,

Fe20sf
0.20 32
.

fiusan

62.00

Sucrose Dextrose Levulose Albuminoids Amids Amido

00 00
.

14

16. 0
.

00 30

(as
acids acid

asparagin)
(as aspartic )
. .

0.30 1
.

70

Nitrogenous

bodies.

3.00

Nitric Ammonia Xanthin Other

0
.

I6

(Tot8lN-0.6%).

0.02

bodies

0
.

30

nitrogenous
Araban
, ,

bodies.
.

0.23

Soluble
Free

gums

2.00 2.00

( Xvlan

Pectin.etc
.

)
Sac-

2
.

00

acids acids

j Melassinic,
( charinic

Glutinic, acids,
etc.

Combined

3.00

00

TotaL

100.00%

100.00%

Molasses
"

also
the
amount

contains
of

small

quantity
upon

of

carmelization the

product,
of

these

depending
Caramel is mixture

ture temperaformed dark-

evaporation

and

boiling.^
and
a

is of

always
several

by

overheating
bodies

cane-sugar

colored

of

uncertain

composition.

Caramelan,
3d

Caramelen, ed.,
1210.

Caramelin,

tee

von

Lippmann,

Ch"unie

der

Zuckerarten,

OPTICAL

METHODS

IN

SUGAR

ANALYSIS.

APPARATUS

AND

MANIPULATIONS.

67.

The

Polariscope.
of

"

The

instrument

used

in

the is

quantitative estimation usually


and
**

sugars

by the
The
names

optical methods
'*

called

polariscope.
are

polarimeter'*

saocharimeter"
common

also
many

sometimes

used and

Sucrose, in
has
ray

with of

sugars

othei'substances,
a

the of

property

rotating the
is taken

plane of polarization of
of this

light. Advantage
of the

property

in

the

construction The

polariscope.
ray

polarization of the
it into
a

of

light is accomplished prism is made crystal of


are

by
a

passing
spar.
so

Nicol from

prism.
a

This

from Iceland

rhombohedron The the end

cut

transparent
each 68". A

surfaces

of the
are

prism, Fig 18,


The and

ground ofif
is then the

that

acute cut

angles
into

prism
B,

two

parts,

through
are

obtuse and

angles and

the

surfaces

polished
forms

cemented

together again, in their original


Canada
are

positions, with
of will On it is is the
answer

balsam. but this

Other

prism
passing

used,

description
this
ray,

for the
a

present
of
an

purposes.

ray

light into

prism
which

separated
from
an

into the

reflected

ordinary prism by
or

the

balsam
ray,

ceinent,and
which
Fio.
18.

extraordinary
through
the

polarized

passes whose

polariscope
construction

and of

upon

properties the depends.


three should sugars be
to

the

instrument remarks

Confining
the
cane-sugar

our

of most noted

interest that 141


sucrose

to

chemist,

it

142

OPTICAL

METHODS

IN

SUGAR

ANALYSIS.

rotates

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 the

plane

of

rotates

the
sugar.

plane

to

the

left and
two

is

or laevorotatory,

left-

hand and

Quartz is of
in certain due

kinds, right and

left hand,

is used

to compensate types of polariscopes

for the rotation The

to sugar.
rotate

of a sugar to power differs for different sugars. determined under certain

the number

plane

of

polarization

The

standard

expressing this, as conditions,is termed the

specific rotatory power. passed through sugar solutions of of the solution different concentrations, or through columns
If the

polarizedray

is

of different

lengths,it
with

will be

observed

that the

the

amount

of the

rotation

varies

the

strength of
Iceland of the

solution

and

length of the column.


These
'of properties sugars, spar,

and

quartz

are

utilized in the
them

construction

polariscope,and
the various
will be

keeping

in

view
as

the

descriptionsof
on,

instruments,

given farther
be divided

types of stood. readily under-

Polariscopesmay
and
may

into two The

shadow viz., classes, shadow-instruments

transition be

tint-instruments. into

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.
A will brief be

subdivided

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

sufficient referred

the

purposes

of of the

this book.

The

reader
more

is tailed de-

hand-books

polariscope for

descriptions of the
instruments.
68.

theory and

construction

of

the

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

shadow

"

the

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

HALF-SHADOW

COMPENSATING

FOLABISCOPE.

143

at

(r

is

plate ot levorotatory quartz, by


fixed scale
means

at

"

is

quartzP is
a

wedge
vernier.

movable

of

the

screw

M,

and
is

at

quarts-wedge,
The

in
upon

position,
which

to to

wliich note

attached distance

the

the

the

quartz-wedge
rotation
an

E the

has

t"een of

moved,

in compensating
to

for

the

of

plane

polarization due
is attached the
to
are

interpoaing
The

optically active body,

wedge.
of

scale
of

is

graduated,

for

technical

work,

read

percentages

cane-sugar.

These

quartz-wedges

dextrorotatoiy

144

OPTICAL

METHODS

IN

BUGAR

ANALYSIS.

The latuB, of

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

constitute
for the

the

compensating
of

appa-

compenaates
as

deviation
The

the

plane
to

polarization,

explained
in
as

above.

Hubstance is placed At H

be

examined,

dissolved

suitable
in
at

solvent,
the

in is used

the
the in

observation-tube,

shown

figure.
the

analyzer,
observing
for

Mirol

prism;
at

7
are

is

telescope

the

field, and
the

the

telescope and
lenses
at

reflector
extreme

reading
are

scale.

The

two

the

right

for

transmitting
lines
to

the the

rays

of

light

from

the the

lamp

in

parallel

Nicol

prism,

forming

polariaer.

The

instrument

described

above

is of the

tion angle-compensais shown scribed de-

type.
in Fig. 20.
in

A This

double-compensating
polariscope
two
sets

instrument

differs from
of

that

already
of

having

quartz

wedges

opposite
arrango-

optical properties
ment

and

two

scales and
in

verniers. 23.

The

of the

wedges

is shown of the
a

Fig,

The the
screw, to

field of vision

above

instruments,
shaded

when If the

set

at

neutral

point,

is

uniformly

disk.
be

milled

controlling the compensating


right
other
or

wedge,
the this disk

slightly turned
will be

the the

left, one-half

Of

shaded
and its

and

light.

It

is from

half-shaded

disk takes

the

compensating

wedges

that

this

in^rument

HALF-SHADOW

FOLABISCOPE

WITH

GLASS

SCALES.

145

double-compensating instrument
Fig. 20. protected from
in The

of recent

construction

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.
.

is shown

wedges
may
rest

have
upon

long
the

stems

so

that A

the hand

of the

observer

glass cell filled with a three of potassium is placed at B per cent solution of bichromate This ray-filter should always be and serves as a ray-filter.^ 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.
69.

table.

Half-shadow
"

Polariscope

with

Glass

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 Jan (Joseffrom dust.
are

The

scales and
a

and

lighted by

engraved on glass are part of the polarized rays which


are

verniers

reflected upon them. Fri6 also make Messrs.

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

'

This

strength of solution product


be of 9.
a

assumes

cell 3

cm.

in length. percentage the


use

For

other

cell of^the

lengths, the
solution
ray

the

length
to

by

the

streaa.sth
of
a

should

According
difference With the

Schonrock in the

chromate bi-

filter makes

of 0.12" filter he No.

polarization w"th
a

white and

light instrument.
without Deut. it 100.12".

obtained

reading

of

100"

(Circular
pp.

44, Bureau

of Standards;

Z. Ver.

Zuckerind.,

1904,

521-558.)

146

OPTICAL

METHODS

IN

SUQAB

ANALTSIS.

quartz-wedge compengating
Byetetn.
The

and

baa

Lippich polorizingmade
to

Readings
of the

may
are

be

accurately

0.01"
to

sugar.

Frifi inBtrumenta

graduated

according
at

the G.

apeciuse

Gcation

International

Commission

20"

and

the normal

weight

of 26 grams

with

the 100

true cubic

meter centi-

flask at 20"
70.

C.

Hall-shadow

Polarfscope
22, is
other

(Julius Peters).
"

This in

instrument.

Fig.
to

double-compensating.
compensation

It is sinulor

principle

the

polariscopes. The

r
148
ANALTSIiS.

OPTICAL

METHODS

IN

BUQAR

According
and
is

to

Wiley

'

this inatniment

ia

extremely

eensitive with

capable of results but tittle inferior to those

the

which Landolt-Lippich polaiiscope,


very

19

constructed

for the

careful scientificresearches. Laurent

72. Laurent for


use

Polariscope
was

(Maison

Laurent),"

The

(Fig, 25) only


are now

originallya half-shadow
monochromatic with with either
a

inBtrument these polari-

with

light, but
half-shadow
or

ecopes

made

triplefield,
for

and
uae

are

also white

provided light.
"

compensation attachment

with

Aaiiculturid Analysis, -1. HI.

LAURENT

POLARISCOPE;. monochromatic of the


a

149

In the

the

Laurent

using polariscope, by
means

light,
screw, to

analyzer is revolved
for the of

milled

compensate

rotation

of

plane
measured vernier. second

solution.

polarization by the sugar The is angular rotation by


The
means

of

scale also

and
a

instrument the

has

scale, called
which read be

scale, on
may As

cane-sugar percentages of sugar

directly.
is
a

stated, there
for
may

device
which end of

the be

Laurent attached

compensating polariscope,
to
as

the shown

front in

the

instrument, permits the


feature

Fig. 2Q, and

use

of white

light.
A
scope

distinctive

polariis the adjustable polarizer. The

of this

Nicol
a

prism

may

be rotated

through
amount
same

small

angle,thus varying the


passes,

of

light that
the

and

at

the the

time

sensitiveness

of

strument. in-

Ito.24.

The

polarized light
of which is thus

is

passed

through
a

disk

of

glass, half
quartz,
This
*

covered the

with

thin feature

plate of
of the

producing

half-shadow

instrument.

type of polariscopeis much


it has
no

used be

in scientific

research,

since

quartz wedges

to

affected

by variations

of temperature.
73.

Transition-ttnt
"

Polariscope.

Soleil-Ventzke-

Scheibler.

^This

in 68

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

radically from
in

It

differs from Nicol

the

half-shadow
at A

ment instrua

having
which
means

additional

prism
The

and

quartz
field is

plate B
varied

produce the
of The the the

color.

tint of the

by
rod

by the

L.

spur-wheel and optical parts at the


as

pinion, revolved
front end " of the Haensch

are polariscope

same

those

in the Schmidt

half-shadow

instrument.

150

OPTICAL

UETH0D8

IN

aUGAB

ANALYSE.

The neutral

field ia colored, and

when

the

instnuneDt
The

is set at the tint for

point the

tint

is unifonn.

eensitive

most

eyes

is the

rose-violet.

The

tint

may

be

varied

by-

revolving
74. scopea in

rod

L. Remarks
are

General

upon in

Polariscopes.
construction
to

"

Polari-

general
and

aimilar

the

typies

described, differing only


Half-shadow
used. These

in detwls

of construction.
are

instruments triple-field
very

most

ally gener-

polariscopes are
type
of and is

sensitive and
is

reliable.
used

The

Laurent and

saccharifneter except
but
a

extensively
outside
a

in France
ments

Belgium,
work

the

higher-grade
and

instruthose

in

research The

little used
room

countries.

necessity of

dark

monochn"-

GENERAL

BBMARKS

UPON

POLARI8COP"B.

151

matic

light render
tor
for
use use

the

factoiy
modified The

in the with

originalLaurent polariscope u industry. The Laurent cane-sugar


light is
United
a

white

convenient

instrument.
used have almost been

trauHit

ion-tint instrumenta
the

were

formerly
States, but

exclusively, especially in

largely replaced by shadow


obviously,
or

polariscopes. Tint instruments,


with accuracy

cannot

be

used in the
to

by

persons

more

less color-blind, and

analysis of dark-colored
secure

materials
are

it is

frequently difficult
for observations.

solutions
,

that

dear

enough
All
200
mm. a

polariscopes
long, and half-length
are

are an or

fitted
instrument

to

receive

observation-tubes

of this size is also supplied


tube. Other

with

100-mm.
COO
a nun.

polariscope factory
the

lengths
A

400

mm.

and

400-mm. the

polariscope is
process, is

satisfactorylength (or
with tlie diffusion

using
fiOO-mm.

milling
"ze

but

process

preferable.
Scale. Veatzke
are

75. Normal
either

The

Polarlscoplc
"

Scale. divided
to

The read

Weight.

Polariscope scales
or

circular degrees
instruments

percentages

of cane-sugar

oii.both. Ventzke
or

Commercial
cane-sugar

usually

liave

only
so

the

scale.
or

The certain
the under

Ventzke

cane-sugar the
to

scale is
be

divided

tliat,if
observed

weight

of

material
100

dissolved
centimeters

in water
and

and

solution

diluted

cubic
in
can a

standard in

conditions
of

200-nim.

tube, the

reading

will be

percentages

152

OPTICAL

METHODS

IN

BUQAB

ANALYSIS.

used, the reading


these
"

will
to

be

100.

The

weight required under


readings
of the
is termed the In

conditiona

give percentage
or

normal

weight"
work,

the

"

factor"
the

instrument.

^lommercial

eepecially in

polariaation of

sugars.

the

divudoDs

of

the

cane^migar

scale

are

usually tenned

"degreea."
The
are

nonnal

weight
used

for

the

German
the

instruments, which
world,
as

very

generally
The

throughout
of this

adopted b;
is 26
must

the grams.

International

Congress
with

Applied
normal

Chemistry,
weight

flask used

hold

MANIPULATION

OF

FOLARISCOPE.

153

100

true
must

cubic be
secure

centimeters

of solution the

at

20" C. be

The made

tion soluat

prepared and
correct

observation

20" C. to The used


100

results.

normal original is 26.048


grams

weight and the


and the material
or

one

stillmost be

geneially
in of

is to

dissolved
'see

Mohr's

cubic is to

centimeters be

Mohr*s

units
at

80)

solution,and
The
grams
to

prepared and

observed

17i" C.

normal

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

100

cubic

centimeters

at

20" C.

and

be

observed

at this 76.

temperature.

Manipulation
solutions and

of

Polarlscope.

"

Methods

of

preparing the
dissolved
to be

will be -described normal

in 80.

Having
material the and

clarified the

weight of the
with
a

fillan polarized, solution and place it


pass

observation-tube in the

portionof

the

light from
with
in

trough of the instrument, suitable lamp through it.


his eye
at the
or

The

observer

small the

/ telescope

of the

instruments of the

Figs. 19, 20, 23, 27,

Laurent, Fric,and
the type of is not

corresponding part Peters polariscopeswill notice that


or

one-half
to

of the disk is shaded

more

ing deeply colored, accordthe

than polariscope,

other, provided the


vertical line
and

instrument

set at the neutral

point. The
be backwards

separating the
if not, the until The
moves a

half -disks should

should be moved

shaiply defined,
or

ocular

forwards

sharp focus is obtained.


observer the should
now

turn

the

milled
or

screw,

which

quartz-wedge compensator,
until read field appears the scale as directed the

the

Laurent,

analyzer of or uniformly shaded


optical
side

the

tinted, then
In

making the observation


of the

axis
to

instrument, and

the eye should not

in page 154. should be in the be moved

from

side. A little

practicewill
in the

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 shading it uniformly. giving greater facility The double compensating polariscopes are providedwith

164

OPTICAL

METHODS

IN

SUGAR

ANALYSIS.

two

scales,in the older instruments,


the other

one

graduated in black
scale is
one.

and

frequently in red.
screw

The

black

operated
For nary ordi-

by the black
work with

and

the

red

by the brass
zero

the red scale is set at


screw.

and

the field is

equalized

the black the

Since

abandonment

length changing with scales are usuallyused, and


for

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


are

marked

to

indicate

whether

right or left readings.


check the scale,remove the
agree.
screw

To

the observation-tube used for invert

and

ize equal-

the field with

readings. Both

readingsshould
To make
an

invert

left-hand
set
at
zero

sugar,

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

and with

the the

readingsshould
With
the

be recorded

sign minus. algebraic


the direct and the scale,

singleboth

compensating
are

instruments the
same

invert

readings

made

on

graduationsextending
fitted small with
a

sides of the The

zero.

Laurent

instruments

are a

device

for

the polarizerthrough rotating the sensitiveness. This

angle, thus
in
in

varying

is convenient A

polarizingvery
the

dark-colored the of
same

solutions.

slightchange
or

position of
the
amount

adjusting lever will increase

decrease

lightthat
time

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


passes

the

polariscope. Having equalizedthe


scale is to shown scale is best

field of the
be

polariscope as
The method Let of the

already
reading position

described, the
the

read.
an

by

example.

1 i 1 11 .1

Fio.

28.

of the

scale and

vernier

be

of the vernier lower number

is between and
note

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

shown

in

156

OPTICAL

METHODS

IN

SUGAR

ANALYSIS.

It is

quite essential
to

that

the

position of the
The if

respect

the be

polariscope be
as

fixed.

light with intensity of the changed, the


i

light should
zero

constant

as

possible,and
be verified.

reading observation
It is difficult under suitable monochromatic The

should the usual

factoryconditions
the

to

provide
type
of

light for
are

Laurent

instruments. the Landolt

lamps used
These

the

Laurent

gas-sodium,
last
such

gas-sodium, and
Bunsen with

the

Laurent

named
as

burning alcohol.
of
a

lamps
the

the eo'ipyle, requirea flame

that

burner, and
fused various

yellow color is imparted


chloride. M. F.
use

to it

by

contact

sodium

Dupont
in and

has

experimented with

soduim finds that

salts for sodium

lamps

for monochromatic tribasic

and light,

chloride

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
"

of the instrument To filled with


an

test water

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

in the This

trough of the instrument


observation
on

and

make

observation.

may the
zero

be

made
so

without

the made the

tube, but
as

the the

adjustment
water.

is not

readily

with

If the

scale is

properly adjusted
Haensch ments instru-

reading
is the

should of
same

be

zero.

The

method

adjusting the Schmidt


for all of their used

"

compensating
makers. is
A

polariscopes
micrometermove
as

and
screw,

is similar to that turned


a

by
of
a

other

by

means

key,

vernier but moved scale


now

short
water

distance. in the

The

arranged to field is equalized


the until the
one

the

usual,
is

with

observation-tube, and
zero

vernier

by the micrometer-screw
and
moved

lines of the The scale


screw

vernier

coincide

with

another.

is

and do

through several degrees by the milled the field is again equalized as before,and if the zero
not

lines These

coincide

the
are

vernier

is to

be

again adjusted.
zeros

manipulations
successive

repeated until the


These

coincide
are

in

eral sev-

observations.

adjustments

very

^Bulletia

Association de 1'

des

ChimiBtes, 14, 1041.

I
ADJUSTMENT OF
A

POLARI8COPE.

1^7

to fatiguing

the

eye,

which

should

be

rested

short time

making the final observations. Certain compensating polariscopes, of the older especially models, are exceedinglysensitive to changes in the position of the source of light. It is advisable to follow or intensity 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, of the and the intensity light should not be changed after adjustingthe instrument until the observation A change in the has been made. of the light, with certain instruments, position or intensity
before will sometimes In lever O
cause
an

error

of 0.5"

or

more.

adjusting the
focused

Laurent

to read polariscopes to

zero,

the

U, Figs.25, 26, is lifted


on

is next

the
zeros

the upper limit,the ocular vertical line which divides the


are now

field into halves; the


means

made
now

to

coincide
be

of the

screw

G.

The is in

field should

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
It is advisable to have the 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" and
a

second

about

60", as

these

parts of the scale


control-tube

are

used

in the most

important polarizations.
made funnel

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

The

by
T

Fig. 29.
a

The

of the

control-tube
as

is filled with it is

sugar

solution, which
The

flows into the tube


screw.

lengthened by turning the milled


tration illus-

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


The

tube

The

committee

of the

Fourth

International Congress of
the
use

Applied Chemistry

also recommends

of pure

cane-

168

OPTICAL

METHODa

IN

BUGAB

ANALYSIS.

Bugftr for

testing the polariacope.

The

method

of

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 when


set

the field of the


the

polariacope
from
man, work-

unevenly shaded
The

at

neutrel
not
an

pomt.
removed

analyzer
and
the

and
or

polarizer should

be

the

instrument
m

adjusted except
event
to

by
for

experienced
the

of the

an

accident

to

polariscope it
very

should
All

be

returned of the

dealer

repairs.
be

parts

polariscope should
parts
of the and

kept

dean be

especially the

exposed

lenses; these wiped with

should

cleanaed with alcohol occasionally

old linen

79.
are

Observation
in Fig. 30.

Tubes.~The
The upper

usual tube

tubes

of

glass
and

shown lower

has

screw-eaps is

the

the

Landolt

slip-cap. The
*"
j-"

slip-cap
undue the

designed
pressure

prevent

feM^^^
\J^

__^

(fm
'tmf

"Pon

cover-glass. The
Laurent
with

tubes

of the French
are

instrument

supplied
have

slip-caps that
catchea.
A

bayonetspring ia
cap

coiled the

^
FiQ. 30.

arranged
bear
upon

inside
the

to

cover-giaaa

and

hold

it in position, without
pressure.

unnecessary

Metal Account

observation-tubes
must

are

used

in many

laboratories.
in very fluctu-

be made

of the expansion

of the metal

careful work, especially if the

laboratory temperature

OBSERVATION

TUBES.

15Q

ates

greatly. Metal
handling and
sometimes

tubes
to

are

liable to distortion
with acids.

through
tubes

careless
are

corrosion
or are

These
to

of silver

plated with

gold

prevent

corrosion.
Tubes be of the tjrpe shown

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
cause

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


in the

striations

to

form

in the
In

liquid. These
of

prevent

an

immediate should

observation.

the event

be left in the Tube In

trough of the
with

the striations, until the polariscope ^This tube

tube field

clears. Observation in

Enlarged End.

"

is shown the

Fig. 31.

using this tube, it is nearly filled with

FiQ.

31.

solution to be

polarized,leaving
upper the

room

for

small

bubble This

of
rangement ar-

air, which

rises to obviates

part of the

enlargement.

necessity of excluding air-bubbles,


"

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

order

to

overcome as

the
secure

prevalent defects in the theoretical design, as well


a

tube

suitable

for

severe

usage,

this Bureau

(U. S. Bureau

wssssam

Fia.

32.

of

Standards) has brought


in

out

the

new

Bates that

type of tube
the

shown carried

Fig.

32.

It will be

observed
are

weight is

upon

two

shoulders, which
No.

integral parts of the


U. S. Bureau of Stand'

Copied
p.

from

Circular

44,

"

Polarimetry,"

ardsr

39.

160

OPTICAL

METHODS

IN

SUGAR

ANALYSIS.

tube from

and

not

upon

the caps,

all danger thereby eliminating

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

field of the instrument

thus

appears
no

for the first time

as

bright, sharply defined


the
are

circle with

overlying haziness,
accuracy.

and ends

reading can be made with increased enlarged with all the attendant

Both

advantages, yet

Fig.

33.

but walls

one

size of
are

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

bending."
Observation Tube with Side in Tvbvle.
"

The

tube

shown

in

Fig.

33

is very

convenient

general sugar-analysis. The


This
of the

cover-glasses need
reduces

rarely be removed. the risk of error by compression

arrangement

cover-glasses.

Fia.

34.

The acid.

tubes

should

be

frequently cleaned
Tube, This

with

diluted

acetic

Pellet's Continuous for very


use

"

rapid polarizationand
for beet-seed
a

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


selection and the

of laboratories
raw

purchase
Pellet

of

material

on

basis

of its sucrose control

content.

The

tube

is also convenient

in the

of the

char-filters in

sugar-refineries.
The without Pellet tube

provides
it from

for the

removing

the

rapid change of solutions trough of the polariscopa.

OBSERVATION

TUBES.

161

The

tube

is

so

arranged that it
to
a

may

form

part of
The

syphon

by
of into then

connecting rubber, tubing the syphon terminates in


the
new

the

tubules.

solution The

and

glass tube pinch-cock on


should be

leg which is dipped the long leg is previous

short

opened.
This of

incoming

hquid displaces the


used

solution.'

arrangement
is

approximately the
accuracy

same

tions only with solupolarization and not when The funnel when

scientific illustrated and be used The before


water.

desired.

arrangement
is
sary, neces-

in

Fig.
use

35 should Uberal

be used

accuracy

in its

quantities of the solution


be and washed with be

should

to wash

the funnel. tube should distilled water left filled with into the

Pellet
a

period of idleness

should

The hands

first of the
were

descriptions of this tube


author
were
a

that
and

came

very

meager,

several
was

ments experi-

made

before
were

tube satisfactory made


as use.

constructed.
to

These the
secure

experiments
tube

not

with

view

improving

construction
a

of the

tube

for immediate
is shown

designed by Pellet, but to The tube finallyadopted

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

instead
annular each

of

one.

The
which grooves

funnel
connects

directs

the

solution

into

an

canal,

by
at

separate
end

openings wilh
The
cover-

of the four

shown

the inner

of the tube. of the

solution

is delivered

against the

surface

FiG.

36.

and by glass, end tube the

similar set of grooves the

and

canal at the flows


cannot

opposite
a

of the tube
to the

displaced
is

solution

through
be made So

bent until

waste-jar. The observation

|)revioussolution

entirelydisplaced.
the field will not

long

as

any

of the old solution remains

be clear.

162

OPTICAL

METHODS

IN

SUGAR

ANALYSIS.

The
accuracy

Pellet

tube

with

the

funnel-inlet
sugars.

may

be

used should

with be

in the and

analysis of

The

funnel

small

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 swirling motion for the plain tube. would imparted to the solution by the rifling probably promote the removal of the previous solution, especially in

testing sugars.

Experiments made

with

Pellet

tube, pro-

FiG.

38.

FiQ.

37.

vided
grooves.

with

glassbody, indicated
Irwersion

the

of desirability

the

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
"

method. double-polarization enclosed in


a

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 ^adumetal

ated

to

fifths of devised

Wiley

degree should be used. the desiccator-caps shown

in

Fig.

37

to

164

OPTICAL

METHODS

IN

SUGAR

ANALYSIS.

be

given only approximately on


materials themselves and

account in the

of the

variations of the

in the

illumination

polariscope. In general the minimum quantity of the leadsalt that will yield a clear and sufficiently tion solulight-colored
should
errors

be

used. into

Excessive the

use

of lead

introduces

portant im-

analysis. The
of the lead

following numbers
of 54.3? Brix
to

refer to cubic
per
one

centimeters

solution Raw

normal

weight of the material:


to 10 cc; cc;
raw

juice, 1.5

.2.5 cc;

sirup,7 5 to 10 control),
96" 89" 80
to

molasses

of 20" Brix

first molasses,7 to 10 cc;


sugar, 2 to 4 cc; 6 to

(vacuum-pan final molasses,


sugar, 1 to 2

25 to 30 cc;
cc; 6
cc

98"
cc;

raw

second

sugar,

filter

press-cake, replace the


179.)
per

Home's solution

dry subacetate
of the
1.25

of lead may

very

often
page

salt with
to

advantagp. (See
of the

proximatel Ap-

100
.

cc.

of

raw

1.5 grams juiceand a like

salt is

required

proportion for other


of the

materials.

Paragraphs 83, 84, relative


and the volume

to the influence of the lead-salt

the sugars consulted.


upon

should precipitates

be

Alumina-cream of lead in

should

be

used

in addition

to

the

tate subace-

clarifyingthe solution in testing a sugar. The alumina-cream alone is usually sufficient in the analysis of high-grade sugars. usually advisable to add a little of the lead reagent to the sugar solution,mix thoroughly, await the subsidence of the precipitate and 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
whether the lead has been used precipitate in sufficient quantity. The in reagent should be measured
appearance

It is

of the

routine should The

work

and

in

so

far with

as

is

possiblethe
are

same

quantity

always
a

be used in
or

similar materials.

materials

sugar

analysis

weighed in

nickel

German-silver

conveniently capsule,made especially


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

material

may

be

very

readily washed
for this

into
use.

the fiask. The

The

capsules lose weight graduallythrough


not

should counterpoise

be filed to correct

loss,

SPECIAL

SUGAB

APPARATUS.

165

but

the stem

or

plug should be unscrewed


the

ajod sufficietitlead

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 inserting the ste.ii
from

be removed

of into the

small the neck

German-Silver of the flask.

funnel, made
This should from the
a

for reach

the
to

purpose,

just below
with the funnel

neck, thus
The

latter. should
room

keeping the sugar solution adhering to


into the flask with left in the flask
"

contact

capsule and
water.
cc.
"

be washed
must

jetof

Sufficient
to

be

about for

20

permit

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. giving
the be examined from below
to note

dissolvingthe material.

whether

undissolved

material

Fio.

38.

remains. with should lead be

After

solution of the material


as

and

its clarification volume Should be in

subacetate

has the

been mark

described, the
with
water.

completed
adhere with the

to

drops of
absorbed

water

to the neck

of the

flas"they should
water

strips of filter-paper.The
solutions should be either

used
or

preparing
water

distilled

other

free of

opticallyactive substances.
of the flask should be be be

The

contents

thoroughly mixed
upon

by
The

shaking and
filter should should be be

poured immediately
for
or

the

filter.

suitable of paper fluted or '^star'^ folded The funnel and


paper

and rapid filtrations, ribbed be funnel should

used.

should

large enough,
as

especiallyin analyzing
of the flask. The above centimeters the

sugars,

to receive
never

the entire contents


so

filter should

be

large
in

to project

edges of the
should

funnel. be be

The used

first few

cubic

of the

filtrate should then

and filtering-cylinder

rinsing the rejected. If the

166

OPTICAL

METHODS

IN

SUQAB

ANALYSIS.

filtrate should
the

not

be bright and is not


in

clear
to

it may be

be

returned

to

but filter,

this

usually

recommended.
and

It

is Eilnays

preferable
considerable
runs a

analyzing
accuracy

sugars
to

other

materials
the

requiring
is best

reject portioca of
filtrate does
not

filtrate until it
to prepare

clear.
new

If the

cle"r, it
of
tempted at-

solution, changing

the

quantity
be

subacetate

of

lead. with

The

polarization should

never

except
It may the

perfectly clear solutions.


be difScult to obtain
cane.

sometimes

clear solutions
The

with of
a

juice and

products of unsound
salt
or

addition

littie common tion will often

sodium

phosphate
both the

followed salt and

by refiltrakieselguhr

remedy

this,or

may

be

used.

Occasionally the difficulty may


If
so,
a

be

due

to sub-

insufficient
acetate

subacetate.
be

little of

Home's

dry

should

added.
"

F'OieTing Devicet.
illustrated in

convenient
A and
many

filteringarrangement funnel,
to

ia

Fig.

39.

is

stemless
a

quarterA

pint

precipiUting-jar, by
4

small

cyUnder.
the

plain

cylinder is preferred
as

chemists

Up-cylinder,
of

the funnel Steniless

makes

closer joint with inches


in

the edge. made

funnels,
of thin

diameter,
are
more

good

tin-^late or
The

copper,

planished, glass.
stemless

convenient,
and with

except for invert solutions,than

advantage

of

the

metal

funnels
ease

heavy
which

glass precipitating-jars or

cylinders

is the

SPECIAL

SUGAR

APPARATUS.

167

they
very

may

be

washed

and

dried.

The

jar and

cylinderare

convenient
"

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

units
grams

should and

be

used

with
or

the
true

old
cc.

normal
C.

weight of 26.048

the metric

at 20"

R
110
"0

Fig.

40.

with

the

normal

weight of
be made

26

grams,

that

adopted by

the

International
Flasks

Commission

for Uniform from

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
should internal diameter
or

than

those

used

in This

the

U.

S.

Customs and The limits

laboratories
the diameters

in research

work.

below specified

should

is unnecessary be adhered t9. and

following maximum
of tolerance the U. of
error

internal diameters
in the

of the neck
are

capacity of flasks

specified by

S. Bureau

of Standards:

168

OPTICAL

METHODS

IN

SUGAR

ANALYSIS.

Tbis such

limit

of tolerance diameter.

is

apparently large for


Of several hundred

flasks

of

small of
a

neck

prominent dealer
writer
were

flasks chased purfor the laboratories under the certificate limits

direction of

of the

and

bearing the maker's


the tolerance

all calibration,

well within

given

in the table. The House of 130

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
cc.

flasks

diameter
12.6 30
mm.

must

be not

less than

11.6

mm.

and

not not

more

than than

mm.

The from

graduation marks
end and 16

shall be
mm.

less

the upper

fyom the lower end


in

of the neck. The flasks shown in

Fig. 40 all conform


with

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


with their of
100

jnarked the

system

capacity and graduation, e.g.,


C* 17.6/17.5" "Contains
or

"Contains for the Mohr


100 true cc,

cc,

flask and

20** C."

for the metric flasks. should the neck


of

cubic-centimeter

The
pletely com-

graduation-mark
encircle flask. Pellet's conical
are

the

of

rubber bottom
Fig.
41.

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

to reduce

breakage. Their form and gives them great stability


^

facilitates the escape

of air-bubbles.

SIECIAL

SUGAR

APPARATUS.

169

Referringto Fig. 40, the


fill most The in the
of

flasks A

and

B the

of various capacities
oratory. sugar-house labare

the

requirements of
Kohlrausch

Stift (C) and

(D) flasks

used
at

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

carbonate commercial

that

deposits upon
acid is

the walls of the flask.

muriatic

usually

used

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
use

Strong cleaning in nitric acid, followed

the chromic

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.
system
to

work There between

without is much the true

having first verified its marked


confusion and.Mohr's marked
as
on

the
cc,

part of

facturers manuone

flasks of the

being sometimes
the flask
an as oven.

having been
above
note

graduated
and oughly thor-

the other. Cleanse has been On


upon

described

dry it in
moisture
return

cooling the flask


the inside

whether if
so

has

condensed
oven.

walls

and

the flask to the

The
errors

weighing should
of the balance in the balance

be

by
Cool but

substitution the do
not

to to

eliminate
room

itself.
case,

flask

perature tem-

wipe it again, and


the leftbe used and

then hand in

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

counterpoising. Remove counterpoise the weight on


for the the flask to the limits of

the balance with

right-hand pan
This

accurate

weights substituted

Fill the flask to the mark

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

flask.

""

Hai^book

of Sugar

Analysis,"

p.

171.

170

OPTICAL

METHODS

IN

SDOAB

ANALTBIB.

of

room

temperature.
the the
water

large pipette should


bo

be
as

used

in

running
wetting
neck of

into the flaak to avoid


Remove
a

far

is possible
to

neck.

water

that

may

adhere

the
ing fillneck

the flask,with flask by

roll of filter-paper. it by level the of


upper

Verify
If

the

of the with part the


of

holding
at

part
eye.

of the

graduation
the
curve

the

the is not

the

lower the small

of

the
or

meniscu?
remove

in
means

hne

with of
a

graduation-mark, pipette and


Place the

odd

water

by

bring it into line.


filled flask
upon

the
of

balance-pan
or

as

before

and

count"rpoiBe it with
the

pieces
the

metal

weights.
the
water

Remove with
an

fla^

and

note

temperature

of

Fis.

42.

accurate

thennometer.
and

Counterpoise the
record the this

metal
that

with
of the

the flask

analytical weights
and
water. correct

weight
of

as

Deducting
of the
not.
water

weight
whether

the

flask

gives the

weight
or

the

balance

ie in prop"

adjustment
Reference

is

now

had
of 100

to

the

tables,

pages to

452

and
or

453,
the

showing
true
cc.

the

weight
at

cc.

(according
temperatures.
of
water

Mobr For

to

table)

various
grams this

example:
C.

Our
ence

flask contains
to

99.958

at

20"

Refei^
of

the

table
cc.

shows

to

be

the

apparent

weight
weight
at to

100
to

Mohr's

at 20"

C, hence
of

the flask is correctly graduated


same

this system.
and

Similarly using the


table
at

flask and
true
cc.

of C.

water

the

corrections

for

20"

The

correction

20"

C.

i3+0.282, which

added

99.95S

172

OPTICAL

METHODS

IN

S^QAB

ANALYSIS.

shown

in F^.
a

43
very

is suitable. convenient
e.g.

The type
the

decimal
for very

balance, shown weight


pan the in half

in

Fig. 43, b
o( In

rapid weighings
of
at
a

the the

same

quantity,

normal

sugar. back
pan.

balance

illustrated,10 'weights,
set

grams 1

in the gram

the

of the
'

instrument of sugar One

counterpoiee
normal of these

other

Two be

sets

and

normal, should
be
the

provided.
for balances
a

weights
the

should

kept

in

reserve

verifying and
should
at

checking
least be

weight of
to
two

others.

The

sensitive

milligrams
materials

with

full load in the pans,

though weights

of sugar

for polarization,to within


accurate.
or

milligrams

are

usually sufficiently through


are

The

errors

that

may

be introduced

ation evapor-

absorption

of moisture
to

in alow
2

weighing

of

more

importance than weights


The venient
bulhon for and

within

milligrams.
in Fig. 44 in is very which
eon-

type
the

of balance

shown

so-called
of

rough

weighings
are

large
This

capacity
balance it from

speed
be and

manipulation
in
a

essentials. hood
to

should dust

placed
That

glass-framed
This

protect
in
100

currents

of air.
of size.
5

instrument

is made
to

several

capacities.
is
a

kilograms,
It should

sensitive

milligrams,

suitable

have

agate bearings

HEATING

DEVICES.

173

and
use

knife in

edges for tropicalwork.


in and molasses.
"

This scale is suitable for

bagasse analysis and

determining the degree Brix


The
water

of massecuites Washr-hoUles, solution bottles should for


on
a

Stock-bottles.

and be The

the

lead

use

in sugar shelf above

analysis,should
the work-table.

kept in large
water-bottle

have

glass syphon-tube with

rubber

connections, a

pinch-cock and

glass-nozzle, forming a convenient ment arrangeand for diluting for washing samples into the sugar-flask the solutions to the graduations on the necks of the flasks. This is a very satisfactory form of wash-bottle, and several about the laboratory. The of these should be distributed
lead subacetate bottle

should

be connected

with

reservoir-

FiG. 45.
,

burette.

The

burette

has

three-way cock,
by
means

one

opening

connecting with the stock-bottle


and
a

of

glasssyphon

rubber

tube. be

The

air-inlet to the

subacetate-of-lead

bottle

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

should

of the lead. precipitation since


very
a

This

small

is not precipitation
are

large stock-bottles should he employed.


Where of lead -subacetate stock-bottle

used

strictly necessary, but where objectionable, the washing arrangement


in

is not

solution

is used

storing samples
solution

containing the concentrated should also be provided.

juice a

Heating

hot-plate is the heating device for laboratories having


Devices.
"

The

electric

most
a

venient con-

24-hours

174

OPTICAL

METHODS

IN

SUGAR

ANALYSIS.

electric service. Where

the generatorsare

only operatedat

be supplemented by stoves. must night the hot-plates 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 since glass is double-refracting cover-glasses, 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, clean and with parallel perfectly 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.

Glasses

and

observation-tubes

should

be

frequentlywashed
The

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 and making an observation; on revolving of the polariscope 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. should be used in a well-ventilated room. The polariscope 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. the instrument the open end, and lights box, opposite 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

VOLUME

OP

THE

LEAD

PBECIPITATB.

175

be the be

painted black.
bottom

The
or

should polariseope

be

fastened to
not

of the box

table,so
scale

that

it may

readily

jarred out of position.


The illumination the of the is effected

by

reflecting

light from
models in the

polariscopelamp
of reflectors.

of instruments. absence

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


upon

The

current

may

be

iently conven-

by
used

and should be supplied by dry-batteries bell push-button. A gas-jetor candle should for this

controlled
never

be
or

lightingon

account

of

overheating the scale


should be

damaging the polariscope.


The
zero

settingof

the

scale polariscope

quently fre-

verified,using standardized
bichromate filter-cell(see page and in

quartz
must

145)

plates. The always be used in


In fact this the

this verification

adjusting the vernier.


be removed from
account

should never ray-filter or on except for refilling


to be

polariscope

of the dark

color of the solution

tested. of the Volume of the


Lead

83.
"

Influence
^The lead

tate. Precipi-

introduces errors into the polariprecipitate of which are probably offset by compensome soopicanalysis, sating of low-grade products. notably in the analysis errors, will The error due to the volume occupied by the precipitate be considered in this paragraph, and those due to influence of the lead
upon

the

sugars

and
on.

other

active optically

bodies

will be

discussed

farther if
a

It is evident

that

part of the volume


there be
no

of the flask be
for the

occupied by
volume
so

solid, and

compensation

occupied, the
matter

high.
but
more

This

polariscopicreading will be too has been studied by numerous chemists,


connection with the

in especially

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
sucrose

at the by the precipitate

moment

of its formation. that


.

From is
no

numerous

experiAientsSachs*
sucrose,

concluded
the
'"'""" da

there

absorption of
"

and

attributed
"

results with

Revue

Universelle

de la Fabrication

Sucre, 1. 451.

176
low
and

OPTICAL

METHODS

IN

SUGAR

ANALYSIS.

products
sodium

to

the

influence with the

of the acetic the

acetates

of

potassium
position decomof the

formed lead view

acid

from

the
power

of the
sucrose.

salt, upon
in the
to

rotatory

This

is strengthened

by the fact that there is a


both beet and

very

perceptible error,
due juices,

of polarization

sugar-cane

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


with
low
*

the

formed, whereas

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.
He dissolved
x

grams

of molasses

in water,

added

sufficient of the
x

af the

lead salt for clarification, completed the volume


to

solution

100

increases frpm Since the. the


same

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


cc,

and

quantity of
volume An

molasses

is increased

with

each

ment experiin the

of the increase

precipitate must
in the volume

increase of the

ratio.

precipitate,

if this

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

nere.the
of the

volume

solution is decreased.
.

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

reading,the
if there is
an

ratio
"

should due
to

increase the volume

with

the

concentration,
I

error,

of the Sachs

not precipitate,

compensated
of beet-molasses

by

other

influences.
5 to and
y

used

quantities
cc,

ranging from
values
of
x

35

grams

in 100

and

substitutingthe
he

in the

ratio and

reducing

obtained

the

followingfigures:
1.906
2.14 1.900 2.13 1.900 2.14 1.906 2.14

1st Series

1.896

2d
The
errors

*'

value constant practically have fully compensated

of the ratio shows

that minus the volume

for that

due

to

of thb
In
a

precipitate. similar experiment with


:

beet-juicesSachs

obtained

the
1st

following numbers Series.


''

0.5446
0.5800
!
""

0.5474

0.5480 0.5842
"

0.5497 0.5860
,1

2d
.

0.5836
' I

...I.

.(i

"

"^ Revue

UniverBelle

de la Fabrication

du Sucre, 1, 451.

VOLUME

OF

THE

LEAD

PREOIPITATB.

177

The
an

increase due
to

in the tha

ratio with volume

juices shows
to correct

that

there there

is is

error

of the
error

precipitate and
it. Cuba with

not

sufficient

compensating by the
to

Experiments
gave

author

in

cane-molasses series of R.

results

similar

those of

of Sachs, and

several

unpublished analyses
at

cane-juices made
gave

by

L.

Cook,

the
and

writer's
lead

instance,
25 gr. :1

the

following results:
ck.

Juice

cc.

50 gr. :2

75

gr. :3

cc.

100

gr. :4 cc.

1st Series

0.628
0.628

0.628 0.630 1. in 100

0.632
0.633

0.633 0.634

2d Series the that

"

No.

is

duplicate of No. weight


normal times
the

The
cc.

polarization of
was

juice using the normal using lour


uncompensated
error

16.36, and
100
cc.

weight in
4
was

and

dividing the
an

polariseope reading by
error

16.49, shomng
of
sucrose.
same

of 0.13 2d

per

cent

The

uncompensated
was

in the

Series, ttsingthe

juice,

0.15*^
In
two

of which after
Juice

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

series of

forty hours,
and

results
40
gr. :2

were

as

follows:
80
gr. :4

lead. .20 gr. :1

cc.

cc.

CO gr. :3

cc.

cc.lOO

gr.

:5 cc"

1st

Series.....
"

0.690

0.691 0.690

0.690(?)
0.692

0.694

0.696

2d As

0.687
case

0.693

0.694

in the

of Sachs's that there

experiments with beets, this work


is
to
a

of Cook

shows

very

perceptible error
of the of

in the

analysis of cane-juices due


Sachs
^

the

volume

precipitate.
the

used

the

following method
usual, using
hot the

determining
of

ume volsub. of
a

of the
acetate

precipitate: Clarify 100


as a

cc.

juice with

of lead Wash and

tall

cylinder instead
all of
a

flask.
water

the

precipitate by decantation, first with


water, until
the

cold

finally with
Transfer the dilute
a

sucrose

is removed. add one-half and

precipitateto weight of
to

ICO-cc.

flask and
the

normal
the

cane-sugar, 100
cc,

dissolve

sugar,

solution

and mix, filter,

using polarize,
calculated
t^'mim^^^^'^^
'"'""'"'

400-mm.

observation-tube.

The

results

are

as

follows:
" " " . "

.^----1

"""""".

'

Revue

Universelle

de

la Fabrication

du

Sucre,

1, 451.

178

OPTICAL

METHODS

IN

BUGAB

ANALYSIS.

Let

P""per
P^"the

cent

of

sucrose

in the

sugar;
up

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

in the

Then

,-i50^ziOOP
99.9;
100.77.

Example:

Let

P="

P'"

Vh^r. Then

^^(100X100.77)-(100X99.
^^^j;^
the method

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

The for the termed of the

followingis
error

of Scheibler of the

ior

correcting
To 100
cc.

due to the volume

predpitate^and usually
method":

"Scheibler's double-dilution

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

polarize as
as

usual;

to

second

portion of 100
to 220

cC:

of and

juiceadd lead polarize.


Calculation subtract remainder the
:

before, complete the volume


second the

cc,

Multiplythe
2.2

product from
and remainder
per
cent

reading by 2, polariscope first reading,multiply the product from the first required reading for the

by

deduct

this

reading. The
calculation

is the
sucrose:

of the

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

18 .0 67.6
28.7

(220 cc.)....

2X28.7"57.4;
"57.16=corrected
page 300
we

67.6-67.4-0.2;
have:

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

15.18 .03 .02


15.23
^
=

required per

cent.
25, 1054.

Zeit. RUbenzucker-Industrie,

80

OPTICAL

METHODS

IN

SUGAR

ANALYSIS.

caused
excess

by excessive
of 0,5
cc. causes

amounts
a a

of subacetate of

of lead.
cc.

An

diminution

1 0.1**;
on

of

0.12**;

cc.

of 0.11" and 3 The


of
cc.

cc.

diminution of 0.90"
a

scale.
excess

rotation
co. excess

reaches

minimum
returns
to

the cane-sugar value when an

is present and and continues added. A

the initial value


the amount
was

with 6

in

to increase with

of lead solution

sugar

99.9" polarizing

used

in these

experiments.
^

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

decrease, but
causes

when
an

the salt reaches increase whieh

maximum

further that
of

addition

finallyexceeds

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

an

increase

action

of the salts is lessened.

is almost
a

i.e.,the specific rotatory power, The specific rotatory power unaffected by varying the quantity of sugar with
relation between the salt and
water.

in

the

constant

The
a

chlorides
ner. man-

of

lithium, sodium, and


'^

potassium behave

in

similar

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.
same

An

examination

of the action of the

in the

same

manner,

but the clilorides of the The

alkalis show

similar relation.
within each
to different group

relation, however,
not

only holds
salts

good

of chlorides and

for two

belonging
in

groups."
power

The

rotatory

of

sucrose

in

water

or

alcohol

solution is not and


to
as

modified
when

by

the presence

of nitrates of sodium

potassiumeven
much
as

the

iSO per cent

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


of the lead

In his

of the influence investigation


deut.
chem.

precipitate,

[_

Berichte

Gesell.

23, 3570; Journ.

Chem.

Soc, 60, 283.

1
INFLUENCE OF SUB ACETATE OF LEAD.

181

that the presence of acetate of potassium very diminished the rotation. The diminution was perceptibly Sachs also noticeable
was

found

with

the

of potassium sulphates the

and

but lead,

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

marked

with

to

that

of the

acetates.

The in part.

presence

of free acetic acid further


states

reduces the
use

this influence of tannic


on

Sachs

that

acid in

solutions decolorizing of the

is very

tionable objec-

account

of the volume

formed precipitate

with

the

lead.
"

Dextrose.
or,

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

lead, under See also Invert-sugar.


neutral of I.evulose.
"

the

conditions analytical is very of lead. of the

The

rotatory power
presence

of levulose

greatly
Acetic levulose is

diminished
acid added

by
to

the

of subacetate the rotation

acidity restores
a

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

partly

precipitated
as

lead salt in the presence

of certain

chlorides,

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

in the

same

solution with

constituents

of which

basic acetate

of lead forms

insoluble combinations
Levulose. In

(Prinsenof of

GJeerligs).
Invert-sugar Dextrose^ and
J
"

the the

presence

the

salts formed

in the

decompositionof

subacetate

lead, dextrose, and levulose are The influence of the basic lead salt Edson).
or power little lead of of undue activity optical gives

in part precipitated
on

(Pellet,

the rotatory of levu'osate


to the

of levulose (seeLevulose)

the formation

prominence
a

dextrose, which
amounts Increasing

is not

affected

and

results in added

plus error.
to

of subacetate

of lead

invert-

the left solutions decrease sugar rotation is to the righton account

rotation,and
of that
error

the finally dextrose. Journal of

of the in the

C. the

H.

Gill called

attention

to

this

Chemical

Society,April, 1871, and


Universdle dc la Fabrication

in the

early editions

Revue

du

Sucre. 1, 151.

182

OPTICAL

METHODS

IN

SUGAR

ANALYSIS.

of this book, the


restore

author
power

advised of th"
the

the

use

of a"etic

acid

to

the

rotatory

levulose.

Acetic sugar;
acetate

acid

slightlylowers
acid sodic chloride

rotatory
an

power

of invertSodic

hydrochloric
and and Wm. the

has

opposite
the

effect.

increase

rotation

(H. A.
The

Weber acids

McPhersons).
the

Sulphuric and hydrochloric


no

increase

rotation; oxalic acid has


as

effect.

rotation increased.

increases If with

warming
the about

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

rotation

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


to corresponding

requires

Malic acid is

acid.

"

^This acid is Isevorotatory. The Malic acid is

artificial malic

opticallyinactive.
of lead. and and

precipitated by
are

subacetate Pectine

Pjrapectine.
"

^These

substances

rotatory dextroof

are

both

precipitated by subacetate
acetate

leadt

and

the

second
"

by normal
Not

of lead. subacetate of

Asparagine.
is rendered lead salt.

precipitable by
solution and

dextrorotatory instead
In water

lead, but Isevorotatory by the


of

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

alkaline solution

In

neutral

and of

alkaline
a

solution

asparagine

Isevorotatory; in
in the
presence

presence

mineral

tory; acid, dextrorotais diminished

of acetic acid the of the acid

rotation becomes

and

with

10

molecules is

0", and
immature

with

additional

acid

dextrorotatory (Degener). Asparagine


from cane;
as

is present in it is
a

that cane-jiiice, especially


to

changed

aspartic acid by the action of lime, and


in

lime

salt is found
"

molasses.*

Aspartic Acid.
the
are

lime

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.
Chimistes
of de

" 2

Bulletin

Aaaoc

France, 3, 131. Substances,


Landolt
"

Optical Rotation
Champion
W.

Organic

Dr. Long's "ng.

ed., 541.
"

and

Pellet, Compt.
Bui.

Rend.^ 83, 819.


p.

"

Maxwell,

38, 2d

Series, La. Expt. Station,

1380.

BONE-BLACK

ERROR.

183

85.

exercises

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


"

or

anknal
For

qharcoal
reason

this

it is desirable to

avoid

using it

possible. It is advised quantitiesranging from


black
to

the

half-normal advise
a

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

in

solution;
solution

others

the

of the and

sugar

the through quantity and then the filtration of sufficient rejectionof the filtrate, for the observation.

small

bone-black

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 and let this liquid filter just completely moisten the latter,
recent

In

off.
which

After
are

four

or

five similar
the the

the filtratesfrom filtrations,


a

test rejected, note

filtrates by

tion observapolariscopic

and be
soon

whether

protected from
as

reading varies. Solutions must evaporation during the filtration. So


no

the

reading is constant, showing


it
as

further This

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 .method filtrate. The
use

record

the

number.

of the

filament nitrogenfilled concent|*ated


one

in polarizingwill usually enable electric-lamp dispensewith animal charcoal.


86.
"

Mazda

to

Influence

of Temperature of

upop

Polarizations*

The

compensating type
at

polariscopecan
at

only give correct


was

readings
The
was

the

temperature

which

it for

standardized., instruments

former 17.5" C 1898

standard
and

temperature

these

usually all the instruments


to this standard.

made 1897

pijor to
the International

about

conformed

In
oi

Commission

for Uniform
as

Methods

Sugar Analysis
100 true
cc.

adopted
20" C.
as

26

grams

the normal

weight

and

at

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

the

and

that of

sucrose

decreases.

Dr.

H.

W.

184

OPTICAL

METHODS

IN

SUGAR

ANALYSIS.

Wiley called the


to

attention

of the IT. S. Treasury


into
a

Department
The ury Treas-

the

errors

introduced

sugar

polarizationsby these
in raw-sugar

conditions

and

prepared

table of corrections.

applies a temperature correction based upon Wiley's observations.


Charles A. Browne
*

testing

made

very

full study of the influence

of temperature

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

in the

arrangement
Brown in which
P*"

obviates

all

questionof

corrections.
=

states

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

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

observation, may polarizing cane-sugar


Neither of lower

Wiley'stable
are

may

also be used.
sugars

table, nor

formula
any

applicable to
factories conditions.

Few, if
under

sugar

are

polarization. equipped for polarizations

standard

to

Obviously certain precautions can, and should, be observed reduce errors: The laboratory and polariscoperoom should
well ventilated should
not

be

and

of the

same

temperature.
a

The wall
or

ariscope polthe

be in the

vicinityof
should

heated be

solutions laboratory-ovens. The polarized at room temperature.


8

prepared and Composite samples of


technical of low

gar,

used

in

part
be

as

basis

of the
a

reports
of the

(run
noon. after-

reports), should

polarized at
rather

time

temperature

iiii tropicallaboratories

than

in the heat

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

temperature

correction

is

"

Dr.

C.

A.

Browne

notes

twelve

errors

that

may

Handbook Dr. C. A.

of Sugar

Analysis,
N. Y. Orleans and

pp.

255-262. Trade of

Browne,
New
comments

Sugar

Lab., read
the in Am. this
up

paper

with

this

title before

the The

Section

Chem.

Soc., Nov.
are

20, 1914.

conclusions

paragraph
of the residual

stracted aberror.

from

this paper,

including the summing

ACCURACY

IN

SACCHARIMBTRIC

ANALYSIS.

185

enter

into

sugar

analysis. While
to
a

these refer specifically to considerable


exto^it in all

sugar-testingthey apply also


other

analyses:
of moisture of moisture in normal

1. Loss 2. 3. Loss

during mixing.
during weighing.

weights. 4. Volume in clarification. of precipitate of levulose. 5. Precipitation


Error
6.

Error

in capacity of flasks.

7.
8. 9.

Imperfect mixing of contents of flask* Evaporation during filtering. Error in length of polariscopetubes.
of bichromate cell. Variations Defects
errors

10. Omission
11. 12.

in temperature.

in scales of saccharimeters.

The

3, 6,
with
Since

and

12

are

iii

general mutually
do be
not appear may

pensating com-

and the
vary
errors

careful flasks each the

management
tubes side of the

in that

results. but

and

selected

slightlyon
in

disappear
may

averages

numbers, the The of duplicate tests.


correct

weights
the
near

balance. the

of easilybe kept within the limits of accuracy be checked The scales of the jK)lariscope may
accurate

important points with


corrections of the be made. be scale may

standard

quartz
in fact " that These

plates and
all parts

Other checked Dr.

points and
with the

Schmidt

Haensch
the
are

control-tube,Fig. 29.
errors

Browne

estimates

following plus
numbered
due
to: as

may

enter

in careless work.

in the

previous list:
Sugar Degrees.

Error

Mixing on paper 2. Evaporation during weighing in clarification. of precipitate 4. Volume of levulose 5. Precipitation of the 7. Imperfect mixing of the contents
1.
. .

+0

05
.

-f0.02 +0
18
.

-|-0.03

flask 8.
10.

+0.05 -|-0.04 -f-0.07 +0.04 +0.48

Evaporation during filtering


Omission of the bichromate cell

11.

Temperature variation from the standard


Total
error

186

OPTICAL

METHODS

IN

SUGAB

ANALYSIS.

The and in the

last

four four

6iT0ts

amounting
be
not

to

0.20** The

are

preventable
residual
error

first work

may

reduced. exceed

final
as

careful

should

+0.12

follows:

Error

due

tor
.

Sugar

Degrees.

1. 2. 4.

Evaporation Evaporation
'Volume
of

in in

mixing weighing

+0.010 +0.005 +0.090 +0.015

precipitate
levulose

6.

Precipitatioikof

Total

error

+0.120

There considered introduced


upon
or

are

other in the

sources

of
pages upon

error

that of this

have

already
such
as

been those

previous
pressure

work,

by
the the

the

cover-glasses, quarta-plates,
temperature
from

pressure tion prepara-

wiping
solution

of the
at
a

standardized different
errors

of the

that

of

observation,
The
use

etc.

Such
cream

are

entirely avoidable.
normal
acetate of

of

alumina

or

the the

lead

in

the

clarification will

instead

of

basic

acetate,
the

when

the
error.

material Home's of

permit,

practically
removes,

eliminates
or

levulose
so,

dry-lead

method It

nearly
that both

the these
of

volume
errors

precipitate
be

error.

is

possible
use

would

reduced

by

the

of color of

dried will the

acetate

lead

in

clarifying, where
The which
to
"

conditions
error

of is
one

admit.
most

temperature
the 0.5**

important
may

with

tropical
in is
extreme
an

chemist
cases.

must

deal.
a

This
constant to
a

amount

Since addition
error

temperature

laboratory

improbable
this

sugar-house,

the

only
tests
or

defense

against

lies the

in

making

important

early in the
the
use

morning

during

low-temperature
corrections.

period,

in

of arbitrary

temperature

188

CHEMICAL

METHODS

IN

SUGAR

ANALYSIS.

After
a

completing

the it

inversion and then and

transfer almost

ths

solution it

to

liter-flask, dilute
caustic
cc.

neutralize
the

with
to

dilute
1000 The be

soda

solution

complete
"
.

volume

solution

contains

dextrose

and

levulose of
j

and

should Wein
:

analyzed
25

by
cc.

the
of

foUowi^jg method
solution 397,

Meissl
of

and

Measure* Soxhlet's
add the
50

(A)
page

and

25

cc,
a

solution

(B),
beaker,

solution,
cc.

416,
and

into boil

250-cc.

of the
flame the

sugar

solution

two

minutes,

using

najted
Collect

of the

lamp.
oxide in and determine
page 235.

cuprous

the

copper

in

it

by

one

of of

the the

methods

118,

Ascertain

the
of

weight
copper

invert-sugar

from
on

the

number

of milligrams

reduced, weight
in

using the table


0.95
to

pages

189, 190, and


terms

OHiltiply
weight
of

this
sucrose

by
the

reduce of since of the

it to

of
used.

the

quantity

material

This

plication multion

is

necessary

sucrose

yields

invert-sugar,

inversion,
If the
to

in

the

ratio

100:95.

material
sucrose,

contains

glucose
the

(reducing-sugar)
before

in

tion addi-

determine
inversion Calculate

reduction
the

inversion described
sucrose as

by
for

118,

and

after

by
the

method

just
of

invert-sugar.

percentage

follows: Per material


90. cent

invert-sugar
=the

after
per

inversion"
cent
sucrose.

glucose

in

the

:""0.95

required
of
selected

Determlnatloa
method of
to

Glucose
for

(Beducing-sugar),
glucose
material

"

The

be

depends
and also

upon

th^.

quantity
sucrose

this

substance

in the

whether

is present.
no

If

sucrose

is present, is to of the be

the used.

method
If
on

described both
page
sucrose

in and

the

ceding pre-

paragraph
are

glucose
be
ployed. em-

present,

one

methods

235

should

DETERMfNATlON

OF

SUCROSE.

180

TABLE

FOR

THE

ESTIMATION

OF

INVERTSUGAR.

190

CHEMICAL

METHODS

OP

SUGAR

ANALYSIS.

TABLE

FOR

THE

ESTIMATION

OF

INVERTnSUGAR.-Con"intt"l.

DENSITY

DETERMINATIONS.

APPARATUS

AND

METHODS.

91.

General

Remarks.
used
in the

"

^The
sugar

expression industry
chemists

"density" synonymously

is

very with
term
"^

commonly

"specific gravity."
the

Sugar
the

also the

frequently "density"

degree

Brix This

or use

degree
word
usage

Baum^

of

the

solution.
but this

of the

density
and
the

is not

strictly
will be

correct,
used The termed
92. in

it is sanctioned
sense

by
book

word

in
on

this

for

brevity
used in

and

convenience. work
are

graduations
"

hydrometers

sugar-

degrees."
Brix
was

Degree

or

Balling." by

This

system
the

of

eter hydromwere

graduation
afterwards

devised and

Balling;
checked in

data Brix. but

recalculated is known is used is the

by

This the ^'The in it


a

hydrometer
name

by

both

names

Germany,
in America. of
sucrose

"Brix'* Brix
sugar
to

almost

exclusively
by weight
commercial

degree
pure

percentage
In the total Brix

solution. consider
or

sugar
as

analysis
percentage
a

is of It

customary solid
is this

degree

Brix

the in

matter,
feature

the of the

solids, dissolved hydrometer, called, which


instrtunent in
or

liquid.
as

spindle,
renders

these
more

instruments

are

commonly
the Baum^
as

it

convenient The
a

than

sugar-house
a

work. in

degree

Brix,

determined
the
matter
oven

by
apparent
in
a

floating
degree

spindle
Brix.
as

sugar

solution, is termed
of total solid in
an

The

percentage

sugar called the


to

solution the

mined deter-

by
Brix.

drying

is often

true

degree
the This
on

Except degree
is

when

qualified
is

by

word be

"true,"
meant.

apparent

Brix termed

understood

spindle
scale The the

often

Balling,

and

the

readings

its

degrees
French

Balling.
use

two

modifications Brix-Vivien

of

this

instrument,
The 191 Brix-

Brix-Dupont

and

the

spindles.

19^

DENSITY

DETERMINATIONS.

Dupont
whereas
to

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

at

15"

C,

the

adopted by the
20" C. Both
The sugar

International

according Congress of
indicate cates indiin
in

Chemistry,
the
terms

of

these

hydrometers
solution
at

percentages by weight. percentage


of of the
cc.

Brix- Vivien in
a

hydrometer
of sugar

15" C.

weight and
well
to

volume,
that

i.e.,grams
the
Brix

100

of solution.
state

be It may modifications solutions 93,

spindle and
in

its

indicate

percentages

of
sugar.

sucrose

water

containing only the pure The Baume. Degree


"

Baum6 relation

(also
with

spelled
the
centage per-

Beaum^) point
water to at

scale

has

no

convenient of
any

composition
which the the standard

Baumd

sugar-house product. The hydrometer sinks in distilled


is marked of zero;

temperature
Baum^ but

the

correspondingpoint
gravity
is marked

in pure

sulphuric acid
the
range

66".
zero,

spindles are

specific also graduated


0"
to

1.8427

for densities is all that Gaslach


the

below

of from

50"

is

required in the sugar industry. Scheibler and later Mategczek and


of the

recalculated,
scale. The

values

graduations
are

of

the

Baum^
or

recalculated

numbers and scale

termed those
at
one

the *'new"

"corrected"
460.

degrqps Baume
The in the the

are was

given in the table, page


time used almost

Baum^
sugar

industry, but
Planters

at

exclusively present chemists usually prefer


sugar-^maker^ still
use

Brix

scale. scale.

and

the

Baum^ 94.
are

Hydrometers
for
use

or

Spindles.-^These
'^saccharometers"
when

instruments

frequently termed
in

specially
This

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


instrument for
is

the

provided
the

with

thermometer. made of

Instruments
metal
and
or

ordinary work,
without standard
the

in the

are factory,

of

and glass,

thermometer. for the

In America

many Ger-

instruments standard

hag

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

HYDBOMETEBS
r\

OR

SPINDLES.

193

corrections

must

be

applied to
normal
when
or

the

ings. read-

Hydrometers
temperature
distilled water and the the
water
a

whose

standard floated in

is

17J*'C.,

at this

temperature,
In

read 0". of

corresponding specifiegravity
is 1.0000. volume other of the sugar
to
at

words, the
solution of
at

weight of
17J" C.
same on

is referred of water

the

weight
The

the

volume page 450

1 7i" C.

table

is constructed

for this normal

temperature,
i 17

17i" C.
whose normal
as

Hydrometers
temperature
International
lU

or

standard

is 20*^0.,

specifiedby the try, Congress of Applied Chemisin water the


at this

when
10
10

floated

tempera*

ture, reac! 0", and

20

gravityis

0.998234. of

specific corresponding The specific gravities solutions,


with
the
corres^

the

21

ponding
Brix,
are "H

degrees
the

given in

table,

Hl^

page

477.

A
1on

In

using the hydrometer,


in the sugar and the

it is floated solution the

reading
at

scale is made
not

the

ig
17:

point R,
The of the and

R\ of Fig. 47.
is at the level

point R

surface of the

liquid
with tion. solu-

ing, is selected for the readsince R' varies


the

the

viscosity of

It is often necessary mate estisolutions to in dark


If 119::

the

position
The made

of

the

^
vo-

point R.
the after

reading of
until suflicient

scale is not

allowing
for the

time
jblOi
4(i.

hydrometer
of the
same

FiQ.

47.

to

become

194

DENSITY

DETERMINATIONS.

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

the solution.

If the

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
use

For

instruments

whose

normal

491 should be used. the

hydrometer

at near

It is necessary in accmrate its normal temperatiure. with caution and onlv

The
for from

correction tables should

be used the

approximate results when


the normal.

temperature
the

differsmuch

Hydrometers
on

the

paper

the

mercury

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

also made

with

corrections

The

writer recommends

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, since at most the
mercury

the instrument
emerges.

need
stems

be

lifted

only until

column

The

should

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

diameter, that the graduation may

be of very and easily

standardized solutions of
the The

pure

sucrose,

at

approximately
graduated.

temperature

at

which

the

instrument be

was

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

cylinder should

number

of grams,

five when

for instance, of distilled water immersed in the

at

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;
is most

convenient, since this is


in

the

temperature
For
whose

usually
accurate

employed
work

tables. preparingspecific-gravity of the should solution be

the temperature be detei*mined


from

specific gravity
for which
the
also

is to
1

exactly

that

Adapted

Bxilletin 13, Chem.

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

Uluftration.

1%
'

DENSITY

DETERMINATIONS.

sponding graduations of
.300, .030, .003, .0003,
hook
case

the
etc.

beam,
Each

and

graduationsr rider is provided with a


for other be

from

which
than of

additional
one

weights may
same

suspended
follows: above in

ia

of The

more

method
the

the falling upon using the balance

graduation.
as

is

pend Susthe

bob

of

the

balance

as

described
and

solution,at the standard


with
the

temperature,
balance

riders

until the

weight the beam is in equilibrium. Read

off the

specificgravity from the position of the weights the beam. on gravity Example: In determining the specific of a sample of cane juice the position of the riders was
follows:
1 at 2 not 3at
4 at
t

as

point of suspension of the bob


on

"=1 .000

the
.

beam.
=0.07 =0 =1 .009

7. 9

.r

Specificgravity
The

.079

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

that

they
the

may

be

filled with

definite volume

of

liquid.

weight with the weight of an


often
more

Given

of this volume,

equal volume
use a

be comit may pared of distilled water. in technical

It is not

necessary

to

pyknometer

work, the

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

of the most

of these is shown for the


excess

in

Fig. 49.

The

side

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 and tube. the
excess

provides

outlet

of

is blotted

with the

paper cap

at

the^ side

At the and
as

required temperature
any

is

placed in position

receives the

further

liquid that
to

temperature

rises

that

be pelled, exmay of the work-room.

TTKNOMETERS.

197
top of the
termine defor the

There
escape

is

minute

opening
in

in the

cap
/TN

of the air.
to

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

It is convenient

volume

of water Committee

at

17i" C.
on

The

national Inter-

Uniform 20" C.

Methods
as

of

Analysis adopted
at

the

standard
water

it to for the solution, referring

4"C., the

temperature
standard

of its used

maximum
is indicated

density. The
as

follows:

C. "-^-75 =1.07936,

meaning
solution each

that and

the" temperature that of


the
water

of the
were

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

that of the water. line, of the pyknometer, described By means in this article, the weighings can held by the readilybe made of the liquid 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

Fig. 49.

of water.

In both

cases

the

bottle is filled at 17^" C.


the standard

determining the specific gravityat


process
is
more

C,
the

the

complicated,since the expansion of


and
the

be taken into densitymust glass pyknometer The account. following description of the calculations, also the table,are
is first filled with from

air

Landolt's

work.*

The

pyknometer
are

recentlyboiled and
The

cooled distilled water, and

and The

is

weighed.
is the

temperature
mass

weight

noted.

weight

apparent

of the water

in the

air,a
great

constant

for the filledand

pyknometer
should

at the

temperature,
be

at which t^,

it

was

therefore

determined

with

care.

Optischem

Drebungsvermogen.

kJ

K8
The

DENSITY

DETERMINATIONS.

calculations
the

are

made
the

by the followingformula, in
values indicated below:

whicli

letters have

TFo,the apparent
Fj Q,
the

mass

of the

water

in the

air at

the

perature tem-

^oJ

apparent

mass

of the

sugar

solution

in the

air at

the

temperature

t;

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

"l=0.0012,

the

air

density;
at the

rf|= specific gravity of the solution of the sugar


t referred to water

perature tem-

at 4" C.

The

first factor

of the

formula
corrects

is the uncorrected the

specific
to

gravity, the
temperature

second and the

factor third

specific gravity for


the reduction

factor

is for

weights
The the end

in

vacuo.

value

of

may

be

taken

from

Landolt's between used for

table

at

of this article.
a mean

If the

difference
may

^and

t^

is small,
SPECIFIC

value, 0.00C024,
OF

be

3^.

GRAVITY

WATER

AT

VARIOUS

TEMPERATURES.

(From

Landolt's

Optischem

Drehungsvermogen.)

GENERAL

ANALYTICAL

WORK.

SAMPLING

AND

AVERAOINQ.

97.
"

General
of the for the

Remarks
most

on

Sampling
often is that

and

Averaging.

One

difficult , and chemist the

unsatisfactory, problems

c^mensugar of

sentative the
not

samples

juices and
manufacture.

diffezent

st.'^es of the

securing rq)revarious products ait If a sample does


value.

of

the In
must

strictly repnaent analyticalwork


order be the that drawn

the average will

composition of the material,


be

usually be of but little if any


may in

the

samples

representative they
to

continuously
Or, they

proportion
be

the
at
a

quantity
intervals,
measured

of

material*
a

must

secured
from

drawing
or

defini^^^

quantity in each
relation method
to

sample,
the
one

weighed quantity of the material, the size of the sample


same

always bearing the sami^ed.


and
The This is termed

amount

of material

second

is the

usually practiced sampling


four trated is illus-

sampling by aliquot parts.


of
a

Importance by the
and D from

proper

method

of

following example:
which
an

Given

lots of

sirup

A,B,C,
Let

average

sample is to be drawn.
Z)"*=200, and
let each mixture
a

A"1000,

5"800,
the others

C=500,
in

and

lot differ from


of

analysis. Manifestly a

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

be

true

oi B, 5 of

would

represent the average


the
to

composition
in

sirup. averaging
the

analyses of
the

various
use

materials

cane-sugar

house, it is advisable
Thus sdlids
**

the

weights rather
sucrose,

than and

the volume. the

wei^ts

of the

juice,the
be
sum

apparent
end of
a

(Brix)
"

should

recorded
of

daily

and

at the

run

or

period the

the 199

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

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
"

be

impossible to
that The will be
even

secure

moderate"sized

sample

of sugarcane
a

representativeof fairly
may

that of

field. able favor-

best the

chemist
to

hope
a

conditions, is

obtain the

accomplish, under sample that will in


to

very

general

way

indicate

condition
to
same

of the

cane.

Thfe
in

ficulty difthe

in of iinalysis

sampling
canes
a

is due the

the

great

variations

from

stool and- also from

various

parts of

even

small
from

field.

Frequently in
to

large factory,

receiving cane
will differ but may
vary

many

the fields,

daily average

little from

day

day whereas

analyses single analyses

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
follow
It

close is
even

behind
more

the

cutters.

difficult to almost
of

sample standing
be

cane,

since
case

the
a

field is entire

an

impenetrable jungle.
cane

In
from
or

this

few

stools

should
from
near

secured ditches
a

various

parts of the
and after these

but fields, should

not

headlands, number,
cane

canes

be

reduced

to

convenient

mixing them thoroughly. of sampling the whole Perhaps the best method
await its arrival at
the

is

to
or

factory, then

car-loads 99.

other and apart from cane, at the the Cane Sampling be

grind several cartanalyze the juice.


accuracy

Diffusion-bai^ry."
considerable

The

cane-chips may

sampled with

SAMPLING

BAGASSE.

201

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

the half

diffuser,and
filled. metal

second

handful

when

the diffuser is about stored in


a

These
or

samples
agate-ware
be taken

should

be

clean
in

covered this
way

should
and be

to

pail. The samples the laboratory at

drawn

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
intervals
of diffusers. Pellet
a
*

frequent The milling

recommends twelve

the

storage of the fresh chips during


open

period of

hours, by placing an
ammonia
in the

bottle containing

concentrated
box. 100.
"

covered

sample-pail or
Diffusion-

Sampling

Bagasse

and

Exhausted

chips. ^To a certain extent the bagasse presents the same The bagasse,however, cane. as the whole sampling difficulties 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
and preservative
In

be attached

to the

inside of the box-cover.

diffusion
a

work, the
from small

exhausted each

chips
as

are

removing

handful

diffuser

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
"

one mill-juice,

from

the first mill and

the second

from

all the

Bulletin

Aasoo.

des

ChimisteB,

XXII,

922.

202

GENERAL

ANALYTICAL

WORK.

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

mills.

It is

tb draw preferable

the firstof these

sample

at
as a

this

Brix of this first sample is used so-called of the normal

juice or

undiluted

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

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

mixed

from

the

or

the crusher

first mill and

juice that would


without
a

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

maceration

water.

This factor should in the


season

be determined its Tariathe

Bufficient number
cane

of times

to note

tions with crusher

and

milling conditions.
and first mill) and The

The that

juicesfrom
from"^ the be hour

(or crusher
are

entire

system

separatelysampled.
devices first and should be

sampling should
for
an

by
or

automatic

continuous

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 crushing by the mills which and many of the impurities of 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
account

of

the

v"ry

heavy

and
20"

use

of the factor:

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 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

GENERAL

ANALYTICAL

WORK.

screw

for

adjustingthe

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
at

of the

cavity and consequently inch hole is drilled at right angles to


size of the

the

outer

end

of the

barrel

and

the be
an

other oval

and the juice-inlet

outlet.

Th^re

should

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 reciprocating part of the juice-pump, reducsuch 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.
A

the

device wire The

that may

be used
from

under
stream

favorable of
a

conditions

is

heavy
bottle. the

leading
wire

the be

should

given

juice to the samplesharp upward turn at


keep the wire free
of

delivery point. It is
further it should

necessary

to

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. be The axle of the wheel be tubular and should be hollow and
a

trash and

few of the

spokes

should

communicate

through the axle with the


terminate in small deliver littleof the

sample
spoons

jar.
which

The
serve

hollow
to

spokes should
a

take up

juice and

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.

it

Samples acting pump


The valve
pressure

may

be drawn

from of
a

by
should
at

means

discharge-pipeof a direct spring-controlledrelief-valve.


open
at

the

be

adjusted to
pump

the moment

of

est high-

each

stroke.

EAMFLING

THE

JDICE.

205

The

difRcultywith
is their hability their sampling
and

most
to

met, erfthese samplers, except the Calu-

clog, tendency
to

to

foul, uncertainty quantity


of

as

to

in proportion

the

liquid
from The

paaaing them sample


canal under into

the probability of not

drawing
mills

an

average
a

certain the

conditions, juices from

e.g.

when

drawing sample
a

which

several
a

flow.

Calumet
is

sampler
with
the

draws necessiurily

correct

when and

it is

connected

the
latter.

dischai^
When from the

line this

from

pump

operated
with the
a

by
canal

sampler
its
a

ia connected

leading

crusher

sample

is from

only

part ol the juice, but


of
a

it is usually

very

good approximation
all mechanical

representative sample.
superior
necessary to

Almost

samplers
It

are

hand in

and

drip samplers.
the

is often
a

sampling

mixed

juices

to

draw

small

measuring-cupful

of juice at regular intervals

and

^th

these
is used

form and

composite
defecators
drawn
one

sample.
are

If the

defecation small
ured meas-

system

the be

large,two
each filling

samples
if the

should
are

whoii

tank;

but

defecators

small

sample will suffice.

If the

206

GENERAL

ANALYTICAL

WORK.

juice flows into


Bimilar
drawn processes,
as

Urge
one

as ttning-tanlui,

in the

Deming
should when

and
be

or

more

small for has

samples

the

tank

is

filling, one,
tank

enunple,
three
or
a

the

four second

feet of
when

juice in it,and
it is If the

nearly filled. juice is


it
or

first

pumped
to

into
from

small which

measuring-tanks,
flows the

liming-tanks,
the

defecatora,
be
or

sample

may

drawn
a

by

the

Horsin-D^oii

siicilar

automatic
below

sampler

as

described

for difFu"on

work.

Duplicate

samples
for

should

be

drawn,
for the

one

the the

density
other

determination

and

polarization.
for the

Methods
tion

preserva"of

of

the

samples

juice
to

and them
page

observations
are

in regard farther
on

given

in

207.

102.

Sampling
"

DiffustOBprocess

Julce.

The

diffusion
measurement

requires the
the

of

juice, drawn
a

from

each

diffuser, in ing-tank.
facilitates
,

small

meaaur-

This

measurement

the automatic

dmw-

ing of
means

the of

juice
the 52,

sample
Uorsin-Dten

by

sampler, Fig.
This

apparatus
cock

consists of
for

three-way
Flo. 62.
a

connecting
alternately
and
float. It is

small

stand-pipe

with

the
a

measuring- tank
suitable

the sample-bottle and The


BO

is operated by
the

sampler
that

is

placed inEide

measuring-tank.

arranged

the sample

of juice drawn

is proportionate

PRESERVATION

OF

SAMPLES.

207

to

the

quantity of juice
battery should
The inlet to

in the the

tank.

The

discharge-pipe
the

from

the

enter

measuring-tank from

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

sample
Care

may

not

be

representative of the
Preservation of
a

tankful

of

juice.
103.
"

of

Samplers.
the

Samples.
source

^In order

that

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

infection

and

sampler itself may not be the decomposition of the

of

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.
Where measured
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

have the

small

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 These time of

prevent sticking when

daily; usually
10-15
cups
cc.

3-5

cc.

cup

for the

sucrose

sample

before

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

the

samples the
The

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
a a pump single pipe-line,

sampler of

the Csdumet

type

may:

208

GENERAL

ANALYTICAL

WORK.

be

connected

with

the

juioe-pump and

be

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 pumped
A must preservative

If the

juices are

be added

to the

samples in compositing.

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
are

1 part of the not


sucrose

juice. Formaldehyde samples that


The
most

should in

salt per 5000 parts of be used in compositing and

to be used

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 juice with the preservative. the sample should be thoroughly mixed of lead is used in solution, estimate of If the subacetate an
of This salt must periods far exceeding 24 hours. used in excessive quantitiesand after each addition for
not

be

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
per
use

should

be added of the
sucrose.

to make

the total

dilution 10
enables It is the

cent

of the

volume table for

juice itsdlf. This


in the
over are

of Schmitz's

to composite the samples preferable thus givingthe chemist a good control itself,

laboratory
the

sampleat

boys, and making regular intervals. 104. Sampling


of the the press and

sure

that

the

subsamples
Cake.

drawn

the

FUter-press
varies This itself.

"

^The

position com-

cake filter-press

in different

parts of

of the cake

makes

accurate strictly

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

8AHPLIN0

THE

FILTER-PRESS

CAXB.

209

pariaoDS
The

are

obtained various

by cutdog

pieces

of

the cake

ayetemfor this

atically fh"m

parts of the press. in Fig. 53 is very suitable

inatrummt

shown

sampling.
that
This it may latter

It ia made

of

heavy
the body

brass the
or

and hand

of such
over

size

readily be grasped by
ia fastened
to

the

cover.

receptacle by bayonet

210

GENERAL

ANALYTICAL

WORK.

catches thick The

and
and

8et""8crew.

The in

cutter

is

brass-tube
the

ind'i

about

i inch

diameter

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
may

cutting edge. the receptacle,so

be

filled from of

each

press.

The

pressmen

should

cut

number

plugs in the usual


are

procedure,

e.g. from

various
so on.

parts of the second


The

cake, then from


in the

the fifth cake

and

plugs

accumulated and

in the

cutter

closing it. A

receptacle, one remaining small tube, open at both


cover

ends, is attached
saturated
with The

to the inside of the

and

holds

sponge

formaldehyde, sample should


be This

for
sent

the
to

sample.
time and
a

preservation of the the laboratory each


on

press

is filled. of presses

provides a check
The

the

sampling

count

cleaned.

cleaned
the presses. The

after removal

oughly sampler should be thorof the plugs and returned to

sample
a

may

also be obtained
for

by
the

means

of^
A

brass-tube,
cork-borer used The with

fitted with
may
care

piston

removing

plugs.
must

be
on

employed
account

for the purpose,

but

be

of risk of

cutting the filtercloth.


vessel in
an

plugs
rated satu-

should

be stored with

in

covered

atmosphere

formaldehyde.
or

"It is difficult to control

check

the

there is a natural as cake, especially 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.

sampling of the tendency for the

press-

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

WORK,

boilera uauaJly fill the if the


p"ns
are

pans

to

the
one

same

point;
measure

in such
answer

tsaees,

of uniform there
pan.

^ze,
be
a

will

for

otherwise ftlt,
one a

should A

set

of proportionate meaaures,
funnel of

for

each

small

stemless

glass forms

convenient Holasaee

measure.

is sampled

in the

same

way

as

sirup,and, according
are

to

the

exigendea
or are

of

the

worii, the
A

eiunples
from time

analyzed
of
the

separately
the

composited.
be the of

composite

sample
to

final molasses
determination the solids

should

prepared
sucrose

time
method the

for

by
the

the

Clerget
of

and

by

drying

for

calculation
a

true

purity.
of the 107.

These

samples should
Sugar.

represent

definite

quantity

material.

Sampling
remove
a

"

The

workman

at

the sugar-scale
of
sugar
aa

'should

sample

from

each

padcage

ite

Fta.

M.

weighs it.

The
a

samples
The

should

be

thrown
to
so

into
receive

tin-box

provided
shown be

with

funnel-shaped

opening
samples

them,

as

in Fig. 54,
at

composite
six

obtained
an

should

analyzed
be made

frequent
every

inten'als, preferably
hours,
and the be number

analysis
packages
use

should

of

represented by calculating the


In

the

sample
in The the

should

recorded

for

in

averages.

sampling

sugar

packages
is
a

"trier"

is

usually
instru-

employed

(Fig. 55).

trier

long trough-like

SAMi'LING

SUGAR.

213

ment,
on

which,

being
remove

plunged
a

into

quantity

of

sugar,

will,
sugar be

withdrawal,
which

sample passed.
all
as

representative
This

of

the should

through

it

has

sample
and

thoroughly
to

mixed,
as

reducing
a

limips,

exposing

it

the

air

short
are

time the

possible.
S.

The

following
sugars:

U.

Treasury

instructions

for

sampling ''Sugar
be

in

hogsheads putting
chime
in be
cases

and the
to

other

wooden

packages
through
constitute

shall the
a

sampled
from

by

\6ng

trier
one

diagonally
trierful
when
an

package sample,
of

chime,
of small
from

to

except
shall

marks,
each

equal
of the

number mark
to

trierfuls

taken

package

Fio.

6"

furnish
out

the

required
of

amount

of

sugar

necessary

to

carry of

the

provisions bags,
ceroons,

the and

regulations.
mats

In

the trier from

sampling
will the be

baskets,
care

the

short

used,
central the in

hping

exercised of
from

to

take

the and of

sample
in

fairly
such

contents

the each When

packages,
class the short hard triers

manner

that be uniform

samples
quantity.
the
use

packages
condition

shall of the the

sugar

renders may be

of

the

impracticable,

knife

used." The

Treasury
in
a

regulations
lot, instead
conforms of
to
a

require
certain conmiercial

the

sampling
of

of

all

the
as

packages

proportion
usage.

them,

formerly.

This

ANALYSIS

OF

THE

SUGARCANE.

108.

Estimation

of

the

Sucrose"

Direct
cane
a

Method.

"

The

first step in the

analysis of the
As has be and been

is the

tion prepara-

of^the sample.
sample
with almost the of the
cane can

shown

representative work,
usual but it is

obtained
without

in diffusion

milling

process to

special apparatus
With
the

impossible

accomplish this.

facili-

FiG. 56.

ties,such
neither be
nor

as

knife

or

shears, the

sample
to

of whole
error

cane

can

prepared rapidly enough


in
a

avoid

suitable
sucrose.

state

of the

division

by ation, evaporfor a thorough


canes

extraction it should different

of the be noted

In the

analysis of whole
varies

that

composition

greatly in
tion prepara-

parts of

the

stalks, thus
be

complicating the

of the

sample.
cane can

Whole

rapidly and

properly shredded
214

by

ESTIMATION

OF

THE

"

StJCROSE.

215

""

fneans

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
of this
one

to

another

and

between vibrators
canes
are

them,
or

bearing lightlyon
forced
Li feed

the is

cylinder, are

steel

arranged to press the the machine, the saws


on

fingers. A against the saws.


at
a

operating
part
of

driven

very

high speed, and


every

account
cane

of

the

staggering of
to
a

the

blades and into

the

is reduced throws

fine SBW-di"st

hair-like
a

fibers.

The is

machine-

the

prepared

cane

box

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
in the
per

residue of the

fnnn

the

diffusion

was

never

more

than

0.07

cent

weight of the
Place
100

cane.
sucrose

For

the

direct estimation follows:


or

of the

in the

whole

cane

proceed' as
suitable

grams add
ten.

dish

.beaker and
boil add another
ten

prepared eane approximately 200

"^

in
oc.

of

and boiling water off the liqtHd and and tions the the

during

minutes; oarefuUy
cc.

drain

portion of -200
minutes.

of water,

again digest during


with
water
a

Repeat

these

diges-*

in all

seven

times, and
other
from

after- the

last press

residue' in

hydraulic or
it and ako in
a

powerful press, uniting


the

portions of solution weigh


100
cc.

drained

chips. Cool the


its

liquid and
To

determine

degree Brix.
of
oc.

of this solution

lead After

for

clarification and

add subaeetate sugar-fiask 110 to complete the volume filtraition

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

thorough mixing and

506.

Froto

the per

cent

sucrose

in the soiiitioh and

the

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


f

the
m
"

wieight of isudxise.^ This


100 grams

of

cane

or

the

^roentiageof

sucrose

in the

cane.

This

macluDe
it is

ho^s Teoently
now

been
as

somewhat
"

modified

from
cane

that

of

the Bffure and

known

the

Warmoth-Hyatt

reducer."

216

ANALYSIS

OF

THE

SUGAR-CANE.

109. Methods.

Estimation
"

of earlier

the

Sucrose. of

Indirect

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

the

days

as

derived
^

by deducting the
called attention
cane

marc
error

from (fflber)

100.

O.
ing assum-

H.

Francis the

to the to be

.ofthis method

in

juice of the

experimenters have juice varies in the


contains is almost be

also shown
same

other homogeneous. Many that the composition of the that the


cane

part of the stalk and


colloidal
sugar. water

water,
or

termed

quite free of
into
a

If

by Soheibler, that piece of a stalk of cane slowly pressed,


of the
sucrose

entered will

small

hand-mill

and. be In view

water

dripfrom
cane

the free end.

tions of these considera-

it is evident
content to terms

that
must

an

indirect estimation include the tise of


a

of the

factor to reduce

of the undiluted and


no

juice. This

factor

quite variable
The
use

great reliance should


is discussed here

necessarily be placed upon


account

is

in which analyses, above

it is used.
on

method

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
'

method.'

In order that
must

such

experimental data
conditions
as

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


a

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
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 of indirect
or as or

in

the

extraction

of

the

The

Royal

Agrioultural and

Commercial

Society

of Britiah

Guiana,

11th

June, 1885.

WOODY

FIBEB

OR

MARC.

217

diluted

Juicesfrom
or

ftllthe mills is ascertained

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 in

cane

the

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

weight
sucrose

of

sucrose

in the

cane

is the

sum

of the

weights of
divided

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

in the

gives the percentage of


There
are

in^the cane.
that
may

several

in the above of the


water

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

conditions

lead

parts with

more

less moisture
may

through
measures

the and

mills; there
modem

by evaporation in passing be inaccuracies of weights,


need
are

analyses. The
mills of

first of these

not

be

pected ex-

where With
run

good

construction

operated.
to

the old types of

mills,however, it is often
the

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
water upon

of

saturation-water the is

and

the

dilution moisture
constant

number.
cannot

The

error

from but

evaporation of the
very

be
a

eliminated,

probably usually
Inaccuracies

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
source

given millingweights, sampling and analysis

in

of

error.

The

of accurately sampling impossibility


use

whole of

canes

usually precludes the factory control,hence given preference.


110.

of the direct method method

analysisin
be

the

just described should

Determination should be

of tlie

The

samples
a

50 grams

of the material

to

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

Stretch

piece of washed

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 the replenishing
water.

The

linen

is

designed

to

serve

218
as
a

ANALYSIS

OF

THE

SUGAR-CANE.

filter. with

Digest the cane-shreds


warm

two not

times hotter

of ten than the of


warm

minutes
75**

each

distilled solution into the

water,
time the

C
,

pouring washing
adhere
to

off the

each beaker the

through

linen,
cane

and

back the

filter. After

fragments with digestions


liquid
at
as

that

water,

digest the
beaker further and

cane-shreds

five times, of ten off the


an or oven

minutes before.

each, in

boilitig water, pouring


residue in

Dry
is

the
no

100** is
a

C, until there

loss of weight,
Use

until there smaller

slight gain

over

the

previous weight.
The of fiber The
marc

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


the
or

in the

cane.

dried

fiber and the

linen beaker then

attract

moisture
contents
as

with

extreme

rapidity;therefore
in
a

and

should
as

be

cooled

desiccator
to

and

weighed
the beaker
on

quickly
of the

possible.
proximate ap-

Preparatory

weighing
should

and
one

residue, their
where

weight

be

placed
be

balance-pans. frequent
are

Special apparatus

should direct

employed
This should

fiber-determinations
be

quired. re-

operating
to

with
cane

capable of comparatively large


or

quantities of
reduce the

bagasse
error.

in order A
venient con-

sampling
form

apparatus
This is
a

is shown

in

Fig. 57.
tractor ex-

simple
is The

of Soxhlet*s

and
or

made

brass.

body
12 inches

of thiti copper of the extractor, 3.5 inches in


are

i4, is approximately
diametel* and
to

long. Lugs
a

provided
about the 3

support
above The of bottom

cylinder, B,
the bottom
of
a

inches

extractor.
cover

cylinder has
80-mesh is of the

removable
gauze

wiresame

and

the A

material. i!|J hold from

of cylinder grams

this size will of shredded


cane.

50 to 100
or

bagasse
FiQ.

larger weight of
below the

57.

The

chamber

lugs is

to

quantity of

shredded

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

220

ANALYSIS

OF

THE

SUGAR-CANE.

percentage
the The
100

oi

Juice
of

66lids

in
and

the
the and

bagasse
purity
the in of

is
the

calculated
residual

from

percentage
sum

sucrose

juice.
from

of the

the

juice

solids of from
to

moisture
the

deducted
The the

give
the train The

percentage

fiber the

bagasse.
of residual the second in

purity
mill in

of the

juice
is

flowing
considered

bagasse-roll
that of the

last

be

juice.
indirect
the

following
Per
cent

example
of

illustrates

method:
4

bagasse,
48 per

25; cent;

sucrose

bagasse,
purity,
100
"

per per

cent; cent;

moisture,
then

residual

juice

78

4-T-.78a"5.13

percent
fiber in in the the

juicensolids; bagasse;

(6.13+48)
=

=46.87

per

cent,
or marc

25X.4687

11.72 The

per

cent,
has with

fiber

cane.

writer

compared
the calculated methods

large
fiber is

number

of method that in

analyses
(2).
he the has

by
The continued dis-

method

(1)

by good
of

agreement

by
the

the direct

two

so

determinations

fiber

bagasse

in

the

factories

under

his

superyision"

(See

also

158t)

ANALYSIS

OF

THE

JUICE.

111. of the

Determination

of
determined

the

Density." by
or means

The
an

density
balance

juice is
be

usually
a

of

hydrometer
convenient
are

(94), though
(95)
may

pyknometer
The Brix

(96)

the

Westphal
more

used.

spindle is the
fiince its

hydrometer
The
as

for this purpose, coefficient of


on

readings
the

used

in

the calculating

purity.
scale, or
the

readings
be converted
on

the the into 477

Baum4

specificgravity
or

determined

by

Westphal
degrees
or
on

balance Brix

pyknometer, by
means

may.

scale

of the

table

page

page

482, according

to the

ard stand-

temperature
In with

selected.

using
the

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

air-bubbles.
minutes The
escape carry to

time
an

required for this usually


into the lowered

varies
ten

from

few

hour, but
be

minutes

suffice.

spindle should
of
away

cylinder, after the


to

the

bubbles, causing the


it the siuface. froth and the

juice

overflow

and

with

mechanical blow
on

impurities,
the surface froth. The

floating upon
of the

It is well to
to

juice

as

it overflows
now

help

remove

the

spindle should
floats, taking
it sinks. of the directed of the After

be lowered
not to wet

farther; into the above the

juice,imtil it point to which


temperature
the scale
as

care

the stem

allowing sufficient time


reach that of the in
use

for the

spindle to
in 94 and

juice, read
The

illustrated be noted for

juice should
temperature
is

temperature Fig. 47. in correcting the observed

density.
The

correction
made

when

using
24" C. the

spindles

whose
480.

normal For

C. is 17i**

with Brix

the aid of the


at

table,
be the table

page

example:
and

Let

18.15"

observed of
221
correo-

density

temperature.

Referring to

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 corrected below

.44, which
17 J "

must

be

added Had

to

18.15, makture temperahave been in is used

fj

ing

the been

subtractive.

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


18.59. corrections for The table of

the

making
at

tanperature
477.

instruments

standard

C. 20"/4"

comparisons fot these instruments

is given in page
11^.

j
of the Trne

Determination Solids

Degree

Brix Method,^
pass

or
^ "

Total

by Drying.
two

Carr and Saiibom^s sizes. should


a

I
a

Prepare pumice-stone in
Ir-mm.

One
a

size should
6-mm.

sieve

and

the

other

perforations. Place
S
mm.

pass layer of the


a

cular sieve,cirfiner pumice-stone dish ; lead


caps

thick
are

on

the

bottom

of and

small

metal

for bottles Place


a

convenient the
coarse

inexpensive for this purpose.

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 oxidizable of materials containing much 70" C. in case readily

layerof

mafcten

The used

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

solids. Method
to

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


"

was

gested sug-

which

it

differs in the Courtonne


to

construction
the

of the

oven

and and

drying-bottles.
makes
a
no

heats

bottles

in water, and

vision pro-

prevent

the return

of re-evaporation,

part of

the water The and and


oven

of condensation. is shown in

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

Bull.

46

Div.

Chemistry,

U.

S. Dept.

Agriculture,

p. 45.

DETERMINATION

OF

THE

TBUE

DEQBEE

BRIX.

223

double, and
by
all
a

the

space

is filled with
or

air.

toy steam-engine
the
oven

other
a

small
very

motor,
unifonn

fan^ D, driven agitatesthe air


temperature
in

inside

and

insures

of it. paorts The A, drying-bottles. with


a

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

tubes

central

Fxo.

58.

condensation
The

in the

tubes,from

back falling

into the bottle.

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

OF

THE

JUICE.

Materiab temperatures,

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
to

expel the last of it.


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 is made with the

factory^svacuum-system
rest upon the

by

means

of

pressure-tubing.The dishes

FiQ.

59.

bottom

of the of the

vessel porcelain
bath.
A

and

are

heated
not

dish

should

be

temperature placed directly


a

to the

under

the

outlet

except this be provided with

water-trap
shallow
at

similar to that in Pellet's Method nickel


center.

Fig. 58.
for
mm.

Total

Sdida.

"

Pellet
20
mm.

uses

capsule 85
The dish

in diameter
a

and

deep

the

has

central

depression about

one-third

depth of the dish and one-third its diameter. ground to pass a 1-mm. Freshly ignitedpumice-stpne, 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

INDEX.

225

10

grams

may

be used.
and

This

is then

diluted with

little

distilled water the


over

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


the entire bottom of the
3

etc., the material


water.

(about

testingmassecuite, grains) is weighed in the central


In

capsule.

depression and is then dissolved in about


This solution is absorbed

cc.

of hot distilled and is followed

by the

stone

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

Finally the
is dried added

stone
oven.

is distributed
A

as

before

and

the

material should be

in the

drop

or

two
a
a

of ammonia
trace

to material

In another
sugar to which

containing even method, Pellet makes


water

acidity. paralleltest, using


of

pure

equivalent to that in the material


The when

to be

tested

has been

added. and

capsule containing the


it
ceases

sugar

is the

weighed
other

at intervals

to lose moisture

dish is assumed
"

Jossers Method.

only dry matter. used ^This method was originally


It has been of

to contain

in

tain cer-

work. agricultural time is


to

slightlymodified Tempany
597,
a

from

time.

The

modification

and

Weil

given here.
A No. stripof S. " S. filter-paper,
a

58

cm.X2

cm.,
cm.

is

rolled into
X 2
cm.

tightcoil and
After

is placed in

weighing-tube 12

stoppered and
10
cc.

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

of

juice is distributed
is now

paper.

The

tube

with

the

stopper removed
in
a

placed in

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
to

control
vacuum.

the aiiw;urrent

and

mercury-column
Total and Solids Smith's
'

to

regulate
the

the

113.

Estimatton Index.
"

of

the

from

Refractive

^Tolman

investigations

"

W.

I. Bui.

1912,

12, 89. 1906, 28" 1470.

"

J. Am.

Chem.

Soc,

226

ANALYSIS

OF

THE

JXHCB.

showed

that

most

sugars the
same

in ^^solutions of

equal percentage
that used
^

composition have
Geriach's with
was

refractive indices, also


may

table of Brix
error

hydrometer ccurections
from
room

be

small

to correct
use

temperatures.
indicates low
use

Main He

the first to that the

the refractometer index

in refinery work.

found
content

refractive
matter

of soUd West
"

in all but the The first to tables

acciu*atelythe products. Geerligs


refractometer and in

and

van

were

the

cane-sugar

factories.

of

Tolman

Smith,
agree

Main, and closelywith by the


examination

GeerUgs, after
one

temperature
refractometer if the

correction is affected material

another.

The

only

solids in

solution, therefore
insoluble matter
solids. Within

under

contains of the

this is not its

included

in the estimate materials

in limitations, i,e,, and


a

containing only soluble


of non-sugars, indications
as
as

solids

small

portion pro-

the refractometer
to

is

very

accurate
as

the

soUds

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

those

sugar

maker, in order
molasses

and

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


to at least for
a

the suitable tiont and

or purities

time.

These have

consideradeterred

the
from

conditions

obtaining in Cuba

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

refractometer; (2) immersion refractometer; instrument. form of Abbe (3) sugar refractometer, a special (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.
^

viz.:

(1) Abbe

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
one

of the

prisms

is

1 "

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

Int.

CentnJbl.,

1008, 79 (1),80a

228

ANALYSIS

OF

THE

JUICE.

range

it is
for

more

accurate

than

the

other
of

types

and

is

quite
the

suitable
and

juicea

of

the
are

usual

range

density.
dealers

tions Instruc-

special tables

supplied by

the

with

"3) The
Abbe's
in the

augoT

T^TOcUmteler,' Fig. 62, is


and has been

^"ecial

fonn

of
use

instrument

designed especially for prisms


of the

eugar-induBtty,

It has

the double

Abbe

Fto.

ai.

instrument

and

dilTers from the

this in the

optical nature
SchAnrock, graduation
"rfdry and

of the and in
a

glass forming having


a

prisms,

designed
Tiie

by

modified

comparator.

is uptm

cylindricalglass strip located


The
the divisions

in the field of view.

of the scale read


0 to 50 in

percent^^
1 per cent

Bubstanoe,
to 85 in

interval

between

60

"

Abstracted

troEn

Zeiu'

inMnntiomi.

REFRACTIVE

INDEX.

229

0.5 per

cent.

Within
to

the

mnge

from

0 table

to

60
and

the
from

scale
60

is
to

'Rraduated
85

according
to

Sehoiirock'B

according
or

Main's

table.
upon

I^e

temperature

standard,
size in Fig. carries the

20"

28"

C,

is

engraved
E

the instrument. in about


a

The

refractomet"r
The

is shown

one-third
which

62.

upright

is fitted with
an

hinge J

easing G, together with

iudependeutly

hinged telescope.

Fio.

62.

The The

OK eyepiece

and

the handle
are

of the telescope are


with
an

shown.
for

priamB, M,
The

N,

provided
to that
a

arrangement
Abbe which when F

temperature (1).
with

control

similar

of the

instrument,
is

prism

is fitted with D. This

window
window The

at R

usually
ing observaccess

covered
very

the cap

is used
cap

dark-colored
zero

solutions. of the scale.


"

gives

for adjustii^ the

Setlinn Ihe Refraelomeler.


the

Place B
on

the instrument
the left and the

in front
mirror

of

observer

with

the handle

Sp

230

ANALYSIS

OF

THE

JUICE.

toward The

window of

or

an

incandescent be about

electric 18

or

gas

lamp..
the

source

light should

inches

from

mirror.

Applying
handle surface B

the

Sample,-"Open
prism with

the

prisma by
solution
A

means

of the

and

place

JEidrop of the
a

upon

the matted

of the lower

rod. the

glass rod should be used. after applying the solution.


"

Close

smoothly rounded prisms immediately

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 the Instrument to the Critical Line. Setting
"

can

be

turned

over

the

entire range K.

of the the

scale with
zero

the
of

assistance the scfle

of the and

handle the

First set to

point

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 which to the division lines of the scale, separates parallel line, less intensely dark. the bright portion from more or one ness change of the inclination of the mirror the brightBy a slight of the field should be tested,while the critical line remains
focus

stationary.
Reading
the
the Scale.
"

^Tum

the with

eyepieceby
the

means

of K

until

critical line coincides Read

the cross-hairs. line In


remove crosses

the scale at of
a

point of intersection of the point where the critical


cent
must

it.

Fractions dark
from

per

be estimated.
over

observing very
the cap
to
an

turn solutions,

the mirror

and

white
not

be

seen.

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

R.

The

be noted

between

very

dark

and

very
as

brightpart
has been
are

of the

field. Bring this line into (Coincidence


and read the scale. the maker

described
plied sup-

tables Temperature-correction with each instrument.


"

by

Examining

Viscous

Solutions.

warm Slightly

the

prismsby

DETERMINATION

OF

THE

STTCROSE.

231

water circulating

through the mounting.


the

Apply
the

the

solution

to

prism and
the

promptly make
of

observation. 114. Solids. moisture


most to
"

Notes

on

Estimation

Total and the

^The determination

of the total sohds

in sugar-house materials
is due the their
to the

is

one

of

tests the chemist unsatisfactory

is called upon

make. several

This of
to

ready decomposition
and

of

constituents

under

some

conditions
It

tendency

to

occlude
that

moisture.

is advisable to

select methods
average

give fairly
and

comparable results under


to
use

conditions the

these in
an

at

all times.
same
a

If

the air-oven, kind of

ducted drying is conweight of material,


!"-

the

same

size and

and
at all times

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


a

"2.

for

given class

of materials.

perature tem-

/\
III "ft
"o

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

that is

s
" "

u{

O
a u "

high

temperatiu'e
water to avoid

(105** C.)
the other

to, drive
a

off low

the
tem^

occluded

and

S
-

very

"

perature
115"

decomposing the invert


of tlie for

sugar.

Determination

Sucrose.
This have
not

Special
method been

Pipette
is

Measurements.^"

applicable with
so

juices that
of that

preserved with
mark,

subacetate

lead.

The

pipette, Fig. 63, is


the

graduated

if filled to

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

52.096

grams,

normal

weights of

the

Hqu*d.

Evidently the pipette may


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

be graduated for

othe^
the

than

normal carried the

weights
m

(52.096
in

stock

dealers,and
of 5" to 25"

uated gradBrix.
'

range

of densities

"

This

pipette
"

was

devised

by

C.

A.

Crampton
the
same

and time.

G.

L.

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


"

It is

I)
Fzo.

sucrose

pipette"

by

tbe

dealers.

68

232

ANALYSIS

OP

THE

JUICE.

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

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

the the

author

prefers
tube tl"e

tube

short

while of

pipette draining, leaving the


such
measurements

chemist with In
as

free

to

continue

series

other

pipettes. using this pipette


Determine

follows:

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


Brix

in the

hydrometer,
correction.

noting
Fill the

the

degree pipette with


3 to 5

without
.

temperature
mark
sponding corre-

juice to the
of diluted
to

with into
a

its observed flask. Add

degree Brix, and


cc.

dischai^e
with

it

100-cc.

lead subacetate
cc.

solution mix

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


tube, and
the 2
to

100

water,
Polarize

of the.flask. divide of the

the filtrate, using a 200-mm.

polariscope
The

reading by

obtain

percentage
the
allowed for

sucrose.

juice should
and

not

be

from expelled
should be

pipette by blowing,
thorough
connection age. drain-

sufficient time

The Home's

sucrose

pipette

may

be

used

in

with after This

dry-lead method

by making
that

the measurement observation.

at the temperature filtration,


use

of the Brix

of the

pipette

obviates

of Schmitz's

tables, but

involves The balance.

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

corresponding

to

an

uncorrected

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

52;096

of the solution. advisable


to
use

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

It is not

these

pipettes with

and should

molasses be

for

guidance in the
with

vacuuma

work.

They

frequently cleaned
of the

strong

solution
116.

of chromic

acid in

sulphuric acid.
Sucrose. General
to the

Determination
"

Methods.

^The

necessityof adding subacetate of lead

DETERMINATION

OF

THE

SUCROSE.

233

juice in sampling somewhat


of the If author measured With

complicatesthe
chloride is

measurement

sample for analysis.


or

formaldehyde
does
not

mercuric the

used, which

the be

recommend,
the
sucrose

with the

sample for analysis may pipetteor otherwise.


of lead used
as

solution

of subacetate
as

serving pre-

agent proceed
Determine Measure subtract volume the

follows: Brix of the

duplicate sample. the composite sample, includingthe lead solution;

degree

the and
to

volume from
these

of the data

lead

solution

from

the

total

calculate
110 per

the amount
cent

of water

required
volume.

dilute the the

juice to

of its

original
mix the

Add

calculated

volume

of water, and

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

Example showing
Volume Volume of

the methods

of calculation: 2705 125 2580


of the
cc.
"

juice and lead solution.


used

of lead solution of

Volume Ten
per cent

juice

cc.

of the volume of 2580

juice

-"

one-tenth Volume Volume The


cent

258 used 125


133
.

cc.
"

of lead solution of water

required to be added.

cc.

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

cc.

or

110

peir

Degree Brix of duplicatesample (uncorrected) Polariscope reading.


'

18.0
60
.

It is advisable

to

acidulate normal

the

water power

used
to

with the

acetic

acid

to

restore

the

rotatory
from

levulose

be present. that may is ascertained The sucrose

Schmitz

table

as

follows:

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

234
the

ANALYSIS

OP

THE

JUICE.

tenths

of

the

number,
The lead

16.11, is the
may

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


in
a

sucrose

be detennined follows:

juice,not
100
cc. cc.

stored

with
a

subacetate, as

Measure

of juice in
and
110

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


add

100

cc,

sufficient subacetate

of lead solution
to

for the clarification,


110 cc,

usually 6-8 cc; acidulatingthe

complete the volume


solution with acetic

previously
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

correction of the lead

should

be

made

for the and

error

due

to

the

volume

(see 83) precipitate


acetic acid.
be

the solutions

should
The

be acidulated

with

analysis of the juice may


*

made

by W.

D. Home's of lead for

method the

using finely powdered dry subacetate


This

clarification.

method
when

as

described

by
in

Home,
sufficient

requires no juice. The quantity


to

measurements

applied in the
lead
is added

analysis of

dry subacetate
a

of

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

required for the clarification of


of the percentage Schmitz's
of
sucrose

100

cc.

of

juice. The table,


be used

calculation
page

is

by Schmitz's
may

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


500. This the
must

method

eliminates

the

error

due

to

the

volume

of

lead

precipitate in other
with caution for

processes

be used

juices or

analysis, but it products contairing


(See 84.)
traces

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

of

damaged
in

may

contain

much. is of great convenience in the storage of dilute them.

Home's control.

dry-lead method
be used does
not

factory

It may samples and


so

juicesin ing compositThe juice usually


of

contains it may be

little levulose

that the influence

tLe lead

upon

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

Joura.

Am.

Chem.

Soc,

26, 186;

Int.

Sugar

Journal, 6, 51.

236

ANALYSIS

OF

THE

JUICE.

Sugars).
be used in

Gravimetric

Methods.

"

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
case.

(1) Method
lion

Using Meissl
"

and

Hiller^s Factors, is recommended

of

the Solvtion, for

^This method

Preparor by the
solution
of

author the

all sugar-cane

products.
as

Prepare
to the

except juice as for polarization


and that

quantity of the
be used.

material Before

the neutral acetate

of lead should

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

of the

flask.

The

filtration should

not

be

ate, immedito

since about full action solution.


more

five minutes' the oxalate. the

standing is
After be

necessary

insure

of

sufficient

time, filter the

Should

filtrate not

perfectly clear, add

kieselguhrand refilter.
solution
may

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;
The add

also

be

kieselguhrto promote
All traces selection of
a

filtration and be removed. for

mix

thoroughly

and

filter.

of lead must

The

glucose

tests is of very tests


were

comparative
factOTies and

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

in the selection of methods refinmes under

in the laboratories and with the

of

the

his control

result

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

agents
care

than

the

carbonate
must

or

sulphate of sodium.
with oxalic acid.

Special
cient Suffi-

to avoid

inversion

be used for the

time and

must

be allowed

of all the lead precipitation

thorough filtration should

follow.

GRAVIMETRIC

METHODS.

237

is the estimation of The next step in the analysis

suitable

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

1, 2y 3,
above

and

cc.

of

the
5

solution
cc.

prepared
heat
to

as

described solution

successively. Add
to the contents
two

of mixed and

Soxhlet's

(!397)
about

of each Allow

tube the

boilingduring
pare Com-

minutes. color which


20

to settle. precipitates

the
note

of the

that

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


supernatant
the volume into For
a

Measure this tube mark

times

of the

deleaded

solution

that

contained
water.

100-cc.

flask and

dilute

it to the

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

with

ascertain

its

weight.
the

It is convenient

to

use

Spencer's

on glucose-pipettes,

making

these measurements in
a

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

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

provided

series of

Cuprous

Oxide.
cc.

"

Measure
copper

50

cc.

of Soxhand add

let's solutioa
25 50
to
cc. cc.

25 (397) i.e., alkali

of the
a

solution and

of the

into solution,
Heat

400-cc.

beaker

of the sugar

solution.

the contents

of the beaker

the

perature boiling-point, taking four minutes to reach this temand continue the heating with very slight ebbulition
two
cc.

during
add
100

minutes.

At

the conclusion

of the

heating-period
and diately imme-

of cold recently hoUed

distilled water

filter and methods


processes

collect the cuprous oxide,using one of the described farther on in connection with the various of the weight ascertaining of the method of copper.

All and that

the

details

of must

preparing the
be

solution

conducting the reduction


the results may

to strictlyadhered be comparable and approach the absolute

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

OF

THE

JUICE.

boiling should
addition
The
FiUration
"

not

be

violent
and the

but

only Juat appuent.


should be

He

of cold water
and invention method of the

filtration
or

prompt.
to

Redvd,Um, of

Caiculaltan

Metailic

Copper.
and

The

the

alimdum
the
as

filtering crucible
at

Spencer'a
instead

of making bottom this

Joint

the Gooch

rim

of the

crucible have

with of

the

crucible, ^
Other
use
.

greatly
of

simplified
of alundum
a

stage

the'analy^s.
are

methoda

filtration than

with
ware.

alundum

given tot

in the absence

(a) Provide

dum Spencer funnel (Fig. 64) or Sargent's aluncnicible-holder (Fig. 65). The
latter is funnel 60"
a

modification
may

of the Spencer

and

be

used

with

any

funnel

of

suitable

size.

With

the Spencer wall of the

funnel

the entire porous crucible be thtvmay


The

oughly washed.
doee not

Sargent
so

holder

permit
of

quite
upper

thorough
of the

washing

the

edge
the

crucible, but, with


are

care, The

results

satisfactory.

funnel

and

Fia.

65.

holder

must the

be of the proper

Mse,

otherwise

the crucible itself filtration.


A the is

will trap brass

washings
funnel

and
may at

prevent
be
a

prompt

Spencer

readily made
cost

by
the

one

of and

Bugar-factory mechanics entjrely satisfactory.


be The

of
walls

few
of

cents, funnel

upper

must

parallel.
These

The

rubber should
be The

rings
funnel

are

carried soft

in stock of

by

the

dealers.

of pure

rubber, and
a

about

i inch

cross-section.

is placed in

suction-filter-

GRAVIMIlTRtC

METHODS.

239

ing device
meyer

such
with
or

as

is shown side

in Fig. 66, The

or

in

heavy

Erien-

flask

tubule.

suction
a

is obtained

by

filter-pump
with the
alundum
account

preferably
ot the

through

pipe

communicating
The
on

vapor-pipe
'

multiple-effect evaporator,
a

enicibles

require

very

efficient

filter-pump
washed

of their alundum

large filtering area.


crucible should be

The hot
DSe.

thoroughly
of
a

with
Ui

water

and

be dried of

in the flame copper


or

lamp

preparatory
should

The

oxides

metallic

copper

be

Fia.

68,

removed

aft"r
with

use

by solution
the

in nitric acid

and

tborou^
of

washing
this

water.

Immediately precipitate
be

after

reduction in the
water.

to

Bubojtide

copper, and is

is collected

alundum The

crucible crucible The

thoroughly only

washed

with
half
on

hot
full the

should oxide subThe


cru-

filled about

during
walls

filtration. of the

distributes

itself

crucible. oxide
in

washing
"

may

be

followed
msy

by moistening
tubstituted sad
for

the

and
most

Alundum

crucibles work
vety

be

platinum
the

of tfa"
These

uidyticHl
lose

ol

the

(sctory
ia

acricultunil
due
to

laborHtoriea. aetion of the

weight

slowly

glucose work,

alkaU.

240

ANALYSIS

OF

THE

JUICE.

cible with crucible in

pure
an

alcohol
oven or

according to the form Proceed by be weighed.


(b) Wedderburn^s
This is the

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

expedite the drying.

of the

methods following
to Metallic

Method

of Reduction

Copper

"

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

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 metal beaker of
or

other beaker

convenient
to
a

metallic

vessel.

Cover

the bottom with

thg

depth of about
will
a serve.

1 centimeter

alcohol.

Denatured with
a

alcohol

Place
warm

the

beaker,covered
the the alcohol

watch-glass,on

hot

plate and

until

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


until the redness the beaker the
to
cover.

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

have it from

been

carried and the

down

with

the flame
remove

let it cool
cover

almost

disappears;
on

from

and The

place the crucible


oxide of copper in the

the

tripod and

replace
and

is almost

reduced instantly
vapor

metallic

copper

atmosphere
of the

of alcoholic

adheres

firmly to the walls


to very

crucible.

The

object of

cooling the crucible


fire to the alcohol.
are

faint redness should


upon

is to prevetat take them removed

setting
ing cover-

If the alcohol

fire the flames after

readily extinguished by blowing


the beaker.
a

The

beaker after

should

be

from It

the is

hot

plate

moment

introducing the
cool for three the

crucible.
or

necessary

to

let the of

crucible

four
to

minutes
avoid
re-

in the

vapor

alcohol, after

reduction

oxidation

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

quite
this be

burned

cooling in a desiccator the crucible is weighed and the weight of copper is ascertained by difference.
The whole
consumes operation as

but
as

five

or

six minutes

and

the

copper

plating is

good

that obtained be
7" 610. 32, 497; 21" 324.

by electrolysis.
with
method,
a

Wedderbum's
"

method
and

may
Chem.

conducted
Original
Votocek
and

Gooch
Vladimir
is.

Journal

Ind.

Eng.

Stanek, Z. Zuckerind.
Chem. Zeit. Chem.

Boehmen,

Laxa, Abatract

Repertorium,

GRAVIMETRIC

METHODS.

241

crucible, but
error

tiie alundum
from
to be

ware

is ash and

more

conTenicnt.
the

An
testa

may

enter
error

occluded
very small

from

jui(", but

ehow

this

usually negligible. The


an.

calculation The

farthra' "tfthe glucoee is ii;iven

Barthel

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

crucibles.

(c) EUdrolytic
.cuprous

Method
an

in

Nilrie crucible

Soiuiwm."
as

Collect

the

oxide in

alundum that be
a

described
must

in Wedderbe

bum's the
very

method, except
crucible need
not

glass funnel
After

used
the

and oxide

tared.
the

washing

thoroughly, change
cc.

receiving-veeselfor
acid fall

the

filtrate.
upon

Iiet 4

of concentrated

nitric

drop by diop

Fia.

67.

the

oxide, being careful that all parts


the acid. Fallow and wash red

of the

latter
hot

are

wetted from
a

by

the a"id
the oxide The
as

with of

jet of
the

water

wash-bottle Should
any

walls

crucible the

thorou(^ly.
acid

of the

remain,
may

repass

filtrate

through
to

the crucible.
copper

oxide

conveniently
method the
100 gauze
*

be reduced

metallic

in the

Wedderbum's oxide. it to
Transfer

and

this
to

be
a

dissolved small the Form


'

instead
and

of

filtrate
re. as

beaker

dilute

approximately platinum platinum-gauze

Deporit
follows:
in diamA

copper
a

electrolytically upon
of

cylinder

52-meah
gauie

1 inch

Coarse

coppnr-wiie

nould

probably
be

aetvt

as

tathode.

Tbs

cDnnectioQ

with

the

copper

must

platinuRi

wire.

242

ANALYSIS

OF

THE

JUICE.

submerged in the by 1.5 inch long. Connect the cylinder 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 be

current

of 10 amperes

and

4 volts.

The

copper

should

completely depositedupon
Rotation its of the

minutes.^ increases
copper

cylinder within 10 to 15 anode during the reduction


the solution

rapidity. The
time
to time to

should

be

tested

for

from
a

It to
to

little anmionia

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
off the electric current, withdraw the

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

acid solution

with

time replacing it with water. large pipette, at the same Repeat this operation until all the acid has been removed, then break and the current, then The of acid in
remove

and

dip the cylinder in


it in
an oven

pure

alcohol minutes.
a

ether, and
must not

dry
be

for
so

few

current

discontinued
now

trace

remains.

The

cylinder is

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.

long as weighed, its deposited.

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 with and the 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
.
" ---

|"

TIT

ri)---

"-

,!,_

"

J. Ind.

and

Eng.

Chem.,

2, 195,

R.

C.

Benner.

..

244

ANALYSIS

or

THE

JUICE.

platinum dish, the


cylinder.
A the Soxhlet Gooch filter

copper

berrigdeposited upon
may

platinum
instead of

tube, Fig. 69,


This
one

be
of

used
a

crucible.

filter consists end of which

tube
a

of hard tubule

glass,6 inches long, into


3

is sealed

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 inches
to

support

an

asbestos-felt filter. filter-tube for


use

Prepare
manner as

the
a

in

the

same a

Gooch

filter and

weigh

it.

Place

small oxide

fimnel
from

in the filter-tube to prevent the cuprous

adhering
the filter

to

its

walls,and

moisten

the

asbestos-felt with
onto

water.
as

Wash described

all of the in (a).

tate precipi-

-A

Dry th^ then of pure current a dry hyprecipitate, drogen pass time the through it, at gently heating same
the
cuprous

oxide
all

with the the

the oxide

fiame

of

Bunsen
to

burner, until
metaUic
state.

of Cool

is reduced in
a

the of

copper

current

hydrogen
reduced
Fio. 6d.

and
may

weight of copper also be determined volmnetricallyby


text-book"
is

weigh it.

The

the methods Methods Wedderburn


in which

of the various
the

Copper
more

Oxide

Weighed.
copper

"

^The the

method

of reduction
are as an

to metallic accurate

and

methods electrolytic involving the weight

than these

the

methods

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 crucibles may
a as

oxide.

Of

latter

accurate

as

the Wedderburn that either

or

trolytic elecor

It

is obvious

alundup

be used. crucible
to

(a) Prepare

Gooch

receive

the

precipitate weigh

by forming
and the felt in

a an

very
oven

thick asbestos
or on
a

felt in it. iron

Dry the crucible


the reduction

hot

plate; cool and


after

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.

GRAVIMETRIC

METHOD.

245

filter.
nor

Care

must

be observed

that
pass

neither into the

suboxide

particlesof asbestos
with* the
a

of per copfiltrate. Follow


a

the of

wash-water ether. Place

Uttle crucible

alcohol,then
in
a
a

with

few

water-oven

and and the

drops dry it

thirty minutes, then The weight of the


copper

cool

it in

desiccator
=

cuprous

oxide X. 888

weigh it. weight of


a

reduced. the
cuprous

(b) Collect
crucible redness Bunsen minutes.
as

oxide

in

an

alundum the

or

Gooch
to

and in
a

thoroughly dry it.


muffle furnace
or

Heat

oxide

full

in the

burner. Cool

Continue

the
a

oxidizing flame of a fifteen heating for about


and then

the crucible in

desiccator

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.
=

CalculcUion Hitter's Method, Let Cu


"

of
"

the

Percentage of Glucose

hy Meissl

and

the

P=the

weight of copper obtained; polarizationof the sample; weight of the


used factor obtained of copper

IT

the

sample in the
from
to

50

cc.

of the

solution F
"

for the

determination;
the table
for

ihe

the

version con-

invert-sugar;
weight of invert-sugar Z;
=

"=

approximate absolute

ZYrz^
lOOP
"-

approximate

per

cent

of

invert-sugar
=

j/;

ii, relative

"

,.

number

for sucrose;

100"12=/,
CuF
=

relative number of invert

for

invert-sugar;

per

cent

sugar.

W Z facilitates
to

readingthe vertical columns; and the ratio of


of the for the table, of copper
purpose to

/, the horizontal columns


Example. The it (W)

ing of find-

the factor (F) for the calculation

invert-sugar.
3.256

grams

of

of a sugar polarization are equivalentto 0.290

is 86.4, and
gram

of copper.

246
"*-.%

ANALYSIS

OF

THE

JUICE.

Then:

lOOP

8640

P+y

86.4+4.45

"95.1*/2;

100-i2"100-95.1=/"=4.9: i?:/"95.1:4.9.

By
column column Where
enters

consultingthe
headed headed these
150 95
:

table

it will be
to

seen

that

the

vertical

is nearest 5 is nearest
meet

Z, 145, and
find the

the
to

horizontal

to the ratio of R
we

/, 95.1
51.2

4.9.

columns GnaX

factor

which

into the CuF


-^liT"
=

calculations:

.290X51.2
" "

=4.56

_.

o.^oo

rtgg

per

cent ^

^ of mvert-sugar.

..

MEISSL

AND OF

KILLER'S
MORE

"

FACTORS
1 PER

FOR

THE
OF

TION DETERMINA-

THAN

CENT

INVERT-SUGAR.

1889, Zeitschrift,
"

p.

735.
may

show that this method Experiments in the determination good degree of accuracy of glucose in cane juices. (G. L. S.) Note.

of

be used leas than 1

with
per cent

DETERMINATION

OF

REDUCING-SUGARS.
"

247

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;
"

(2) Gravimetric

boil

five minutes.

In the

boiling always reduction,


cc.

use

the

naked flask

flame. from Filter

Having
the

completed
and

remove

the

flame

add

100

cold

distilled

water.

immediately through a Gooch in the precipitate by copper


collect the
on

the crucible,and determine the electrolytic method, or filter-tube and reduce it


as

cuprous page

oxide 244.

in 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
can

described

be

determined

to

within

.01 per

cent

with and

certainty.
Glucose.
"

(3) Gravimetric
Determine
the

Determinaiion

of Sucrose

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
119.

Determination Volumetric

of Methods.

Beducing-sugars
"

(Glu^
methods of

cose).

^Volumetric

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 conand method of heating, of dilution, containing-vessel

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
"

with

oxalate
to 100

of
cc.

potassium

in small

excess

and

dilute

the

precipitate. calculations are simplified The by the use 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 burettereading of approximately
described.
The
measurements
.

solution

Filter off the

20

in

the

titration

about

to

be

of

the

standard

solutions

for

this

Trait6

d'analyse

des

Mati^res

Sucr^ea,

D.

Sidersky,

148.

248

ANALYSIS

OF

THE

JUICE.

process Such The


a

are

mort

conveniently

made

with

automatic ia shown
in

burettes.

burette, designed
is filled shown

by Squibb,
end of the

Fig.

70.

burette

by suction
at

applied at the
rubber
burette

mouth-piece
tube.
to
a

the

The

reagent
a

is drawn the

into the

point

little above is

zero-mark
excess

and the of
the

mouth-piece
solution

released.
back

The

syphons

into the reservoir, leaving

the burette

filled to the zero-maric.

JIL Jl

The solution

test

is made into

as
a

follows:

Measure

10

cc.

of

Violette'a

(296)

large test-tube,
dilute it with

1.5 inches 10
ec.

in diameter

by

9 inches

long,

and

of water.

Heat

DETERMINATION

OP

REDUCING-SUGARS.

249

solution

to
a

the few

over boiling-point

the

naked

flame

of

prepared juice, and boil two minutes. Repeat these operations until the blue color almost disappears, taking care to add the juice
little

lamp,

add

cubic

centimeters

of the

by
or

littleas
two

drop
the the

at

point is approached and then only a time until the blue color disappears. After
two

this

first

boilingof
for

minutes, it is only necessary


A the
a

to

boil

liquid a few seconds, after each addition.

sand-glass
the

is convenient

timing
or

first

boiling.
the

When

color
for

just disappears, filter off


copper,

portion of

liquid to

test
or

using

Wiley

Knorr-Wiley
a,
are

filter-tube

other

convenient

filter. made
ten

Wiley's filter-tubes. Fig. 71,


.

from

pieces of
One then A and

glass tubing one-fourth


end of the tube

inch

bore

by
to

inches of
a a

is softened
a

in the flame wood

long. lamp and


shoulder. this end is

pressed against
piece of
tied into and the in
water

block linen

of is

form
over

washed In

stretched the

place.
in

using
is

this tube

filter end

dipped
film

whijch

suspended
the linen

finelydivided
with

asbestos,
a

by mouth-suction
asbestos. small In diameter

is covered

of

Knorr's and

modification
a

of this filterthe tube

perforatedplatinum disk takes indicated in Fig. the place of the linen, as 71,b. In usingthese the solution is filtered through the asbestos film by tubes mouth-suction and with the Wiley filter is poured from the
is of tube into the
test

solution. off the

With
end

the

Knorr

filter the the be be

asbestos

must

liquid then

wiped expelled by
dilute with

be

of the The

tube, and
should and then

blowing.
nitric acid

tubes

dipped into very thoroughly washed


chemists Many and place it on
a

after use,

water.

a drop of the solution prefer to remove The piece of end-reaction filter-paper.

precipitateremains
with In
must
a

in

the

center

of

the

moistened

spot,
it

the filtered solution around whatever be tested


cent way

it.

the

filtered

solution

is obtained

10-per

This filtrate is acidulated with for copper. solution of acetic acid and then a drop of a

very

dilute solution

of

ferrocyanideof potassium, 20

grams

of the

tion colorato it; a brown salt per liter of water, is added indicates the presence of copper, and if this color appears.

250

ANALYSIS

OF

THE

JUICE.

more

of the

sugar

solution be used.

the color test carefiilly as when all of the copper is reduced finally very further coloration. The

juicemust be added decreases in intensity until


The there will be
no

followed, after
the

be readily progress of the test may little practice, of by noting the appearance

and the color of the supernatant liquid. precipitate The test should be repeated, adding nearly enough now
sugar

of the then
at

solution
as

at

once

to

reduce

all of the

proceed
end

before.

The

should burette-reading calculation

copjjer; be made
as

the

of the

operation. The
1
cc.

is made

follows: Let TF="the B^ihe


X

weight of juicein
burette

of the solution;

reading; "-the required per cent;


0.05X100
x^

then

^^^
W
=

When
or a;

is .05 gram

the

formula

reduces

to

rc"=

"

"

"

the

of the burette-reading reciprocal by multiplied of

100.

A these If
a

table

reciprocalsis given

on

page

484

for

use

in

calculations.

multipleof 5 grams of juiceis diluted to 100 cc. for of the burette-readingmultiplied this test, the reciprocal 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 of the sucrose the principle pipette (115) may be used on the juice and obviate the necessityof dividing to measure gravityor weighing the sample. by the specific
Violette's This
copper may

solution

be avoided the other

on standing. decomposes somewhat of the one by preparingtwo solutions,

and

of the alkali.
are

In and

making
the
10

test 10 cc.

of each
are

of these

solutions

used

cc.

of water

omitted.

(2) Soxhlet^s

volumetric
a

method.

"

Prepare the
as

analysis and

make

test preliminary

juice for described in (1), to

252

ANALYSIS

OF

THE

JUICE.

in

100

CO.

water,

add
to
cc.

sufficient 200 of
a

subaoetate

of

lead
To

*"

for
cc.

dilute clarifiQation, of the filtrate add of sodium;


to

cc,

mix, and

filter.

lOO

25

concentrated

solution of carbonate
100
sponding cc., corre-

of this filtrate take mix, and filter;


10

Boil 100
in
an

cc.

of the material, for the reduction. grams Soldaini solution five minutes fiame over a naked

little by Erlenmeyer flask,then add the sugar solution, additional five jninutes. little,continuing the heating an Remove
the

flask,add
an

100

cc.

cold distilled water,


a

collect the

precipitateon
under pressure.
are

asbestos Wash
no

felt in

Gooch

crucible, filtering
water

the

with hot precipitate Three


or

until the

wash-waters
are

longer alkaline.
Add
to

four

washings
25
cc.

usuallv

sufficient.

the

cuprous

oxide

normal

the standardized two acid, and sulphuric acid, i.e., heat -three crystals of chlorate of potassium, and gently or oxide is completely in soluti"Hi. This until the cuprous

operation should
the solution with
the

be
a

conducted standard

in

beaker

or

flask.

Titrate

alkali solution, and acid used reduced. of ammonia


as

determine
from

by difference
volume
use
a

volume

of the

up,

and

this

the

amount

of copper solution
copper
as

It is for

preferable to
titration,

half-normal

this

the sulphate of letting


the

act
:

the

indicator.
cc.

Prepare strength
added

ammonia

solution with 800

fallows
of

Mix

200

of commercial
the

ammonia

cc.

water. cc,

Determine
to which copper

of this solution
2
cc.

by

25 titrating

has

been

of

concentrated

sulphate of
sufficient normal.

solution, against
until the the blue
to

the

normal

sulphuric acid, adding the


water

acid

color

disappears. Add
to

ammonia

solution In

make the

it one-half titration

proceed as follows: Oool the of the copper-sulphate solution resultingfrom the treatment oxide with sulphuric acid and chlorate of potassium ; cuprous making
add
50
cc.

half-normal

ammonia The blue

solution. color
on

Titrate

with

the
each

normal addition
as

sulphuric acid.
of the
as

disappears with
the stirring is not

acid, but

reappears

solution

long

there

When

all the

which ammonia is any is saturated, the ammonia

saturated.

color of the

liquid

The

lead

should

be

removed acatic acid

by precipitation with (G. L. S.).

potassium

oxalate

after

acidulation

with

DETERMINATION

OF

REDUCING-SUGARS.

253

is

no

longer blue but


is cubic centimeter

faint green.
to

Note
copper

the

burette-

reading, which
Cach

equivalent
of

the

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.
120.

the

General

Remarks

on
"

the

Determination

of

Olucose
and
sugar

Geerligs, Pellet,Edson that a part of the reducingother chemists have shown is carried down with the lead precipitatewhen subof lead is used

(Beducing^sugars).

The writer, the solutions. clarifying used acetic acid to acting on the suggestion of C. H. Gill,^ and Pellet decompose the lead levulosate in optical work
acetate

in

and

Edson
tests

afterward and also


of

advised

the

use

of acetic acid in

cose glu-

normal and AH

acetate

expressed a preference for the use of the lead in preparing solutions for both glucose
be removed reduction.
from

sucrose

tests.

traces

of lead must

the solution before

proceeding with
have been used

the

Several

deleading agents

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 adopted oxalate of potassium or sodium provisionally * that states dry oxalic acid in deleading. Bomtrager sodium The bonate carsulphate is preferable to the carbonate. is Very generally used in deleading and of sodium
very

with

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 kieselguhr in conjunction with the oxalic acid or filtration. The to promote experiments mentioned
that the its salts showed
of
pletion com-

careful

deleading agent
to

may

be added
on

in advance

of the volume

the mark small.


must

the

provided the flask,


not

percentages of glucose are


be immediate. of the

The be

filtration should allowed for the

Ample

time

action

deleading agent.
Soc, April. 1871.
,

" 3

J. of the Zdt

Chem.

a^-gew.

Cham

1892, 333.

254

'

ANALYSIS

OP

THE

JUICE.

121. Normal

Determination
Ash.
"

of
grams

the
of

Ash.

"

Carixmaled

Ask

or

Dry

10

platinum dish, then


temperature, and

incinerate
at
a

juice in a shallow the residue, first at


dull-red heat. The

teured
a

low

afterward

wei^t
rise

of ash X 10 =per ash. cent of normal In this determination the temperature above
a

should

never

low-red which cooled

heat.

carbonates should
as

be

largelyof alkaline quickly absorb moisture from the air, it in a desiccator and be weighed as quickly
As be

the

ash consists

possible.
This

incineration- may

accomplished

over

the flame

of

electric or An lamp, but it is preferable to use a muffle. tory. gasolene muffle furnace should be used in the factory laboraa

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
as

The

carbonated

ash is

follows:

The

material

is heated bum

in

large
It After

platinum dish until it takes fire and


swells the
to
a

the flames

out.

greatly and
has

is difiicult to confine to the been and


an

dish.

material

sufficiently charred, it is transferred


is rubbed
to
a

glassmortar
upon

powder.

The is

is washed extracted

ashless
water.

paper

fflter and

powder thoroughly
for further

with

hot The

The

filtrate is reserved insoluble matter


are

treatment. to the

filter and
are

returned

platinum dish and evaporated


contents to
are

is

now

The ffltrate completely ashed. dr3rnessin the platinxmi dish and the heated
to low

dish and
any

then

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
"

sulphuric acid carefullyover


carbonized
mass

to

moisten
a

the

residue acid

and

heat

it the

the

flame
porous

of and

lamp.
converts

The the

renders

carbonates

into

sulphates.
When
a

the charred heated


may to

mass

ceases

to

transfer the dish swell,


off the the carbon. for carbonated

to

muffle

redness

and

bum

The

temperature
but
care

be

higher than
not

ash,

must

be

observed

to fuse

the ash.

DETERMINATION

OP

THE

TOTAL

NITROGEN.

256

^^^^e ash
\'"in The in be

should

be in

moLstened
the muffle in the

with
to

sulphuric acid

and

reheated

sulphides are
the

formed

decompose sulphides. reduction of the sulphates


the
centage, per-

in heating In

the presence
ash

of carbon.

customary
to

"sulphated-ash" method, one*tenth


is deducted for the

weight

of the

before

the calculating of

compensate
is

formation

stead sulphates inusage.

of carbonates.
true

This
very

follows beet sugar


number and factor should

The

correction

variable

often

imates approx-

25 per cent. for each

A correction

be determined

factory and each material.


"

(See 136.)
is shown
A
narrow

^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
a, at

drilled in the walls ", holes are heavy platinum c, df Fig. 73, and
are

wires

inserted. for
a

These

wires

form
Fig.
72.

supports
the dishes A
.

trough of platinumX, y, z, upon

foil.Fig. 72,
rest

Wj

which

during the
is
at cut

tion. incineradome The


Fig. 73.

hcde muffle

in the

of

the

i, Fig, 74.
a

muffle

is and

placed
is

upon

suitable support

heated

by

wing

top

burners.
123.

Determination
and
"

of the

Total

Nitrogen
"

the

Albuminoids.

Total

method
as

termined Nitrogen. ^The nitrogen is decombustion by the moist tions, modificaof Kjeldahl with

Fig.

74.

adopted by the association


digestion. 10
"

of Official

Agricultural
in
a

Chemists.^

(1) Th3

cc. a

of the
550-cc.

juice,dried
oxide
on a

small

capsule, xure brought approximately .7 gram


sulphuric acid.
The

into of flask

with digestion-flask and frame


20
cc. an

mercuric
is

of clined inthe

placed

in

and position,
"

heated
Soc.

below
151.

the

of boiling-point
' "

'

Journ.

Am.

Cbetn.

16,

'Adapted

from

Bulletin

46, Div.

Cfaem.

U. S. Dept.

Agrto.

256

ANALYSIS

OF

THE

JUICE.

acid

for from

5 to

15

minutes,

or

until

frothinghas cea.^
raised is until the

If the mixture
be

froths

badly,
The

small heat

piece of paraffinemay required till clear liquid,which

added

to

prevent it.

is then

acid the is

boils
contents

briskly. No
of the has

further

attention
a

flask have

become

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
or coloriess,

only

very the

"

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

to the

Next from

add

50

cc. or

of

saturated

caustic-soda make the

solution,free strongly
it does flask the the
so

nitrates,
mix the
at

sufflcient to

reaction

alkaline, pouring it down


not
once

the side of the flask acid solution. be

that

with

the

Connect

with

condenser, which

should

of block

tin, mix
has

contents
over

by shaking, and

distil until all ammonia The first 150 ammonia.


to
one cc.

passed

into the standard

acid.

of the distillate This

generally contain U3ually requires from


will Tive distillate is then the calculations
are

all of the
40

operation
a

minutes with

hour

and

half. and the

titrated made
as

standard

ammonia,
to

usual.
a

Previous

use,

reagents should
which which
will

be tested

by

blank

experiment with
that
are

sugar, present

partially reduce
otherwise
"

ary

nitrates

might

escape

notice. mined nitrogen is deterof Stutzer,and the percentage

Albuminoid

nitrogen, ^The albuminoid

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

La.
6

Expt.
instead

Sta. Bui. of 6.25


6
on

38, 2d
as a

Series,
of the

p.

1375,

advises
many

the

factor He
bases

is customary

by

plantof

analysts.
albumin"Hd

this factor

study

composition

the

matter

of cane-iuioe.

ACIDITY

OF

THK

JUICE.

257

liquid is alkaline; filter;rub the precipitateup with water and wash by decantacontaining 5 cc. of glycerolper liter, filtration 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
mass

that

can

be of

measured

out

with
per

pipette. Determine
centimeter of this

the

quantity
Place

cupric hydrate
of the

cubic

mixture. 10 grams

juicein
a

bes^er, add

100

cc.

of water*

heat

add boiling;' containing about 0.5


to

quantity of cupric hydrate mixture of the hydrate; stir thoroughly, gram


with the cold water,

filter when the


to

cold, wash

and, without

removing,

from precipitate the method

determine filter,

nitrogen according

of total nitrogen, given for the determination adding sufficient potassium sulphid solution to completely The filter-papers used precipitateall copper and mercury.
must

be

free practically is rich of


a
in

from

nitrogen.
solution

If the
a

substance
few cubic

examined
centimeters

alkaline

phosphates, add
of alum
mix

concentrated and

just before

adding
serves

the
to

cupric hydrate,
decompose
the

alkaline
free

not

done, cupric phosphate and


the

by stirring.This phosphates. If this be alkali may be formed,

well

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
"

a on

normal
page

alkali solution, preferably caustic


417.

soda, is given
the

The

decinormal
cc.

solution

is

prepared from
cc.

normal
It

by diluting 100
is very litmus be difficult to
paper
a as an

of the latter to 1000


when

note

is neutrality If litmus
paper.
as an

reached

in

using
it of

indicator.

paper

is used

should

very

sensitive neutral
may

few

drops
The

logwood
excess

solution
a

be
or a

used violet

indicator.

logwood
of
an

assumes

purple
as

color in the the

presence

of the
to

alkali.

In

making

titration
20
cc.

it is

cDnvenient

proceed

follows:

Measure

juice

In

the

case

of sorghum-cane

5"*W,

heat

on

water-bath

10 minutes.

258

ANALYSIS

OF

THE

JUICE.

into

beaker

or

porcelain
to

dish Measure

and

add into little

lew

drops
the with
test

of

logwood

solution normal

it.

this

juice little,

one-tenth
constant

caustic-soda
As from

solution,
liquid
to

by

stirring.
drops
of it

the time

approaches
time
in
a

neutrality,
separate
at

few

dish,

with

logwood

solution. and in record


terms

Multiply
the of
test

the

burette-reading
as

neutrality
100
cc.

by
juice

product

the

acidity

per

of

decinormal is
not

alkali.

The

above

required
the
defecation.

except

in

special

tigations, inves-

or

in

control
of is If made the few

of

124.

Analysis

Clarified

Juice.
"

The

analysis
as

of
of

the normal is

clarified

juice

by

the

same

methods is
must

that

the

juice.
case

carbonation

process

used,
receive
the first all

which

the

in

very

factories,
carbonic

the

juice acid,

an

additional

treatment and before

with the

after

car-

bonation, limeitcontainQi

analysis,

to

precipitate

of

the

260

SIRUP,

MASSECUITES,

AND

MOLASSES.

the

non-sucrose,

are

of the

same so

specific gravity
far
as

as

cane-

sugar.

This

is

true practically

bodies, but is not


associated These with with the sugars salts the in Since with
a

hydrate regards the carbofor the inorganic salts which are in the massecuites and molasses.

having such high cpecificgravity, as carbohydrates, infhience the density marked degree. very
ratio of
non-sucrose

compared
tions determina-

the

to

the
as

sucrose

increases
sugar

each

stage of the manufacture,


the

commercial

is

removed,

difference

between the

the

apparent

percentage

of total solids,as

percentage,
becomes

as

the true by ascei*tained by actuallydrying the material,

indicated

hydrometer, and

larger.
from these remarks total that calculations massecuites of the and
Brix
or

It is evident

degree
with

apparent
the

solid9 in

molasses, from
caution similar There

and

density of the product, must be accepted then only for comparative purposes when
of

conditions is another

analysis are
that
a

maintained. has
not

condition

yet
that
at

been

tioned. men-

The

density (Brix) of
one

solution calculated from


from

spindling
from the

at

dilution

is different

calculated
tion. dilube

hydrometer Thus, for example, if

number

ascertained
one

another

part of
and

final molasses

dissolved in two
the be Brix

parts of
it would
one

water

this solution be this

spindled,
been

of the molasses than in

calculated from
be had
one

spindlingwill

higher
to

part of the-molasses
This

dissolved due with

only
and

part of water.
of the
to
a

difference is partly
on

the

contraction

solution of sugar
contraction This

dilution
tion solube

water

partly though

similar

of the

of the

salts in the

molasses.
one were

difference would

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
even

final molasses
indicated The

may

be from

5 to

10

per

cent

below the

bers num-

by

dilution and of dilution

spindling.
and

methods
are

spindling,given in this

customarily used, and the results must not be considered absolute,but only as suitable for comparisons.
book,
those

SPECIFIC

GRAVITY.

SIDERSKY's

METHOD.

261

127. This

Specific Gravity.
is

Sidersky's

Method.

i"

boiled applicable to samples of massecuites blank and to molasses, but not to grained strikes. The suitable a required is a 50-cc. sugar-flask, apparatus method and
a

heating arrangement,
stopper.
into the Grind
one

funnel

with

glassrod
funnel it in
a

for

end

of the
a

glassrod with moistened


Fill the
set

funnel, to form
of the massecuite

stopper.
or

emery with a

sample
The When

molasses, and
to

iron support, and heat

with the flame of carefully distribute

cylindrical lamp.
heat.

object of the
the material

iron is

cylinderis
and

the

quite warm, into the flask, lift the glass rod


2
as or

lower the stem fillthe

of the funnel

latter to within
very

3
not

cc.

of the mark.
smear
a

Remove

to

the neck few

carefullyso of the flask with molasses. Keep


to

the funnel

the

sample hot
cool

minutes
room

facilitate the

escape

of the

air, then
then and mark.

It to the

temperature
of
on

by immersing the
contents,
17
to

flask in cold reduce


run

water. the

Dry
the

and

weigh the flask and


the material of the

temperature
flask
are

J" C,
to

water The

into

top

molasses,

the
:

calculations

shown

in the

example following

Weight
''

of flask and
'' ''

molasses

91 .570 25.276 66
.

grams
*'

empty

it

' '

the molasses and


water.

295

grams
grams

Weight
''

of flask,molasses
''
''

94.672
91.570

and

molasses in cc.)

ti

(I

water

(also its vo'mne

3.102

grams;

and

50-3.102
"

46.898

By means corresponding
It is very
on

molasses; 66.295-51.4136, the required specific gravity at 17i" C. find the degree Brix of the table, page 482, we
to

=46.898, the volume

of the

this

specific gravity to
make
a

be
test

79.6".

difficult to of the for

correct

account

air-bubbles.
the

by this method the only It is, however,


of

direct

method

specific gravity

massecuites

and

heavy molasses

that is used.
iZeitschrift, 1881,
p.

192.

262

SlBTJFj

UASSECUTTEB

AND

MOLAB6BB.

128.

Weight

of

Unit

Volume

of

Massecnlte." ia the
of
a

modification

of Sidersky's methoii
may

desuribed
the

previous
certain

paragraph
volume
of
course,

be used

to ascertain

weight
foot

of massecuite.

The

selectbn
the

of the unit volume


cubic
or

will,
or

depend
for

upon

whether

gallon partly
The

device

making

this measurement conHista of


a

is shown

in of

section
any

in Fig, 7S.
mze

This

cylindrical veasel
of metal.
be

convenient

and

preferably cylinders metal, CC,


from supports
and

rim
a

of the

should

ground
be
to

true,

strip
which

of

should
ade
a

provided,
of the drawn

extends

side

cylinder
to
'

glaas tube
in

capillary, as
m

shown

TT'.

Pins

PP' in

the

rim

of the

cylinder and
in the the latter

fitting
strip
of

corresponding
insure
same

holes

metal
in
to

replacing
position.
the

always
cylinder
masee-

the

Fill the
lo

approximately
in

point

with
in

cuite, place the


then
run

capillary-tube
from tube
a

position,
very The tube

water

burette

cautiously
instant
rises This
FiQ. 76.
some

until

the

is reached.

the

water

reaches

the

it

distance

into
be

it

by capillarity.
and is
more

may

readily
if colored

noted

plainly
of the
and the

water

used.

A
to

previous determination
the bottom

of the
should

volume
be made

of

the

cylinder
water.

tube

with
to

With
the

this volume
volume

that

of the

water

required
of the

cMnplete
is

with

massecuite,
may be

that

massecuite the

readily
of the

ascertained
material. In

and

compared

with

weight

making this
at

test

the maasecuite

should
of this for

be of the temperature

which the

the

measurements

product
the

are

to

be
of

made

in

factory,
be

and

correction

expansion
Uaed

the It

cylinder should
is

applied.
this method
cannot

evident

that

be

\"iiere

are vibrations of machinery Degree 139. Apparent

felt, Brix. DetermlnatloB


a

by
of

Dllntton

and

SpllndUDg.^Di3solve

weighed

quantity

DILUTION

AND

SPLINDLING.

263

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
an error as

material in

described
number

on

page to

222,

and the

by
true

ascertain

multiply the degree Brix of


and of solids is number

rected cor-

the

material. method.

This The

is the

customary
or

commercial

Brix than

percentage
the

several degrees lower

apparent

factory usually ling. by spind-

130.

The
on are

Brix Solids by Befractometer. or Apparent has been described method of using the refractometer
"

page

225.

When

dilution

and

clarification of the

unnecessary

this method

gives results that

sample closely approximate

those If the material

by drying.
contains the be crystals of sugar these must refractometer only indicates the solid When solution is
on

since dissolved,
matter

that

is in

solution.
as

employed
in this
error

the

calculation

is made

is indicated involve

farther the

paragraph.

Dilution

methods

contraction
may

of similar methods

by spindling. The
very to

error

be reduced If
a

by working with
of water be added

concentrated
a

sr

lutions.

volume

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
molasses definite conditions be observed that the results
may

be

comparable.
In the event

of

the method a highly colored material, testing


may
a

of Tischtschenko

be

used.

Mix

the
sucrose as

material of known is

with

an

equal weight
and determine the

of of

solution

of pure

position com-

as

high

concentration

practicableand
the
on

refractive

index.

Ascertain

percentage
page

of solids in the mixture The

by

means

of the table material

492.

percentage of solids in the

is ascertained

by

solution from deducting the per cent of solids in the sucrose The principle of the method twice the solids in the mixture. of calculation for other mixtures is the
same as

that

of the

dilution formulae If necessary


to
as

(307).
dilute the follows: material with

lation water, the calcu-

is made

264

SIRUP,

MASSECUITES

AND

MOLASSES.

Let

the required percentage of solids

(Brix);

TF==
t^;'^

weight of the material

used; weight of the diluted solution;

then
Wx^bw
131.

and

x^bw/W,
or

True of Carr

Brlx and

Total

Solids
and the

by
vacuum

Drying."
method In the

The

method
are

Sanborn for this of the

(IIS)
latter methods

recommended
use

determination. material. In
a

method after

gram

both small

weighing the material, dissolve it in


in order
to

quantity
over

of distilled water

distribute

it evenly

the

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 cent

of

Dry the sample and


112, and
to note

calculate

the percentage,
same

as

directed

in

the remarks

in the

paragraph in regard
The method

the
132.

decomposition of levulose.
Determination the of the of

Sucrose."
sucrose

of

determining
or

percentage

in

sample
of

of the'

molasses

majssecuite

depends upon
of the of

the

purpose

analysis.
For of the the

ordinary purposes
processes

factory, for the control

various and is not

manufacture,
the

especiallythe

vacuum-pan
of
sucrose

work, crystallizer

required.
per cent

The
sucrose

percentage relation,however, between


and the

absolute

the the

apparent

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
conditions similar of

coeflficient of

analysis

and

adhere the

to

them will not

with be

all
parable. com-

materials, otherwise
the of

results

For

purposes

produced in the various


the total loss of sucrose, conrniercial
to

comparing the commercial sugar of the and periods crop determining


essential that
the

molasses avoid
error

it is very samples be and


to

final

or

analyzed,using every
obtain absolute

caution preas

results

DETERMINATION
.

OP

THE

SUCROSE.

265

nearly
the
"

as

the

above

processes of analysis will permit. considerations for what methods may and modifications of the

In

view

of

be termed

will

factory tests" be given:


Determination
or

Clerget process
"

of
15"

sucrosCf

factory tests.
and is dilute

Dissolve the solution

the
to

massecuite

molasses

approximately
after
a

Brix.

little

of

the

solution

and

usually quickly the degree Brix experience. proceed as in 115, using the sucroseplished accom-

in water This

Ascertain

pipette.
Home's it is

dry-lead method

may

be

used

in these method of

tests, but
on

to modify the usually advisable of the high levulose account content

shghtly
to

massecuites

and

molasses. 15** and

Dilute 16"

the

massecuite

or

molasses

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 shakThe clarification is most
may

glass cylinder which while shaking. hand


a

conveniently effected in a small be covered by the palm of the


to 50
cc.

Filter and

of the

in filtrate, make

50-55
to 55

cc'
cc.

add fiask, ^ith


water.

dilute acetic acid to Polarize

acidityand
in
to
a

up

this solution

200-mm.

tube for under

and the

increase dilution.

the

reading by one-tenth
to

compensate

Refer

Home's

the

polariscope reading and

table, page 494, and opposite the degree Brix


of

find the coefficient of


It is convenient

purityof
a

the solution.

to have 100-cc.

number

cylindersmarked

at

approximately the
as

follows:

point and to modify the method Fill the cylinder to the mark with the diluted
molasses; add
of the
a

massecuite lead from


mix
measure a

or

"struck"
spoon

measure a measure

of the

dry

conical

measuring

and

of

sand;

the contents

guhr.
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
of all the lead.

Shake, filter and


526. The

polarize. Find
table should
at

purity by Home's
to
cover
a

table,page
wider
range

be

extended
most

of densities

the

places
in

used.
coefficient of
tests.

The these

purity is all that is usually required


be noted that
on

It should

account

of the

large

266

SIRUP,

MASSECUITES

AND

MOLASSES.

dilution of the material otherwise


133.

i!ie coefficient is lower

than

it would

be.

Clerget's
the

Method

for

Sucrose.

"

This

is often

"double-polarisation tions method," since two polarizain made, one before and the other after inversion, are order to eliminate the influence of the invert-sugarthat may be present. Cane-sugar products usually contain the three
termed
sugars, rect (+), dextrose (+) and levulose (" ). The dipolarization is therefore the resultant of the polarizations
sucrose

of these three sugars.

original Clerget method, 50 cc. of the sugar solution inverted by the addition of 5 cc. of concentrated chloric hydroare acid in a 50-55-cc. with heating to 68" C. during flask, fifteen minutes, followed by rapid cooling. This method quires rethe use of Clerget^sconstant, 144. The calculations
In the
are

made

as

in the

following modifications
in the work.
to
or

of the

method.
are

The

modifications

described

following pages
risk of
error

those have

usually used in
been

cane-sugar
a

All the modifications

devised with

view

reducingthe
to

through

decompositionof levulose
134.

Clerget's
Modification.

Method.
"

simplifythe work.^ man) Herzf eld's (Official Gerinstructions

The

given here
meet

are

modified

from slightly

those Dissolve

of Herzfeld
65.12

to

cane-sugar

factory conditions:
or

grams 500-cc.

of

massecuite

molasises in water, contained


grams

in

(Mohr) flask, or
of lead
cc.

65

if

true

cc.

flask is used.
to the

Add

subacetate

for

dilute clarification,

mark, mix and filter. To 50


50-55
cc.

of the filtrate contained


to

in

a cc.

flask add

acetic acid

acidityand dilute
temperature, and
tube
55 cc,

to 55

Polarize this solution, noting

the
mm.

reduce

the. reading

to

terms for

of

200-

and

normal

solution.

Correct

the

dilution

increasingthe reading by 1/10. Enter this number ."Ni the direct polarization. Delead filtrate by the addition of a portion of the original It is not necessary that all the lead be dry sodium oxalate.^
to

removed
1

in

but deleading,
the the
use

the
of dry

quantity left should be


oxalic

very
agent this is

Cross

recommends
for

acid

as

deleading
If the

in

preparing
in
excess

both
of the

direct

and

invert
to

polarisations.

uoed

quantity
Lt

required ^xpt.
Sta.

precipitate

lead, the

filtration

may

be

difficult.

Bui.

135, p. 29.

268

SIRUP,

MASSECUITES

AND

MOLASSES.

duoe.

Prof.

Herzfeld
York

requested

the

International

mittee Com-

Congress Meeting of the International of Applied Chemistry) to revise his table of constants, as several investigatorshave reported apparently high results
(New
in its
use.

Steuerwald

has shown

that

Herzfeld's

constants

these numbers give high results and has redetermined table: published them in the following convenient
STEUERWALD'S
TABLE Inversion OF CONSTANTS.

and

(Hersf eld's

Method).

The

sucrose

is calculated
constants
as

by

Herzfeld's Select
a

formula, using
constant
sponding corre-

Steuerwald^s

follows:

to the

invert this for

polariscope-readingand
*'

temperature
Since'

and the

substitute

constant" minus

in the in

formula.
cane-sugar

invert-reading is always
Archief., 1913, 21, 1383;
Int.

work,

Sugar

Journ., 1914,

16, 82.

CLBRQET

METHOD.

269

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

divide

the

of the

direct-

and

30.4+17.9
="
~

48.3
=

=36.85. 131.06
may

"

143.06-12

The
room

inversion

be The

conducted

at the

temperature.
within above

inversion is always
at
a

complete
wlien

twenty-four hours
20** C. and the in

temperature
is
as

fact

there is certaintythat

ture temperaso

always above

20** a

period
The

short

sixteen hours

is sufficient.

twentyvenient. con-

four-hour

period is usually the


From

most

time with

this it appears is available, the tedious

that, when
inversion
with
tainty cer-

heating may
of freedom The shown

be avoided from

and

destruction

of levu-

lose. flask

special inversion in Fig. 76 eliminates pipette


in this The modification
serves

convenient

FiQ.

76.

measurements

of the
to
measure

method.

body of the flask

solution,the middle completes 100 cc. 135. Clerget's


wald.* with
"

section is for the acid and

the sugar the top mark

Method

as

Modified
at
room

by

Steuer-

The

inversion acid

is conducted

temperature
constants

increased

table of strength. A special

is

required. Prepare the solution


Measure and 1.188 add
sp. 30 gr.
cc.

as

described of the

in the

preceding paragraph.
a

50 of

cc.

filtrate into

100-cc.

flask

hydrochloric acid of 1.1 sp. gr. (acid of diluted with an equal volume Set of water).
if the temperature is between 25" C. Dilute
same

aside three hours


or

20" and
to

25** C.
100
cc.

two

hours

if above

the solution

and
as

polarize,observing the
have been described

temperature

conditions

in the

preceding paragraph. The

^Archie!,, 1913, 21, 831; Int. Sugar Journ., 1913, 15, 489.

270

SIRUP,

MASBEGUITES

AND

MOLASSES.

followingtable of
the
terms

consianits

must

be used

in connection be reduced
cc.

with
to

Herzfeld

fonnula.

The

readings should

of the normal before

weight of the material in 100

tion of solu-

making the calculations:


TABLE
at
room

STEUERWALD'S

OF

CONSTANTS.
with 30
cc.

(Inversion

temperature

acid.)

136.

Determination
in I2I9 except
use

of from ash

the

Ash."

Proceed

as

is directed

2 to 3 grams

of the material. the by dissolving


mg.

The

burning

to

normal

is facilitated then

material
of zinc

in diluted

alcohol and

incorporating 50

be deducted from oxide, the weight of which must the ash before the calculations. Or, incinerate with benzoic

acid.
cent

Dissolve

25

grams

of the
the

acid in 100

cc.

of 90 and

per

alcohol.

Moisten
a

sample with
Add
2
cc.

water

then

caramelize it at

low heat*

of the benzoic solution


at

incinerate and, after evaporating the alcohol,

incipient

red heat
For From

in the muffle furnace. is described in


a

proceedas sulphated-ash

3 to 5 grains of the material is

paragraph l^Sl. suitable quantity for

the test. 137.

Acidity

and

Alkalinity.
and

Solutions of massecuites

Qualitative Tests." molasses are usually so dark-

CRT8TALLIZED

8UOAR

IN

HASSECniTB.

271

colored be
made. 25
cc.

that

the

usual
'

tests

for acidity the


material

or

alkaUnity
method:
a

cannot fer Trans-

Buiaaon
of
n

advises
of the

followii^
to

solution

gloss-atoppeiied
and
10
a
cc,

flask; add
of washed

one

drop

of neutral

eorallin solution
and tlien

ether.

Agitate thoroughly
to

wait

few The

seconds

for the ether


excess

separate
or a

and

rise to the surface.


reacts

slightest
a,nd The and

of acid
its color to in

alkali

upon
as

the
case

eorallin
may

changes
water

yellow

or

red

the
must

be.

used

dissolving the material


be neutral. author of the the

be

distilled

the ether
In the

must

experience largely
upon

the

success

of this metliod eorallin.


He
uses

depends
the

quality
as

of the for

alcohol

soluble eorallin
of
one

prepared
of the

staining in
he
uses

copy. micros-

Instead drops
138.

drop
of
in

solution

several

of the eorallin dissolved Estimation the

in alcohol.

tallized Crys-

Sugar
"

Masseculte.

Kara

Method.
to
raw

^"TWm
sugar

method,
will be

aa

applied
cui["r
BURftr

first described,
a

then its application to

masse-

Weigh
and
an

30

to

50
a

grams

of

faw
con-

transfer

it to

glass dish
of pure the
sugar
a

taiting
and

equal weight
Mix

drous anhyand

glycerine.
rod, and
over

glycerine intimately place


acid.
to time

with
a

glass

the dish

in

desiccator
or

fused

calcium

chloride

strong

sulphuric
from time

Repeat
until the the in

the

mixing
formly uni-

crystalsare
glycerine
work
quires re-

well

separated, and
distributed This

molasses the

solution.

preparatory and

fifteen minutes
Place the
a

Upwards.
shown
to

in plug of dry filtering-cotton of the transfer

funnel

apparatus
the mixture
cover.

in the
Pio.
77.

Fig. 77;
funnel and

re-laco

the

Filter
a

off the glycrine solution, using


pump. The mixttire

filler-

should

be

protected

from

the moisture

'Zeit.

Rubeniucker-Indugtrie,

31, 500.

272

SIRUP,

MASSECUITES

AND

MOLASSES.

of the air

during filtration by
anhydrous
contact

chloride of calcium
in the

tube,

as

shown Since

at the top of the funnel-cover

figure.
moisture
so

the

glycerine absorbs
with moist

with
far
as

great rapidity, its

air should

possiblebe avoided.
Polarize obtained the above normal and
*

weight

of

the

glycerine filtrate

as

calculate

the

crystallized sugar

by the

following formulae:
x=" sucrose

in the molasses
sucrose sucrose

attached
raw

to the

crystals;

P~per
p^sper
x^

cent
cent

in the in the P"

sugar;

glycerinefiltrate;
=

and

the

percentage

of

crystallized

100-p
sugar.

Example.

"

Polarization

of the

raw

sugar*

tion 95.6; polariza-

of the filtrate =6.75.


"=

=7.55; "^^1^X6.75
of

and

95.6-7.55=88.05

the In

percentage
view

of
cane sucrose

present in
cuites the ascertained is not

crystallized sugar. the large proportion of glucose usually to masseproducts, to apply the method
x,

P, and

p, in accurate

work, should

be

This by the modified Clei^et method, page 266. of Karcz' method the case in the following modification
*

by Perepletchikow:
Transfer with
an

the

normal

weight of the
of Karcz' the

massecuite,
and

treated
as

indefinite

quantity
Wash

anhydrous

glycerine,

described

above,

to

apparatus

filter ofif the

glycerinesolution.
of the funnel from the

glycerine until the filtrate


apparatus

with repeated portions crystals is no Remove longer colored. and


The

wash

the

crystals into

sugar-flask and
the percentage

polarize them.
of This method

polariscope reading is usually requires double

crystalsin the massecuite.


"

Duponi'8 method* polarizationwith


1
"

cane

products.
Bohem,
de

Zeitschrift

j. Zuckerindustrie
Bui.

Jan., 1895.
des

Zapiski, 1894, 18, 346. Manuel-Agenda


des

Association

Chimistes, 12, 407.


et

Fabricants

Sucre, Gallois

Dupont,

1891,

p.

293.

CRYSTALLIZED

SUGAR

IN

MASSECUITB.

573

Heat

quantity
500 grams

of
to

massecuite 85*^ shown covered


as'

of and
,

known the 87. thin

polarization,
sugar

for small of the the


trifugal. cen-

example centrifugal, centrifugal


sugar
as

C.

purge

in sieve

such should

as

is be

in

Fig.
with

The flannel.
means

Dry
of the and the foUow-

thoroughly
Polarize the the

possible
massecuite, percentage

by
the of

crystals by

the

molasses.

Calculate

crystals

ing

formula: Let x="the

weight massecuite;

of

crystallized

sucrose

in

one

part

of

"=

polarization

of of of

the the the

massecuite; crystals;
molasses.

-polarization polarization
d

p^s=

d'
"

.'.

x"=

and
".

100x=the

crystallized

sucrose

in

100

P-P

parts

of

massecuite.

Example.

Let

=84.5;
=

100;

p'"60.6.

"'^^~^'a^0.eO^
-

and

100aj"e0.66,

the

percent-

age
138a.

of

crystals

in of

the

massecuite. Glucose."Proceed
as

Determination
in

the

is

described

paragraph

118.

ANALYSIS

OF

SUGARS.

130.
sugar

Polarizadon."Weigh
in
a

the

normal

weight
water
to

of

the

the sugar,
mass.

capsule. Add sufficient for the water waiting a moment


moist
sugar may

nickel

to

moisten

penetrate the

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
flask. The with
more

The

The

sugar

may

be and

washed readily neck of the be

through the funnel.


be
not

capsule, funnel
a

flask must observed

washed
to
use

jet of

water.

Care
cc.

should

than

about be

60

of water

in these
use

operations. The
(see
page

flask should

well

cleaned

before

169)
the

to

prevent
above

water

from
a

adhering

to the neck. to

Dissolve the sugar


Hold whether flask all the

by imparting

rotary motion

the

flask.
see

the level of the eye

ocasionallyto

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**),
of the
sugar.

White

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 volto foam

the neck of the flask. If washing down down interferes with this operation it should be broken
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 Having

the solution.

If

drops of

water

adhere

to

the neck

of the flask they should

by a stripof filter-paper. finished these operations, cover the mouth of the


*274

be absorbed

276

ANALYSIS

OF

SUGARS.

141.

Determination

of

Glucose."

The

method

to

be

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 Potarizing above 99**. Dissolve 40 grams in water, add normal of sugar, contained in a 200 cc. flask, 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
"

to 100

cc.

and
50

thus
cc.

one

filtration may

be avoided.
cc. a

Measure

of Soxhlet's
cc.

solution and and add 50


to

25
cc.

25 solution, i.e., of the alkali (297) into sugar

of the copper 400 cc. beaker Heat the

of

the deleaded

solution.

taking about four minutes to reach this boiling, temperature and continue the boilingexactly two minutes. At the conclusion of the heating add 100 cc. of cold recently
mixture 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. table by inspection: following
HERZFELD'S TABLE IN OR CENT LESS OF FOR MATERIALS THE

DETERMINATION CONTAINING
AND MORE
1 PER

OF

VERT-SUGAR IN-

CENT
99

INVERT-SUGAR

THAN

PER

SUCROSE.

ESTIMATION

OP

THE

MOISTURE.

277

142. driven the the

Estimation
off

of
an

the
oven.

Moisture."
The

The

moisture

is

by drying in
If the
sugar

temperature
upon

at which

operation is conducted
sugar.

depends
not

the
as

character
a

of

is of low should be

grade, such
rise above in
vacuum.

molasses in

sugar,

the temperature
sugars

lOO"* C. and Modem


raw-

fact such
sugar

should
now

dried

factories

produce
of

little low-grade
may

product, hence
comparatively
at

the

temperature

drying

usually be
be
may
even

high. A sugar of large and exceptionallyhigh-test sugars


110** C. is not A

crystal should

dried

105"

C.
to

be heated
moisture

Large crystalsare
off until
a

liable to occlude

that

driven

temperature

of 105** C.
3 grams

is reached.

drying period of three hours for 2 to of a broad the bottom spread evenly over usually sufficient. Low-grade sugars,
should
two
or

of sugar shallow dish is

in

the

absence
in
a

of

vacuum-oven,,

receive three for


a
a

preliminarydrying
should be
at

water-oven
an

and

after

hours short

transferred to
105** C.

air-oven and
recommends

be

dried

period

Pellet

conducting
with the contains. both should
143.

test parallel

with

granulated sugar,
of
water

moistened
the

estimated
When the

percentage

that
to

sample
sugar

granulated

sugar

ceases

lose moisture dried

samples
in
a

are

considered

dry.

The

be cooled

Determination
as

desiccator preparatory to weighing. of the Ash. ^The sulphated-ash


"

method both

described

on

page

270

for massecuites

is used

in

testing. factory and commercial Iron in 144. Sugars. Sulphide


"

Colorimetric

Method.'
of
pure

^Prepare a stock solution containing 10 grams solved discrystallized ferrous sulphate, FeS04-7H"0,
a
a

in addition
cc.

50-60 few

per

cent

pure

sucrose

with the solution,


to 1000

of

drops of sulphuricacid,and dilute

The acid should be very with the sugar solution. diluted before adding it to the sugar solution. Dilute
to

largely
time
of this

this stock
as

solution with
cc.

distilled water, 100


cc.

from
cc.

time

required, e.g., 10
cc. are
"

to

and

50

solution The

to 500 tests

made
'

in Nessler's

cylinders,a number
'

of
' "

Eastick, Og^lvle and

Linfield, Int. Si"gar Journ., 14, 428.

278

ANALYSIS

OF

SUGARS.

which
Into
a

of the

same

diameter and

height should be provided.

cylindersmeasure amounts increasing 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
series of these
3 to 10 grams of the sugar
cc.

in
2

Nessler's
of the

dilute cylinder,

the solution to 100


Let the

and

add

cc.

sulphide solution.

Stand ten minutes and then match the color cylinders of those containing of that including the sample with one then contain Both the same the stock solution. quantity used. of iron, The t.c, the quantity of iron in the sugar

cylindersshould stand
The

on

white

paper

in

making

the

parisons. com-

sulphide is prepared by saturating ammonium with sulphureted hydrogen and then adding an
of ammonium the
case

droxide hyequal
the

volume
In

hydroxide.
sugars,

of dark

incinerate the sugar,


at

with

addition

of iron-free

sulphuric acid, burning

the

lowest

the ash in a Dissolve minimum possible temperature. quantity of iron-free hydrochloricacid and proceed with this solution
145.
on
as

has been Dutch

described. Color

The

Standards."

entering certain countries,pay If their color is No. 16 Dutch polarization and color. they pay a higher rate of duty than standard, e.g., or lighter,
if darker The than this standard. color standards
to

Foreign sugars duty according to their

Dutch

consist

of

set

of

samples
These
are

of sugar
are

numbered
an

prepared by
the sugar renewed
from

up establishment in sealed
to

20, which

'is white
in Holland The

sugar. and

plied sup-

trade time

bottles.

samples should
sugar

be

time, since the color of the

is not

permanent.
sugar

Centrifugal 96**
when especially The with chemist
a

will

usuallybe darker than


in with the

No.

16

molasses
a

is boiled

first
be

sugar.'

of

tropical sugar
16, so
as

should factory
the

supplied
of sugar

sample

of No.
or

to avoid

shipment
and

of this color

lighterto certain countries


rendment
sugar

consequent

loss to the factory-owners. The Rendment." 146. of refined that siigar


a raw

estimated yield will produce. This esti-

is the

RENDMENT.

279

Biate

is in

based different

upon

refining
countries

experience
and for five of the the
**

and
of

is

calculated different

ously vari-

sugars

origin.
of the

The

American from the of

refiners

deduct

times

the

percentage
to

ash

polarization
rendment,
or

raw

sugar

obtain the

percentage

analysis"

of

sugar.

ANALYSIS

OF

THE

FILTER-PRESS

CAKE.

r
147.

Preparation
as

of

the

Sample.
in

"

^The

sample
be

of

press-cakeobtained
to

directed

104, should
of
a

reduced

small

fragments and mixed


If the
a

by

means

spatula or
be necessary

lax^
to

scissors. rub With will it to

cake

is very
a

soft it may then

paste in
cane

large mortar,
may

subsample
the

it.

good
be firm

and the

careful

management
be

press-cake
of the
in X

and

sample
tared

readily reduced.
5

148.

Moisture
a

Determination."
shallow

-Dry
to

grams

press-cake, in
a

dish,

constant

water-oven

at

approximately
be

100** C.

The

weight loss of weight

20=

percentage of moisture.

The before

sample

should

partly dried

at

low

temperature

to 100" C, otherwise the surfaces of heating the oven be covered with a glazed coatthe fragments of press-cakemay ing

which convenient
to have

would

prevent the

escape

of moisture.

It would

be

in all
ovens,

open-dish dryings of sugar-house materials


one

two

heated

to

low

temperature
25

and

the

other

to the

final'temperature.
Determination.
to
a
"

149.

Sucrose

^Transfer Add
cream

grams

of

cake filter-press
to the

small it to
a

mortar.
a

boilinghot
with the

water

sample
cc.

and

rub into

smooth

Wash add the


6

the material subacetate


to

100-cc.

flask with

pestle. hot water, cool,


of the flask thoroughly,

of lead
cc,

solution the

(54.3** Brix), complete

volume

100

mix

contents

and polarize. The polariscopereading is the filter, in the press-cake. percentage of sucrose of the sample, 50 grams convenient It is usually to use more of lead while rubbing the material and add the subacetate
to
a

cream

and

wash

all into last

200-cc.

flask. This facilitates

the

removal A

of the

portionsof
neck

mortar.

flask with

the

press-cake from the enlarged above the gradua*


the 28a

SUCROSE

DETERMINATION.

281

tion

is

more

convenient

in

this

analysis

than

an

ordinary

sugar-flask

(Fig.
The in is

78).

object

in

using
instead the of

25

grams

of the of

the

material

this
to

analysis
correct

of volume

normal the
matter.

weight
lead
cipitate pre-

for that

and Parallel

the

insoluble

experiments,

on

sample

of and

filter-

press
100
oe.

cake,

by
by

the

method acetic of in each

described,
acid,
lime
9.6

also

modified
to

adding
saccharates

after and

cooling,
tated precipicent

decompose levulose,

gave

per

of

sucrose.

A
to

third

portion
with of hot

of
water

this and washed

sample
defecated
onto

was

rubbed with filter. hot and The


100
water

cream

Fig.

7"

subaoetate The 200

lead,
was

then continued The

washing
cc.

with

very

to

nearly
to

of

filtrate.

filtrate

was

cooled
of
4.6.

diluted residue and

200

cc.

and

polarized,
into
a

giving

reading
and 0.5. diluted The other

was

washed The

sugar-flask polarized
same as

to

cc.

filtered.
0.5

filtrate the

sum

of

4.6X2+

is

9.7,

or

nearly
that
25

in

the

two

experiments,
correct
amount

showing
of

grams

is
to

approximately
use

the of
the

average

material

instead writer have

normal similar

weight.
results
to

Many
those

experiments
described.

by

the

given

ANALYSIS

OF

THE CHIPS

BAGASSE

AND

EXHAUSTED

(DIFFUSION),
the

1^.
the

Preiiaratton of
as

Samples."
be

After

securing
oughly thorbe

sample

described

in 100, it should

rapidly and

mixed

and
to

quickly reduced
The

subsampled. The subsample should small piecesby chopping or shredding.


small.

preparation of the sample for the sucrose important. The pieces should be very
laboratories

test is especially

The
to

Java
pass

require this sample to be fine enough

^ 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,

however, has stated


is reallylargely due

that the apparent

influence

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
to incorrect

largest admissible the opinion of the writei^ attempts


the diameter of the. finer than Norris'

piece of bagasse.
to

In

reduce

the
errors

material

lead to specification may the the drying of the sample, especially when

through
content

sucrose

is

high.
found
4
per

Norris

made

numerous

tests

to

ascertain

the

average

loss of moisture it to average


cent

and and

during the preparation of the sample the chopper is covered 2 per cent when
uncovered. From be these

when the
even

observations
as

it is evident
as

that

sample should
then the is often
a

prepared
numbers

rapidly
be
a

is

and possible,
too

sucrose

may

httle
may
sucrose

high.

There

offset this error, in the

compensating error viz., slightly imperfect extraction


result in

that
of the

digestion.
may
a

Slow

preparation of the sample

large error

1 "

Int.

Sugar

Journ., 1912, Sugar

14, 43.

Ibid., 5.
Planters'

Bui. 32, Haw. "Ibid., 8.


i

Ezpt. Sta., 32. 282

284

ANALYSIS

OF

BAGASSE

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

151.

Determination
in the

of

the

Moisture."
it is of

As

has

been
to

indicated

preceding paragraph,
on

importance

dry
be

large sample

account

of the lack of uniform

tion distribu-

of the moisture.

It is also in which

important that the sample


it is received from the

dried in the condition


error

to avoid mills,

from both

drying during the manipulations.


a

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 vacuumshown that
ovens

Experiments laboratory have

upon

manufacturing scale and

in the

at low

temperatures is not dependable.

Many
less.

writers From

recommend the

drying samples of

20

grams

or

even

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 of that shown requiresa specialoven onthfB principle
"

in

is The Fig. 81. oven provided with a removable and the clamps, E, insure an
oven

cylindricalcast-iron vessel, C,
cover,

D.

rubber-gasket, /^
the

jointbetween air-tight
The

body

of the

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
cover.

and

the

but
water

this does heater

not

appear
an

to be

necessary.

small

size feed-

is

inexpensive and
exhaust drawn

efficient
steam

heating device.
the

If this heater the air should

is uiSed with be

from

engines,
steam
over

through the
steam

copper

the coil,
pass

surrounding it,but with live


the coil, The
heat specific

the air should

of air is

low, hence

the

pipes

DBTBRMIKATION

OF

THE

HOIBTtTRE.

285

should used.
A

be

covered

ajid

very

large volume
of Two

o! it must

be

cylindrical bagasae-baaket
oven as

very
or

thin
more

sheet

brass, A,
should

fits in the

is indicated.

baskets

be

provided

and

tared

if many
is of

samples
brass

are

to be dried.

The

bottom
as

of the

banket

finely perforated brass


Sheet

plate, such
about 625 1'he

is used

in centrifugals.
square

containing

round

holes per of the and

inch is suitable for this purpose.


A
narrow

top

basket makes and


a

is open.

flange supports
The

the

basket

joint vilh the iron castings. bagasse and


the
pressure

weight
air
are

of

the

basket

of the

ueaally sufGraent
gasket
forms oS

to

insure
may

good
be
of the

joint, but
used. The

if need

be,

steam-packing

thermMneter,
If the
oven

H, indicates the temperature


one

air current.
should in the

of A

battery,

stop-valve

be provided in the
current
on

pipe
of

G.

valve

is also convenient
to

regulating the
steam

air.

If it is desired

leave
oven,

turned
to

the

ejector, F, when
an

opening the
cover
or

it is necessary for
use

provide

fur-eock

in the

elsewhere

in breaking the

This

oven

may

be

constructed

of any

convenient
a

'siw.

Those

constructed and
12

for the nriter


inches
or

will receive

basket will hold

8 inohes

in diameter

deep.
2

This

basket

gram 1 kilo-

of loose bagasse

kilograms if lightly packed.

The

286

ANALYSIS

OF

BAGASSE

ANP

EXHAUSTED

CHIi"S.

drying period is extended


basket shown The of this size may in

ft

few minutes

be used

A by the packing. with the 5-kilogram balance

Fig, 44.
of

method

drying is as follows:

work, reduee, the sample to about 2 pling; fill the tared basket with 2 be necessary. packing it lightlyas may
in the oven,
steam

Assuming efficient millkilograms by subsamkilograms of bagasse,


Insert the basket sufficient
very

the replace

cover

and

turn
a

high-|;":e8sure
current

into the The

ejector to produce
be heated
to any

strong
The

of

air. above

air should

conveni^t

temperature

110" C. and

pr^erably

to 130" C.

air-pipeshould

be well covered. varies with the temperature of the air and drying -period 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
a

little experiencewith thfe oven


"the basket

may

be

fixed,remove

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
per

arbitrarily place it in a

cent

of
cent
oven

dry
of
as

matter.

The

per

cent

moisture

is 100

minus

the per The

dry matter. originallydesigned by the writer


lower section contains the six
oven

is self-

contained. and

The

heating-coils,
grams

in the upper are The capacity each.


more

bagasse

drjdng-tubes of 200
is less

illustrated

expensive and
may

is

accessible for be

easily

It repairsthan the older model. built in the plantation shops, largely from

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,
"

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

moisture

in

it.

Wrap

up

about

"""-

"

"--

"

"

--

' ---

-t
--

"i-_,j,_

_^^^^

Journ.

Ind.

and

Eng.

Chem.,

June, 1910, 9t No.

6.

DETERMINATION

OF

THE

MOISTURE.

287

dr3ing-oven described
the

farther

on.

In

making

the

weighings
this introduces otherwise the air.

package should

be

transferred

out directly to the scale with-

awaiting
a

the

cooling of the material.


this
error

While
would from

small error,
case

is smaller of

than

be The

the

through absorption

moisture shown

calculati""i oi the moisture

is best

ing by the follow-

example: Weight Dry


of the

mosquito-netting and mosquito-netting

pins.
*

60 56
. .

grams
t(

weight

of the

and

pins.

Moisture

grams grams
""

Weight Dry

of the

package of bagasse package


of

2060
1096

weight

of the

bagasse

Moisture
"

in the
" "

bagasse and netting... bagasse

netting

964 4

grams
"

i4

I*

"*"

960

grams

2060 9C0
H-

-60 2000

=2000= X 100

weight of the
=48.0 per is
cent
so

bagasse used.
moisture
in the

of

bagasse.
that
an

Tlie
error

quantity of bagasse
of 1 gram in

large in
an

this method
error

the

weight makes
the

of

only

.05 in

the

p"er cent.

Experience
very

has

shown and
at

dryings by this method


24

to

be

complete,
desiccation
a

that 110* C.

usually
could

hours

are

required
for the

for the

Manifestly netting.
fall from A the

metal

basket

be

substituted

small

quantity of bagasse-dust will sometimes


its

package, but
shown in

weight is

too

small

to

ciably appre-

affect the accuracy The


tests.
oven

of the test.

Fig. 82

is suitable

for

use

in

these

Drying
as

in

Metal

Trays.

"

Shallow
A

metal suitable of

trays

may
use

be
on

used the

containers balance

for the and

bagasse.
50

size for

sugar

holding

grams

bagasse is 4 inches by 8
progresses
or

inches the

by

1.25 of

inches the

deep.
of

The

drying
gauze
oven

faster

if

bottom The

tray is of wire
the

perforated sheet
be
at

brass.

temperature

should

least

110** C. and

preferably 130" C.

1
288
ANALYSIS OP

BAQASSE

AND

EXHAUSTED

CHIPS.

SUam

drying-otien. The
"

steam

drying-oven is

shown

id

Fig.

82.

It

is

most

conveniently constructed

of

2-incb

Two steam manifolds, or planka of well-seasoned lumber. live used with steam to heat the coils,C, of iron pipe are
oven.

Half-inch
use

iron

pipe is suitable
of one,
at A

for

making

the

coils.

The the

of two

coils, instead

facilitates

regulating

temperature. Holes in the door of the


eir escapes
oven

oven

admit

air, and. the moist


can

wiirm

at

D.

thermometer
a

readily
wall
near

be

inserted in the shelf B.


mesh This

by boring
or

hole in the of
a

the

shelf

tray B is made door


the

wire

screen.

The
be

should

be large. The

and

other

parts should

protected
'

from

warping by
be

There

should
to

usual carpenter's expedients. pipes, globe-valveson each of the inlet and tailsteam

each

coil,to regulate the


water.

and

the

dischai^ge

of the condensation
An
oven

house
many

of this type is a very convenient part of a sug"rnot only be used It may for latxHutory equipment. tests, but DeterminatloD
The
serves

moisture

also in

drying glass-ware, etc.


"

153.

of the

Sucrose.

Single-digestion
of

Method.

"

following is the usual method


sucrose

detfrmining
50 grama 1000

the percentage of

in the in
cc. a

bagasse: Weigh
and
2
cc.

of
cc.

finelydivided bagasse
capacity and add
sodium carbonate.
600

dry, tared flask of about


of be
a

water

5%

solution of
a

The

flask

should
a

provided with
about

reflux condenser, for which


4 feet

purpose

small glass tube

long will

answer,

DETERMINATION

OF

THE

SUCROSE.

289

and continue gentleboiling hour. Cool and weigh the flask and the heating during one Drain off a portion of the solution, contents. clarifyit with tube. dry subacetate of lead and polarizeit,using a 400-mm. in the solution is made calculation of the sucrose The by described for use with dry lead,page 500. Schmitz's as table, 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 the degree With these very dilute solutions, table, page 506. Heat the contents of the flask to Brix The need
not

be considered of

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

Weight

of flask +
"

bagasse +

water

620
110

grams
"

"

"

"

bagasse +water fiber in bagasse


thin

510
=

'*

50X0.45=

22.5
487.5 page

''

"

juice method, juice,Home's


-r-

"

Polarization
mm.

per The

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
copper

of thin

X2=5.56.
A for

Fig.83, may digester,


This should be

be conveniently about
4

substituted

the

flask.

inches

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

disk

for

mixing
tube.

purposes,

should should

pass

through and
moved
up

extend
down

above

the

The

rod

be

and

either by hand or mechanically. A Kodak occasionally 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, results in with consequent large return from the condenser,
a

dilution

error.

2d0

ANALTBIB

OF

BAQABSE

AND

BXHAU8TBD

CHIPS.

Repotted JHgttlwn
a

Method.
cover

"

In 100

suitable
grams

dish,preferttbt"
finely divided
Drain peat Rein all

porcelain caseerole,
with
water

of

bagaase
off the

and

boil it durir^ ten


with the
an

minutes.
iron spoon.

pressing the bagasse liquid,

this

digestion
Press

with the
press

water

and of the unite

decantation in
a

eight times.
hydraulic
those
or

residue and

bagasse
Cool the

powerful
to

other

the

liquid expressed liquid


to

portions already di'ained off.

the

ordmary
a

temperature
water
to

and

measure
an

it, adding, if need easily measurable

be,
179.

Uttle

briug

it to

volume.
page

Clarify the solution


The

by Home's

dry-lead method,
may

degree

Brix

of this very

dilute soluticn
a

be neglected. observationof

Polarize the solution,preferably using

600-mm. the

tube, and
table
on

calculate
page 500.

the

sucrose

with

aid
has 3.

Schmita's used
per

If the should

600-mm, be divided

tube

been This

the
cent

polariacope reading
sucrose

by

is that of the extract,

Con^dcr

the cubic

centimeters

292

ANALYSIS

OF

BAOASSE

AND

EXHAUSTED

CHIPS.

at the
cover.

when not in top of the inner vessel,


It should
not

use, and

serve

as

be removed

until after the At the

completion
^

of

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 The calculation of the per
cent
sucrose

and

it in cold water. made


as

is

in the
states

Norris

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 as in the'cane, directly 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
Let

are

obtained

in the mill control.


matter

/Si=the P=the C=the

bagasse; bagasse; per cent sucrose coefficient of purity of the residual juice (see dry
in the

in the

next a;=per

paragraph); cent fiber (marc) in the bagasse,


x="Sf-100P/C.

then

Steuerwald, of the Java


of the various
at the conclusion most

Experiment Station,in
of fiber
as

an

gation investi-

methods

arrived determination, above

that the indii-ect method He considers and

gives the
the aqueous

reliable results. alcohol-extraction methods

the claims concludes

of the .waterthat

and

methods

and the alcoholic extraction, give high figures, correcting for the separation of saccharetin from the even gives low figures. fiber, ^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,
"

since

the

between

bagasse receives its final and heaviest the juiceflowingfrom the last pair of rolls,

pressure

the last

EXHAUSTED

DIFFUSION-CHIPS,

SUCROSE.

293

roll

probably
The the
155.

more

nearly
of The

approximates
purity
of is this made

the

true

residual in culating cal-

juice.

coefficient fiber.

juice
as

is

used

analysis

for

other

juices.
press Ex"

Exhausted the

Diffusion-chips,
juice
a

Sucrose.

thin

from

the

well-drained several in

chips
times

by
with

passing heavy
press.

them

through
at

laboratory-mill
the

pressure,

press

chips
as

powerful juices.

hydraulic
Consider the

The

analysis
of The this

is

made
to

for that

other of

ization polar-

juice
of

be thin

the in

exhausted

chips.
chips
fresh be cane,
sponds corre-

weight
very

the

juice
the

well-drained
of the

nearly
so

with
it. in of

wei^^t
This

and

it

is the

usual

to

consider

weight
the is fiber found

may

estimated
a

by
stant, con-

following i.e., all

method,
the fiber

which the

is in

considered
the

cane

bagasse:

Let

F F'

the the

fiber
fiber

per per

cent cent

cane; exhausted

chips;

"

100=

the the

weight weight

of of

the thin

cane;

juice

in

the

chips,

then

F'(a;+F')=100F
of thin

and

100F/r-F',
cane.

the

weight

juice

per

100

Both

the hence

fresh the

and direct

exhausted fiber

chips
detenninations

may

be

accurately
be used

sampled,
in this

may

calculatioQ.

ANALYSIS

OF

FACTORY

WASTES.
Diffusion
the

156.
"

Analysis
at

o! Waste
waste

Water,
waters

Prooess.

^The

polarizationof
least
a

from

diffusion-battery
in order
to
are

requires
attain

50O-iiim.

observation-^ube The
waters

reasonable

accuracy.

after iOtration of

the use usually clear enough to polarize without As few planters have polariscopeslong enough f op a mtist tube, a Ghezmcal method generallybe used. Concentrate the s"mple to 5 per cent of its volulne.
.

lead.

SOO-^nm.

Invert tion propor-

the

sucrose

by
cc.

means

of 75

hydrochloric acid
cc.

in the

of

acid. to

of the concentrated

89).
sodium

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

Nearly hydrate.

neutralize

the

acid,
the

after

sample (see inversion^ with

Determine

quantity of glucose is
may

too

small

to be

taken

account

of, and
189. the of

be

neglected* Use Meissl and Weiu's


prese?ice

table,l"age
of sucrose
oa

The
waste

of
an

aicpnsiderable amotint
evidence
of gross

in paft

water

is

neglect

the

the

batterymen. 157. Analysis


of

of

Foam
a

from littleether

Sirups,

etc."

current

or compressed air,

will

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

rapidly evaporated, liquid. Remove the

described,beginning 125. 158. Analysis of the


water

Boiler is

Feed-Water.

"

^The

feedthat the the

for

the
from

steam-boilers the

evaporated
steam

juice and

largely derived from sirup. ^The water from


of the first vessel
of

condensed

in the

calandria and

the calandrias multiple effect, and the coils and


source

coils of the heaters

tubes of water

of the various

vacuum-pans forms a very

important

supply for the boilers.

Sugar
294

may

ANALYSIS

OF

THE

BOILER

PEED-WATER.

295

enter from

these
the

waters

through entrainment

with

the

vapors

sirup and in the heating""urfaces. Sugar


causes

juice and

through defects that develop


foam in the boilers and may

the

water

to

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
to

the

tubes

and

shells of

the

causing boilers,

pitting and overheating. The sugar is supposed to be first hydrolized,after which the dextrose and levulose decompose. The dextrose formic and acetic acids,and produces levulins,
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 form

only when
on

the water levulose


af^ear
to

contains in

ammonia

or

soda*. Except
monia am-

for its action

does not Fats


water form

forming humic compounds, the plates. injure


with the

introduced absorb thin

into

hlgh-^essure boilers
compounds
and'
no

feed-

the humie which

threads retards

but longer float, deposit in non-conducting layers.^ action whi(;h is most

Ammonia
at

the chemical

vigorous

the hottest

parts of the boiler.

position Sugar itself does not attack the boiler metal, but itsdecomand physically. The products do, both chemiisally 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 the
.

addition

of soda

to the

water

or

by reducing preferably

acidity of the juices.


that
a

thorough control of the feed-wat^r is The moment the best ^feguard against sugar. sugar appears
in the water should
as

Jt is evident

this should be

be turned' to the down.

sewer

and

the boilers

thoroughly blown
be used
at very

below

should

"-naphthol test frequent intervals in testing


of sugar in it. The odor

The

the water

and in tracing the

sources

Osier

.-Ungar.

Zeit.

Zuckerind,

1912,

43,

397;

Int.

Sugar

Jou^n.,

1912,

14, 472.

296

ANALYSIS

OF

FACTORY

WASTES*

of the
sugar.

steam

is very

pronounced when

the water

contaiiis

Qtuditativeand Approximate Quantitative Tests for Traces Sugar


in Water,

of
be its
pa-

detected

water circulating qualitativelyby the o-naphthol method,


"

^The

sucrose

in the

may

and
a

quantity also
cent

estimated

as

follows:

Add

drops

of

20

alcoholic solution of

then by means test-tube, in 10 of the tube, run In the of presence of


sucrose

a-naphth"d to 2 cc. of the water in a of a pipette, reaching to the bottom of concentrated sulphuric acid. cc.
a

violet

zone

appears

at

the

line

demarkation

of the

two

Uquids and

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
per ceut si^crose

the

color

with

O.OOr per cent sucrose, aoid used The in this test

darknned of very wine; the entipe solution is colored. is that


must

pure

The time

strictlychemically and the a-naphthol should be of very good quality. solution of the reagent should be freshlyprepared from
to time test 1

be

and is

should

not

be colored. When the solution


a

"

This

extr^nely deUcate.
sucrose

tains con-

part of
the

in 10,000,000 parts of water in the

paleof and

Ulac

color

is shown
sugar

test, and

with

0.2

per

cent

sucrose,

is charred

by the acid.^

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.

Automatic
"

Alarm
^This alarm

for is

Sugar
based

in
upon

the the

BoUer

Feed-water.* in

change

It is comdensity of the water in the presence of sugar. posed of two communicating tubes (communicating vessels) within and the other. The
water

one

is stagnant
at
a

in the

inner A

tube

flows through the

outer

constant to

level.

float a change of level in the inner tube causes close an electrical circuit and ring a bell. Since
^

rise and
water

the

Rapp

and

Besemf

elder, Deutsche 6, 198;


Ed.

Zuckerind.,
in Jour.

1892,
Chem.

538. Soo.

Monatsch.

Chem., Lavan,

Abstract

Abs., 50.

923.
I

Avertiseur

Gallois, Paris.

COBALTOUS

NITRATE

TEST

FOR

SUCROSE.

297

is

of

the

same

temperature
corrected. The of the the 1.001

in

both
columns will of

tubes,
are

the 1.5 the

density
meters

is

automatically .therefore
It increased be is
a

high,
1
mm.

solution that

sp.

gr.

lift

float

evident

sensibility
contact.

the The

instrument instrument free

may

be

by
in A and

adjusting
a

should

placed

convenient bell in should the Nitrate solution

location be

as

as

possible
feed-water

of

vibrations.

placed

near

the

pump 160.

another Cobaltous

laboratory.
Test add After
5

for of

Sucrose.^
"

^To
cent

about of

15

cc.

of

sugar

cc.

per

tion solutwo

cobaltous add
2

nitrate. of
50

thoroughly
solution of

mixing
sodium

the

solutions,
"Pure
sucrose

cc.

per

cent

hydrate.
color

gives
permanent.
soon

by

this Pure

treatment

an

amethyst-violet

which color

is which

dextrose

gives
green.

turquoise-blue
When the is dextrose
two

passes

into coloration
1

light

sugars

are

mixed

the and

produced
sucrose

by
in
9

sucrose

the

predominant
can

one,

part
the

parts
with
with

be such

distinguished.
as

If

sucrose

be

mixed

ties, impurior

gum-arabic
lead before

or

dextrin,
the

treat test.

alcohol

subacetate

of

applying

"

Agricultural

Analysis.

H.

W.

Wiley.

Vol.

lit,

p.

189.

ANALYSIS

OF

MOLASSES

CATTLE-FOOD

(MOLASCUIT).^

161.

Determination
a

of tlie Moisture*

"

Dry
and
as

granu)

of the food in

flat dish, at the temperature


10

of

boiUng water,

for

hours; cool in
the

desiccator

weigh..
before..

Repeat
If note

drying 1 hour and weigh there has been only a slightchange


the total los;s as This the

of

weight,
driven the
centage per-

weightof

water

off.

The

weight multiplied by 20 is of moisture in the sample. lead bottle-caps, used by dealers


very

in chenafor

ical supplies,form
moisture
8

conyenient dishes They


to
are

determinations. and
may
use

very

pensive inex-

be obtained

of many

different
away.
"

sizes.
162.
erate 131. 163. 2

After

they
of the

are

be

thrown

Determination
grams

of material

tlie Ash.
as

^Incin*

described

in

Etiier

Extract."
as

Extract

to 3 grams

of

the

food, dried
161,
with
is most

described

in

"

graph para-

anhydrous

alcohol-free ether.
in Soxhtube tared
is .connected
a

The

extraction

conveniently made
modification
in of

percolator,using Knorr^s
let's apparatus
D is

shown

Fig.
with

85.
a

The small
tube

connected

by
reflux

cork The

flask

containing ether.
with
a

outer

condenser

and from wire. small

the

tube

percolator is prevented tube Z) by a spiralC of copper


or

closing the
A

syphon-

tube
1

is sealed

into

the

lower
of

part of the

percolator
A^cultural
298

Partly based

upon

methods

Official Association

of

Chemists

300

ANALYSIS

OF

MOLASSES

CATTLE-FOOD.

166.

Sucrose

and

Glucose.
"

^The methods

sucrose

and in

glucose!
page
a

are

determined solution for

by

the

chemical
is

given by
10
water

187.

The

analysis
of

prepared

extracting
grams
on a

smafl

weighed
with The The

portion
successive

the

cattle-food,
of

for

example,!

portions
is

boiling
to
a

filter-paper.
500
ec

filtrate

cooled
tests

and in

diluted the

suitable work

volume,
will indicate

preliminary
dilution. Notes the control excellent

glucose

the

proper
167.

on

Cattle-food

Analyste."The required
The

moisture

and the in

sugar of

tests

are

usually

by
material

the

factory
is

in

the condition

maiiufacture. for the

usually
further

analysis,

without

preparation.

DEFINITIONS WORK

OF AND

EXPRESSIONS
THEIR

USED APPLICATIONS.

IN

SUGAR

168.

Normal
"

Juice. normal
or

Undiluted undiluted
as

Julee.

Absolute

Juice. assumed These

The
to

juice

was

originally

be

the

juice
now

expressions are

actually exists in the cane. applied to the juice extracted by


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


cane

has established
water

the latter.

is known

to

contain

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
cane,

it may
"

be

well to consider

this the

water-soluble
water

stituents con-

solids dissolved ^juice

in all the the

contained

in This the
are

the

cane.

This
assume

may

be

termed

"absolute

juice."
and cells The

would

that all the cells may

be broken

down

solids be
never

distributed in their liquid content.

extracted therefore the juice ruptured in milling, in dry milling can juice. only approximate the "absolute" This the inferential fact has an important bearing upon all methods 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,

purity of
mixed
to

culated juice (109). A factor is caland that of the from the aensity of the crusher-juice juicesobtained in dry-miUing. This factor is applied
or

the mixed

diluted

crusher-juicedensity to ascertain that of the normal juice Crusher-juice Brix, 20^; mixed juice. Example:
the 301

302

EXPRESSIONS

USED

IN

SUGAR

WORK.

Brix, 19.7;
323. 169.
are as

factor

or

ratio

19.7 4-20 =0.985.

See

also page

Mixed used

Juice.
to indicate

Diluted the
sent

Juice.

"

These

sions expres-

juice extracted

by

all the

mills
This

mixed it is finally

and

to the defecation-staUon.

juice is usually diluted witli the saturation


170.

water.

Bagasse.
' '

Megasse.

"

This

is the

woody
The

residue word

left aft^
'*

megasse 171.
as

expressing the juice from the is used in th^ English colonies. The Residual Juice. bagasse
"

cane.r

may

be

sponge

that absorbs and

retains

part of the

r^arded juice. The


^'

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 residual

juice is determined.
the percentage
In

This
or

number
marc

is used

in

culating cal-

of fiber

in the

bagasse and
the
same

cane.

practice the juiceflowing from purity


as

the last nijill of the


to have

train

or

the last roll of that mill is considered

coefficient of
uses

the true

residual juice. The

writer

the

juice from
Fiber
or
cane.

the

of the last mill in this discharge-roli

test. 17;5. matter

Marc.
The

"

This fiber

is
or

the

water-insoluble mined deter-

of the

true

cellulose is not

in the factory control. 173.


cane

Sirup.---The sirup is the concentrated juice of the


which
no

from

sugar

has

been

extracted.

This

is the

^'meladura"

of the

''sirup'' has an it is applied where


removed.
174.

factories. The word Spanish-Ammcan in sugar refineries opposite meaning


to

solutions

frpm which

sugar

ha^

been

Massecuite.

"

The

massecuite

is

the

trated concen-

sirup or molasses in which


or

the sugar

has been
a

lized crystal-

the material

has

been concentrated to

crystallize. Massecuites are numbers indicating their purity or


it will of crystals 175.
sugar

point where designated by names or


of crops of

the number
.

that

are

to be removed.
a

Molasses.-rWhen
sugar

massecuite

is ^un

in

the centrifugalmachine the mother liquor. This and is designated by names

crystals are separated from termed liquid is now ''molasses,"


and numbers

correspondingwith

CIBCULATING

WATER.

303

the massecuites. residue


aocoimt

The
no

'^

final '^

or

true
can

molasses be

is the liquid
on

from of

which

more

sugar

removed, either

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 circulating through this apparatus. This water is often termed "cooling-towerwater."
" "
"

177.

Sweet-water.
of the

"

^The

calandrias
into it

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 refinery practiceany very apparatus it contains no sugar.
dilute sugar
178. vapors
**

solution is termed
"

"sweet-water."
sugar

Entrainment.
from

^When

h carried off with

the

the evaporators and

vacuum-pans,

this is called

entrainment."
179.

Coefficient

of

Purity." The

coefficient of
sucrose

purity as
parent ap-

is the percentage usuallyapplied

of apparent This

in the

solids (Brix) of the material.

coefficient is calculated

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.
in the
same
as

manner,

except

that

the

percentage

of

solid the

matter
sucrose

ascertained
as are

by actuallydrying the material

and

determined used.

by

the

Clergetor double"polarization
industry is
and that the
sucrose

method
The
term
'*

general usage
coefficient of the

in the

sugar
to

to

apply

the

purity"

the number

when

calculated

from

apparent

degree Brix

by direct
so

polarization. It
is an

is well known

this coefficient
for

lated calcu-

approximate number, but


in sugar
so

comparative
and

purposes

it is of great value

manufacture

will doubtless

always be

used.

Frequently approximate data of the purity

304

EXPBESSIONS

USED

IN

SUGAR

WORK.

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

apparent

coefficient, bearing in mind


must

its

shortcomings.
that the

Since

allowances

be

made,

it is adrisable
very

analyses be always conducted under be given the that due weight may
On used
among

similar

conditions,

coefficient.

the in the
or

other

hand,

the

true

special
various in

researches

of purUy is only coefficient and in making comparisons


different stages of the of two
''

products

at

facture manu-

comparing

the work word

or

more

factories.
nevet

In

using this coefficient the


case,

true"

should wotild

be

omitted,^as is pften the


be

renderingwhat

otherwise

valuable
The

^^ta almost

useless.

expressions ''quotientof purity," ''degree of purity," often simply "the of purity," and quotient," "exponent
and
the

"exponent"
modem and

are

used

With
molasses

methods

refening to this coefficient. of sugar-house work, "boiling in"


the

in

in motion, using crystallization

apparent

coefficient is very

frequently required
Coefficient, Glucose

and

is of very

great

value.
180*

Glucos^:
Ratio.
Per
cent
=r
" "

per

100
as

Suerose,

Glucose

"

^This number

is calculated

follows:

glucose
-,
"

X 100

- "

-.

"glucose
*

": coefficient.
,

"

Per
"
" "

cent

sucrose
'

This

coefficient is useful

in

detecting inversion
no sucrose

of

sucrose

in the manufacture.

Provided and
no

has been been

separated
or

from

the

material
an

glucose
the

has

removed

destroyed;
inversion. It is of both sugars
*

increase

in

glucose

coefficient

indicates

but hardly probable that by possible


sucrose

the

destruction
the
two

and

glucose the
the
samfe
"

relations

between have

might remain
Saline
sucrose

and

yet inversion
saline

occurred.

181.

Coefficient.
per

^The of ash.

coefficient is the

quantity of

unit

Calculoiion: Per
-r=r

cent cent

sucrose
"

,.
"

"saune

coefficient.

Per

ash

APPARENT

DILtJnON.

305

182.

Apparent
noraial

Dilution
amount

(Diffusion
of water

Process)."

The added

apparent dilution is the


to

that has been

to that of the juice to increase its volume certain juice-contentin the diffusion-juice.This assumes a

the

cane.

183. in

Actual

Dilution.

"

^This and

expression is used
its

both

milling and diffusion work


to

is the percentage of water

added the

the

normal

juice to reduce
of the normal

density to
actual

that
tion, evapora-

of

diluted

juice. Hence
terms

it represents

the

in percentage
water
terms

to juice,

reniove

the
to

of dilution. of the

This
the

number
cane.
"

is

preferablyreduced
remarks in

weight of
on

184. 179 all the in

Notes

Coefflcientis.

The
true

paragraph

regard

to

apparent
from

and

coefficients

apply

to

coefficients

derived

the

percentage

"of sucrose,

degree Brix, or the solids by drying. According to usage, otherwise stated, the apparent coefficients are except where
meant.

185" Available
the that calculation
a

Sugar.
be

"

Several
sugar
or

formulae

are

in

use

for

of available

factory should

able

to

the sugar it is assjimed lobtain with juicesof a

given analysis. Manifestlythere


control the
in the the

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 should be of its impurities,as well as its richness, nature

taken take
up

into
more

account.

cane

grown

on

certain

soils may

melassigenicsubstances than one of the same and and equal apparent richness purity from another soil, consequently the proportion of actually available sugar formula would indicate whereas a would be quite different,
canes

the

to be

equal.
are

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 the elements
of the must

Available

sugar-numbers

but

take these elements

into account. available


sugar

The

application of practical

calculations^

306

EXPRESSIONS

USED

IN

SUGAR

WORK.

except in estimatingreturn
the present work of
a a

from

new

investment,is

in

paring com-

period or with that of


SOU and of climate. several Such

factory with that of some ous previlocated as regards factorysimilarly


are

calculations

of value

in the
a

trol con-

establishments
event

operated under
to know

central out (1) with-

organization. In this stock-taking, how

it is desirable

nearly a factory is approaching its much efficiency; (2) how previously demonstrated sugar whether the factory is becoming is in process to determine congested and
modification

requires either
or

reduced

a grinding-rate,

of the process, much and of


sugar

closer

supervisionof the

sonnel; per-

(3) how

accounting
reduce the extraction. Available
cane

reasons

for commercial is in process or it is more (4) whether profitable to sacrifice somewhat in

rate

grinding or
estimates

juice
when

sugar
on

also

become

necessary

is

purchased

basis of its for

analysis.
sugar
were

The based
sugar

earlier formulae
upon

available

evidently
of beetbranches
cane-sugar

refiningexperience and
The
are

possibly that
of these of the

factories.

conditions
very

in both those

of

the

industry

unlike

factory and
The

will not
sugar

apply very
from
cane.

fullyin the calculation

of the

production of

following formula by Winter and Carp was published ^ and is based upon experience in Java, by Prinsen-Geerligs which represents very favorable tropicalconditions:
X
=

available
cent

sucrose sucrose

per

cent

cane; terms

^=per
C

in the

juice in
the

of the

weight of

the cane;
="

coefficient of

purity of
a;=/SX

juice.

(-f )
"

To
sugar,

calculate the available


divide the value of
x

sucroee

to terms

of the available

of the sugar by the polarization 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
^

International

Sugar

Journal, 6, 439.

308

EXPRESSIONS

USED

IN

SUGAR

WORK.

It should

be

remembered
than "to

that

"run"
as

liable to fluctuations

date,"
runs.

figures are more they may be affected


It should be stated

by the

errors

of estimate

of two

operated beyond its normal capacity, factory was n umber froni thus necessitating sUght changes in its efficiency
that this time
s'

to
as

time. the

This "to

affects

the

estimate

of

the

available

gar

date" the

number, for the previous efficiency


Also
crop

run

is used

in

calculation.

in the is used.

first

run

the

average 186.

number Sucrose

for the

previous
or
sucrose

Betentlon

Recovery."
sugar.

This

number

is the percentage of the retained


or

in the extracted

juice that is
ing In the follow-

recovered of
a

in the commercial
sucrose

example
number: Sucrose Sucrose

balance, 92.32

is the

retention

in the extracted in the sugar

juice, per
cent

cent.
. .

100 in 92
.

per

sucrose

the extracted

juice
per cent
sucrose

32

Sucrose

in the molasses

in the extracted Sucrose


in the

juice.
cent
sucrose

6.58

press-cakeper in the extracted juice


in the undetermined in the extracted

.44
p^r cent
crose su-

Sucrose

juice

66

100

Number. Efficiency Boiling-House Many factories use numbers how retical to show efficiency nearly a theoThis number is usually yield of sugar is obtained.
187.
"

the

percentage
number
sugar

relation

between the

the

actual

retention
upon

or aa

recovery

(186) and
formula.
A

number

based

available

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

100(1.4" 40/Purity)

may

be

ascertained

by

inspection.

BOILING-HOUSE

EFFICIENCY

NUMBER.

309

The

efficiency
available,
in

number
it takes

is

of
into

value
account

in

calculating
the

sugar

actually

as

losses with
sugar

in

facture manu-

the
on

particular
whose work

factory
the

as

compared

those fotmula

in

the

factory
This

available 100 in

is

based.

number

may

exceed

some

cases.

GHEMIOAL

CONTROL

OF

SUGARrHOUSE

WORK.

188.

Introductory." The chemical

control of the factory

is intended

primarily to guide the manufacture best practice and to assist in detecting and
in the

along lines of reducing losses

of sugar. The chemist the

factory corresponds with the auditor in

accounting department. He charges the superintendent with the sucrose material entering the factory in the raw
and credits him with that and the
sucrose

losses.

leaving it in the products, byproducts, It is his duty to trace the travel of milling considers
the from its

and

locate losses. of the


cane

The

control

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 of
not

juice and
so

sucrose

to

the

engineer. The

engineer should
extracted reduction in

proportion of sugar that lost. The effort should as always be the of losses. It requires the assistance of the chemist
causes

much

consider

the

the locating The

of these losses.
sugar

of the crystallization The

should

receive

constant

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

attention.

large part of the crystallizer capacity for the low-purity massecuites. The be must crystallizers controlled the best conditions to meet of equipment and
a

reservation

of

manufacture. and

Molasses the

is often

sold

on

basis of its test,

in this event

control of the massecuites

becomes

of

additional The it upon


content sugar

importance.
of

quality
a

the

sugar

must

be

controlled

to

maintain moisture

basis of the most


must

profitable analysis. The


certain limits
to

be

kept within

protect the
310

from

deterioration

in storage.

INTRODUCTORY.

311

The

chemist is also the statistician of the factory. He

reports the quantity and

quality of the

raw

materials,the

and of analysis of the materials in process of manufacture the products and by-products. The chemist tistics staprepares that have
a

bearing upon
and

the

control

and

economy

of the manufacture Research Uie work


or

the business of the establishment. with the

in connection
processes

improvements

in

equipment

is often and

called for and


on training

this often the part

necessitates

both

technical

chemical

of the chemist. The future with

laboratory should
all the His

be

for part of the traiiiing-school chemist

superintendents. The

becomes

acquiunted
mani"

methods, problems and


control of the work

difficulties of the

facture. the

should

familiarize him

with

details of the processes. The chemist's tunately training unforlacks the opportunity for practice in directing and This of
must
come.

controlling labor.
leave the
a

to

him

before

he

can

acquire
A that their methods

must superintendent. He good .working knowledge of pan-boiling.

school

the

also

lesson

that

must

be be

samples
must

must must

early in factory control is representative of the materials and unquestionable. Apparatus


to the work
as required,

learned

integrity

be

and the

be

adapted
the

in hand. in the

Where

highest feasible
raw

accuracy

is

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 instead
appear

and

of apparent for sucrose, etc., but in routine control; necessary

this does not

usually

The from

weight

of

the and

cane

this number

reported to the chemist and the weight and analysis of the raw
mill-control
sucrose

is

juice extracted he calculates the the weight of the engineer and

numbers
to

for the in

chargeable
for this The mill

superintendent. He must later the products, by-products and


depoids
very

aecount

sucrose

losses.

control

the analysisof the bagasse, and largely upon this analysis. in some upon cases, entirely in the control of the The juice is the starting-pcnnt raw also elementsof Its weight and analysis manufacture. are

312

CHEMICAL

CONTROL

OF

SUGAR-HOUSE

WORK.

extracted weight of the sucrose juice plus that remaining in the bagasse is the baas determination of the percentage and weight of sucrose The in the
caaie

the mill control.

in the
of

the

ing entertion. extrac-

and

for the calculation

of the

sucrose

The

analysis of the sirup


of the

or

concentrated

cane-

juice,the
the
trol con-

"meladura" of the

is Spanish-American factories,

of the juice and its evaporation, and purification 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
.

Careful specifiedpuritiesby the injectionof molasses. control of this work is essential to a systeiratic grading of
to

the materials

for

the most limitations

extraction profitable of the

of the sugar,

tests factory. Control also often are required in the conduct of the crystallizers. The controlled both as products, sugar and molasses, are
a

considering the

check

upon

the

manufacture

and

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 solids
must

be

determined

for

loss

of

sucrose

may

occur

through
A

entrainment

in the of the is

multiple-effectsand
temperatures
In the of the

vacuum-pans.

knowledge

condensing and

condenser-waters

required in estimating this loss (313). opinion of the author, many


manufacture
are

of the so-called mechanical actual inherent

losses in

not

losses, but
in certain

are

apparently
the processes

so

through inaccuracies
of

of

analysis.
can

Except in very large factories,which force of chemists, a complete chemical


The the
the

afford

sufficient
ticable. prac-

contlrol is not the

chemist

must

judge

from

be omitted factory what work may of the sugar-house. He must under all conditions efficiency he detei^nine when properly, to some degree, may

equipment of without decreasing

WEIGHTS

AND

MEASURES.

313

sacrifice accuracy for the sake of figuresfor immediate use. It is

promptly obtaining approximate


ical large factory, that the chemthe laboratory records well

just
as

as

important,
the accounts

in

control

be that

cctaiplete and

arranged
full and

of the various

departments

be

accimtte.

WEIGHTS

AND

MEASURES.

189.

General
"

Considerations

in

regard
all
or

to

Weiglits
to

and
measures same

Measures. should

It is quite essential that


be of the
same

weights and
the

system

be

reduced

system. America, where


units The used

This

remark
not

it is

applies especiallyiii Spanish unusual to find English and Spanish

indescriminately.
be adopted ^ould weights and measures accuratelyas possible. A checking-system should the conditions of the factory and in so to meet eliminate in the calculations be possible errors of

system

applied as
be far devised
as

190.
not.

may Cane

Weights."
cane,

There

are

few

factories

that
even

do
a

weigh their
of
a

especially among
control. Cane of the in

those

making

pretense
are

chemical
to

weights, however,
in
a

not

essentia
may

the control

boiling-house,and
mill control. In

measure

be

dispensed
the

with

this

event

the

mill

control

depends juices.
to
use

entirely upon
the

the

analysis

of the

bagasse and
in Cuba.

It is the
cane

general custom
These The
is ton
some

Spanish pound in weighing reported in arrobas


contains
on

weights

are

of

25

pounds, Sp.
to

{tondada)
confusion the

2000

pounds

(libras) Sp.
makers the
as

There the

the

part of scaleA decree of

equivalence of
are

Spanish pound, though


a as

leading scales Spanish

properly graduated.
in Havana
gave

Spanish Captain General


100

the

equivalence

pounds
=

=46.0096

101 .4338 Spanish pounds graduated in Spanish pounds

100 kilograms, therefore avoirdupoispounds. Scale-beams


use

the word in most

"libra." factories
to

It is the the This


cane
on

custom
a

in Cuba scale

and

reweigh

central

inmiediately before

grinding it.

w^ght

i^ould

be used

in the control.

314

CHEMICAL

CONTROL

OF

SUGAR-HOUSE

WORK.

It

may

occur

the

chemist

through conditions that the weight of the

beyond
cane

the be

control

of

must

estimated

and Small the factories, 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
cane

is flumed

or

floated to the mills in water. for


an

These Such
cane

special conditions
methods should statistical purposes

call

inferential method.
in

only be
and

used
not

estimating the
serious

for the

in

the

control

of

factory.
constituent

Inferential methods
of

require a knowledge of
may

some

the

.cane

that

be

traced

through the

The following or solids, sucrose. millingprocess, e.g., the fiber, example, from the records of a factory, illustrates aji inferential method: Assume

juicewill
cane.

appliedto the analysisof the give approximately the percentage of sucrose


a

factor which

crusher in the fiber

This

factor the

varies with

the

variety of

cane,

the with

content

and

milling conditions.

It is smalls

light

than

heavy crushing. The factor approximates 0.85. with factors varying frozn a heavy crushing. Deerr ^ found
minimum of 0.81
to to
a

maximum
Pellet
may
*

of 0.848 the factor in


as

and

an

average

of

0.825. from

According
0.83
to

Egypt
in

is

usually
The

0.84 and

be
as

low
as

as

0.82 to 0.80.

writer has determined numbers

factors

low

0.80

Cuba, the low

being probably the result of the


the crusher:

very

large duty

requiredof
Factor

assumed
of the crusher extracted
cane

0.80
18
.

Polarization Tons Fiber


sucrose

juice
.

45

in the mixed

juice. .305.7
11.3 48.9 9= 23.11 4.5 14.76

test) (direct Fiber in the bagasse (direct test)


in the

Bagasse
Sucrose Sucrose Sucrose

per

cent

cane

11. 3X100-5-48. cent


=

in the

bagasse, per

in the cane, per cent 18.45X0.80= in the bagasse per cent cane =23.11

X0.045=

1.04
M^

I *

Int.

Sugar

Journ.,

Int. Sugar

1911, 13, 15. Journ., 1912, 14, 587.

316

CHEMICAL

CONTROL

OF

SUGAR-HOUSE

WORK.

free overflow 3-inch The ''T"

for the is
a

juice,without
should be

interference by
calibrated
must

foam.

suitable size. with


water
to

measuring-tanks
;

under

service

conditions. volume

Corrections

be

applied

the measured for

for temperature, with the

milk of lime added

and

air entrained determined

shouldbe
and
,

for air juice. The allowance experimentally. It varies with milling A tank should be be filled to After the
a

pumping
with

conditions.

overflow
few

juice and

its temperature and

noted.

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
.

hours

the temperature

to

entrainment

of air.

The

method is

of
on

the weight calculating


page

of the

juicefrom its volume


factories
are

given
to

347. the

Many
block which
of

compelled
be

measure

juice in the
to

defecators. wood

Such

measurement

is

very to

unsatisfactory.A
must

should

arranged

indicate the point


be made

tjbevessel is to be filled.
of lime the
use

Correction

for

the milk
to

and

for temperature.

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 surface with them. a part of the precipitated impuritiesto jihe This, scum adds of making to the difficulty an accurate heat
rreasurement.

The

calculations

are

made

as

given

on

page

347. ii is tank allow

quite

usual practice in Louisiana, whsre


used for the defecation and

is often the

a'.ngle to clarification,
a

in the troughs some time in to remain skinmiings. with them; this order tQ separate the clear juice entrained into the defecator back and drawn clear juice is finally of its volume. The account no being taken recladified, Yolvune of such juice should be determined, and average.

deducted
soon

calculatingthe net learn that.it is only by


in
can

volume.
.

The
care

chemist and

will

extreme

vigilance

that

he"

succeed

under

these

conditions

in obtaining

MEASUREMENT

OP

THE

JUICE.

317

i'easonably accurate
to

measurements

and

samples.

In

tion addi-

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
sources
error

the

of

tanks. When
to

large tanks are used as in these processes it is well which provide a printed sheet for each liming-tank, on
workman when used. should
note

the and lime

the

time

when

he

begins filling
of milk of the ascertain

he finishes With

and the volume filling a tank data the chemist


can

these

number record
account of the

of tanks

filled with

juice,whether
correction of lime.
to

the be

workman's

is correct, and of the volume

also the

applied

on

of the milk

The

temperatiu'e

juiceshould

also be

noted. occasionally
"

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, belt strainers and now so generally used.
AiUomatic Measurement

thorough straining facilitates the measurement juice,though it will not usually admit of the use of
This The cold
sources

of the
meters.

automatic

or

semi-automatic the

measurement

of

the

juice,as it flows from


of
error

indicated
measurement

for such One


meand

eliminates mai^y mills,, o^ the in the preening paragraph. Apparatus of the juiceis but httle used. " of measurement
an

of of
a

thi^most
as

reliable methods of tanks described and

combination that

automatic
on

by recording
illustrated

is

apparatus such in Fig. 86. This

farther

and

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

CONTROL

OP

SUGAH-HODSE

WOBK.

tank.
exact

colored

float in the

gauge-tube facilitates noting the


is
more

measurement.

This
of for
more an

reliable
float.

than
Several

the

urement meas-

by
have
been

means

ordinary
the
accurate

methods

devised

raeasurenient
a

of

the

but diffusion-juice, the

espedally
drawing
too

with much

view
or

to

preventing
little juice.

batteryman

from

too

Pta.

sa.

The

method

suggested above,
below,
is
in take

together mth
one a

the

automatic convenient.

register
The The very

described

of

the

moat

workmen automatic

pride
The

record-sheet

free

of

errors.

registration of tlie amount by


of direct

erf juice is of
from

great importance.
or

weight of the juice derived


ia the baas
accurate

its volume,

weighing,
the

of

neariy
edge knowlin

ftll calculations of the


errors

sugaf-house
of
in

losses.

An

volume and

juice

is of

cspedal
and occasion

value

locating

preventing

undue

tion. irregular dilu-

Irregularitiesof dilution
sugar,

not

only
The in of

losses

ol

but of

mcrease

the cost

of fuel.

automatic

ratus appa-

Horsin-D6on,
of

illustrated the rate


a

lilg.86, drawing

registers the
and

amount

juice drawn, and essentially of


A of
a

all delays.

It

consists

recording cylmder revolved


meaSuring-tank
with
a

by

clockwork.
oy
means

float vrire

in
or

the chain

is which

connected revolves

drum,

WEIGHT

OF

THE

SIRUP.

319

when

the

float rises

pinion, which
turn

is a falls; on the shaft of the dnun in revolving engages a rack; this latter in
or

is attached the and


on

to

small

arm,

which float

carries

pendL
the

When

juice'enters the tank by


the
reason

the and

revolves lifts,

drum,
a

of the

rack

pinion the penciltraces


The
paper

line
12

paper-coveredcylinder.
to

is divided

into each

parts, corresponding
into

the

hours

of two

watches;^

part is subdivided
once

5-minute hours. in

revolves
instrument should The be

every may

twelve
used

The cylinder spaces. It is obvious that this


"

also be
to
a

mill-work, in which

case

it

attached

suitable measuring-tank.
"

Weight of the Juice.


its volume for

In

the
be

juice from
corrected

and
to

calculating the weight of should density, the volume

correspond with conditions of the graduation of the hydrometer. In using the Brix which are graduated to give the density of the spindles, solution at 17)^ C. as compared with water at this t^npera*
ture, the volimie
The of the cubic

expansion

juice should be corrected


foot of water and lbs.,
at

to

171" C.
ture, temperaStates

weight

of

the normal of the

17J**C, is 62.2795

that
per

United

gallon,of whibh
These numbers

there
may

are

7.4805

be used

foot,is 8.3255 lbs. in calculatingthe weight of the


A

cubic

juice under
If the

the

above

conditions.

table

is

given

to

facilitate these calculations

hydrometers

are

(page 495). graduated

to

the

temperature

standard

adopted by the International Chemical Congress, The the volume to 4" C. of the juice should be corrected
a

weight of
193.

cubic foot of water


and for

at 4"

C. is 62.3565 of the

lbs.

Measurement used

Weight

Sirup.

"

The

methods

of the

sirup is not

juice apply with sirup. The usually required,except in taking


in process. Deerr
uses

weight
account

of the stock of the material of

the

weight

the available sugar.' calculating 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
"
' " '

sirup in his method

"

^The
ftre
*

iniervals between
"

the

hours

to

12

a.m.,

12

to

p.u.,

etc.,

termed

watches."

Bui. 41. Hawaiian

Sugar Planters'

Expt. Sta.

320

CHEMICAL

CONTROL

OF

SUGAR-HOUSE

WORK.

This

makes

accurate

routine

measurement

difficult

if

feasible. The

sirup miist

be

measured occasionally for the


run

in

taking

account

of the sugar

this purpose the tanks should be gauged iEtndthe volume per inch of depth In these measurements it is more convenient be tabulated.

in process

reports.

For

to note

the "inches

out"

and

figurethe sirup in the tank Weight


of the
or

by

difference.
194.

Measurement

and

Massecuites.

"It with

is difficult to the

factories. direct be

weigh a massecuite methods of manufacture prevailing in modem is discharged into the massecuite When cars,
may

accuratelymeasure

weighing
in the
in

be

resorted

to, but
cars.

special care
The
extra

must

observed

taring the

empty

labor

involved

in securing weighing, and the difficulty in most satisfactorylaborers, usually prevent this work factories. It is also
when

impracticable to accuratelymeasure it is discharged directly into the


into

the

cuite masse-

centrifugal

mixers

or

weight
The

can

Under these conditions the crystallizers. only be calculated approximately. (See page 345.)

measurements

in

the

mixer

and

especially in
after

the

should be made crystallizers immediately on massecuite,on account of its increase in volume


or

striking the
stirring

further The

crystallization.
or

measurement

weight of the
of
"

massecuite

is

usually

only required
the

at the end

run"

or

period for calculating

In very quantity of sugar in process of manufacture. in these when measurements, large factories the errors of made, are so small as compared with the amount carefully be neglected. in process that they may material A

sample of
for

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
time^xheck
per the may
are

package
scales

weighing of the sugar, since a small error Automatic appreciably affect his calculations.
coming
i.e.,
into extensive sugar.
use

in

weighing

dry white

sugar,

granulated

An

empty

ba^

SUGAR-WEIGHTS.

321-

forms

part of the
and does
very

when counterpoise,
away

using this
allowance

class of
tare.

packages,
These

with

other

for

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
mechanical
losses. automatic scales
are now

scales

give

reliable

Dependable
These the
use a

made

for

raw

sug^.

mechanical into the

arrangement

to regulate the flow of to

sugar

weighing-hopper and quantity. One


more

adjust the

''dribble'' will
raw

or

last small

type of these scales

accurately weigh
sugar per

than method

80

hour. loss.''

This

bags of 325 lbs. of the of weighing reduces


and the "Libra" scales

''undetermined
are

Richardson's

in
195a.

use

in Cuba.

Measurement
of the molasses

of the is

Molasses.

"

^The

urement meas-

accompanied

ing by difficulties arisMolasses is very

from viscous

the nature and drains

of the material
very

itself.

slowly from
in
a

the containers, making


uncertain.

successive

measurement

tank

Further,
This of the

heavy

molasses

occludes

considerable quantitiesof air.


the

occlusion commercial
Molasses
to

of air raises

question of
reduced with

definition

gallon of final molasses.


that has been
water

preparatory
Final molasses
account

is readilymeasured reboiling be

in the tanks. when

should its is

weighed in tank-cars
in the
498 page

possible, on
A

of

importance
on

factory control.
for the measurement

"wantage

table" in of

given

of the molasses
amount

horizontal
air occluded it and the

cylindricaltanks
varies with that the

(tank-cars). The

filling period measuring. molasses weighed less than In an experiment by the writer, a 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 is the most for molasses stored in float, satisfactory copper very large tanks. elapsesbetween
and filling

container,the method

of

322

CHEMICAL

CONTROL

OF

SUGAR-HOUSE

WORK.

MILL

EXTRACTION.

quantity of juice or sugar removed from the cane by the mills,the mill extraction,is (1) The weight percentage usuallyexpressed in two ways, viz., 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. Extraction.
"

Mill

The

only to the fact that it directly it is less indicates the sucrose but also because extraction, influenced by the variations in the composition of the cane. the direct analysis This number was formerly based upon
ewes

its

increasinguse

not

of the

cane

or

upon

sucrose

number

derived
cane

in the incorrect is of uniform

assumption that the juiceas it exists in the composition.


(1) Extraction
Juice. the
"

in

Weight Terms

of the Cane
or

and

Normal

Divide

the

weight of
and

diluted

mixed

juice (169) by
to
tain ascer-

weight of the
the per cent

cane

point off for percentage,

cent

cane

dilute extraction ; calculate the dilution per from the dilute (1H)7) and subtract this number number.
cent in

extraction normal

The
cane.

remainder

is

the

extraction

of

juiceper
and

(2) Extraction
in the Cane
sucrose

PercentageTerms
Juice.
"

of the Weights of Sucrose


Calculate the

the Extracted

weights of

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
saturation-water. extracted the
cane.

in the diluted

in the weights of sucrose in juice and the bagasse is the weight of sucrose The weight of sucrose in the extracted juicedivided
sum

The

of the

by that in the
extraction the extracted

cane

and

the

quotient multipliedby 100 is the


of the
sucrose

number

in terms

in the

cane

and

in

juice.
in

(3) Extraction
calculations
water
are

without Saturation. Dry Milling^i.e.,

"

The
no

similar to those of (1) and be considered. of

(2) except that

of dilution need

methods Example illustrating

the extraction: calculating

324

CHiaMCAL

CONTROL

OP

SUGAR-HOUSE

WORK.

times mills:

used

in

supplying information
per cent
cane
=

for

adjusting

the

(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
from mill to miU. Saturation.
water

Juice extracted

198.

Maceration.

Imbibition.

"

^The

quantity of
be
measurement.

used in saturatingthe
estimation of the water

bagasse can
or

only
made

determined

with An

certaintyby weighing

by
in

accurate

is sometimes

by
the
open
cane.

an

inferential method
cane.

similar to that used

estimating
are

weight of the
to the
same

Inferential m^^thods for the water

those for the weight of the as objections be

The
on

water
cane over

should

actuallyweighed and its percentage


or

the

calculated
to

it should

be

measured

and

culated cal-

weight. The
cane.

percentage should be in terms

of the The in Java The

weight of the
and

dilution in terms the Hawaiian

of the normal

juiceis used largely


cane

Islands to indicate the saturation.


on

percentage of water
per cent

the

weight of the

is also used

in Hawaii. Saturation the


cane
cane
=

weight of the
=

waters-

weight of

XIOO.
per
cent

juice (Brix of normal juice" Brix of diluted juice) -s-Brix of diluted juice XIOO. There confusion is much in the sugar-chemists 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 be evaporated on the total juice, that must account actually
"

Dilution

normal

of the

use

of saturation.

For

the

saturation-water,
the is suggested.

as

culated cal-

from *'Per cent

its weight and that of the cane,


or

saturation"

''maceration"

expression Sugar-

house reports, in

the quantity of water used,should indicating ''Percent dilution" and. "Per employ both the expressions
cent

saturation."

CONTROL

OF

THE

SUGAR-BOILING.

325

CONTROL

OF

THE

SUGAR-BOILING.

109.

Control

of Vacuum-pans
vacuum-pans of moderate and

and

Crystallizers.
"

The

control of the

requires crystallizers
in the

work rapid analytical The

accuracy.

analysis of
or

the the

sirup

as

made the the

daily routine
be drawn

work,

in its stead

of analysis

juice,and that of the


latter to of the desired

molasses into If
a

indicate the
pan
to

quantity
a

of

the
cut

produce
be

massecuite

purity.
cuite masse-

strike is to that for of

boiled,the purity of ihe above


molasses
to

and the data

the

be

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-

calculatingthe

for the purpose: accuracy Let 100=total weight of massecuite

in the
case

strike;
of
a

F="

purity of the sirup,or, in the


that
of the

cut

strike,

massecuite
be

left in the

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
"=

100

*-x=

percent age of the strike


or

to

be derived

from

sirup

from

previous boiling;

100
"*" ^"^
r

(P-M)
i"
"

"

V
a

The of
a

of the materials used in making proportions


certain

mixture

diagram
to base

also be quickly calculated by the purity may It is not feasible in pan-work method, page 347.
on

the calculations

actual

weights. The

approximate
the
lasses mo-

densities of the massecuite


to be boiled in

for example, and footing, should,however, be considered. massecuite should be

brought to the laboratory immediately the strike is dropped. A portion of


this should be dissolved in water
15" A
to form
a

sample of the mixed

solution

of about

Brix,'and
second
and

its apparent portion should be


the

purity should be determined. fugal purged in a laboratory centribe

purity of the molasses


in this

determined

as

above. If

dry lead defecation is used

work, the labor

of

326

CHEMICAL

CONTROL

OP

SUGAR-HOUSE

WORK.

the apparent coefficient of purity may calculating 526. table, by the use of Home's page

be avoided

FiQ. 87.

The

puritydata

of the massecuites and

molassed samples be should to- the promptly sent superintendent and the pan-boiler. All mixed strikes, especiaUy those
of the lowest

purity, should

be

controlled

in this way. The relation the between purity of the and the the molaisses

massecuite from it in

purged

diately laboratory,immeis a valuable after boiling, guide in boiling low-purity mixed strikes.
are centrifugals in Fig. 87, and shown a filtering Thi" filt^* is indevice in Fig. 88. expensive

Convenient

and
a

very

efficient. It is

funnel,' sparable at the ing. ground joint,A, to facilitate cleancopper

surface is of filtering oentrifugal lining-sieve having about


625
Pjq gg

The

round sieve

holes
must

per

square

inch.

The braces.

be

TJie funnel

is used

in connection

supported by with a vaeuum-

INVERSION.

327

filtering flask
with the
vacuum

or

and bell-glass

plate. factory.

Connection

is made

system
this method

of

the

Very

often

of control poor.
When

will indica^^^e whether


a

the

pap-boiling
yields
indicates
pans,
a

is

good

or

low-purity massecuite

immediate purging, it high-purity molasses, on boiling. A few days' experience with the poor work the with these

following the
indicate the whether
pans
"

control-tesJls, will

usually
best
200*

results

and In

sugar-boilersare obtaining the material are capable of yielding.


the
manufacture
a

Inversion. the
cane,

of
sucrose

white due
to

sugar

from

there varies

is often with in

loss of

inverraw-

sion, and
sugar

which

the acidity of the juice.


the of
event

In

factories,except
inversion
to to

of serious since

delays, there
the

is

little if any

the The

sucrose, alkaline

juice is gradu-

limed

neutrality
to

phenol.
is caused
adds

condition

aUy
less and

changes

neutrality in the storage-tanks.


sucrose

Inversion

of

by all acids, to
inverting with

greater
all.

or

degree, the
some

mineral
weaker

great rapidity

of the

organic acids
salts of invertive in

scarcely at
action
on

Many
the

inorganic salts and latter feebly, exercise an


alone in the will invert
presence
sucrose

organic acids, though


sucrose. more

Heat

water-solution, but invert-sugar,* is


viz.
:

rapidly
The of ulose. These

of

air.
posed com-

product
The
sugars

of

the
of

inversion,
two sugars,

equal parts

dextrose

and in page in

lev56.

properties of
are

these

sugars

are

given
and

acted levulose

upon

by the
is very
of

lime

heat

the The

defecation,

and

is often

in part

decomposed.'
in the
to
no

decomposition
defecation and

of this sugar

noticeable the there

alkaline the

the

dark

color Provided

juice is due
has been

composit de-

products.
of the
sucrose

position decomto

glucose,a comparison
of the inversion has

of the ratio of the

glucose
not.

juices,etc. under

examination,
taken

wiU
or

usually
The

indicate

whether

place
and

"

In cane-sugar
in the

manufacture, Juice and

the

invert-sugar
are

other

reducing

stances subfor

products

usually

called

gittCose, and

brevity

this expression is used

in this book.

828

CHEMICAL

CONTROL

OF

SUGAR-HOUSE

WORK.

difference inversion From

between

the in
a

glucose ratios is

not

measure
"

of

except
the above

general

way.

renoiarks,it is evident
cannot

that

loss of and

sucrose

through inversion
from in the the

always
and losses

be

detected
sucrose

estimated

percentages
raw

and

quantities of products.
will
not

and

materials

It

can

glucose usually be
one

detected,
another.
In

however,

as

often

balance

using the followingformulae,for the calculation


the above considerations in
the

of inversion,

should

be
^

kept in view:
etc.
"

Sucrose

inverted

evaporation
of

The

inversion,
by
the of the

except

in

the

diffusion-battery,may
formula Dr. Station: unit unit unit unit of
of

be

calculated

following extended
Louisiana Let
a
=

William

Stubbs

Experiment
sucrose

per

juice;
juice; sirup sirup
or or

6=
c=*

glucose per
sucrose

per

of
of of

massecuite, etc.; massecuite, etb.;

rf^

glucose per
total

^=the Let

weight

juice (nounds);
in the
sugars

total

sucrose

removed

and

by by

losses

gf=

(pounds); total glucose removed (pounds) ;

in the

sugars

and

losses

a;i= total inversion; in concentration a;2=loss


^

of the

juice to

sirup

or

1st

massecuite;
afj" loss in concentration

of the

juice to massecuite.

_^^E(ad-ch) -\-cg-ds]
^^^
""''

100c

+ 95d

(2) When
concentration reduces
to

neither
of

sucrose

nor

glucose is removed,
1st
'

as

in the

to sirup or jiiice

massecuite, the formula

95^(arf-c")
"2
=
'

100c

+ 95d

INVERSION.

329
in the sugars,

(3) When
and the

there is

no

glucose removed
to

^"0,

formula

reduces

9^E(ad-ch)-d8]
^'"^ 100c + 95d

The B.

following generalformulae
U.S.N.,
"

for inversion of

by Lieut.
Dr.

A.

Clements,
:
" '

are

modifications

Stubbs'

formula

"

"

(1)

af=sucrose

inverted

per

cent

sucrose

in the original

juice;
"S=
sucrose sucrose

removed in the

in

sugars

and

by losses

per

cent

original juice;
in sugars and

i7=

glucose removed
sucrose
in

by

losses per

cent

the original juice;


cent
sucro"e

rj"per

-f- per glucose in the juice the juice X 100;

cent

in

r2=per

cent

glucose in

the

massecuite

or

molasses,

etc., -5-per cent

sucrose

in ditto X 100.

^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; rz-Vr+g-rJS
x=^a-

cent

of

10000 95

(3) Calculation
re
=

of inversion

in terms

of the

glucose:
cent

inversion

per

cent

juice;
in the
-5- per juice

/^i*=percent
in

sucrose

glucose

ditto;
cent
sucrose

^,=per
4-

in

the

sirup

or

massecuite, etc.,
etc., per unit of

per

cent

glucose in ditto;
sugars,

in the removed "S3=sucrose glucose in the juice;

330

CHEMICAL

CONTROL

OF

SUGAR-HOUSE

WORK.

"7ji=glucoaeremoved 6"glucose
cent

in the

sugars,

etc., per

unit

of

glucose in the juice;


per

juice.

Xf^b

100^

100 1.05263.
95 901.

Formulae

for

the

Calculation

of

Inversion

in

the

Diffusion-battery.^
pe" per
cent cent cent cent cent
sucrose

in the

diflfusion-juice
'

glucose in the diffusion-juice


sucrose

"

per per

in the
in the

normal normal

juice juice
'

glucose

6= x=b

per

glucose in the diffusion juice;


=inversion in the

"

~7~"
"

battery

per

cent

1+

95

Fjj '

diffusion-juice. (2)
a=per
per
r
=
'

cent

sucrose

in the
in the

diffusion-juice;
diffusion-juice
X 100
'

cent cent cent cent

glucose
^ sucrose

'

per
per

in the
in the
7"7 m

diffusion-juice
normal
normal

'

-^

glucose
sucrose

r2=per

p^-T-XlOO;
the

juice

"

juice

x=a

"

!"^=

in version

in

the

battery

per

cent

Jiffusion-juice.
(3) [p" (100" e)P].9j"xe=in version
in the

battery
in
-r-

cent per-

diffusion-juice. p=per glucose juice; P""per cent


*" Fonnulas

cent

glucose
normal
Dr.

diffusion

in

the

juice
Stubbs*

100;

(1) and

(2)

are

baaed

upon

formula.

332

CHEMICAL

CONTROL

OF

SUGAR-HOUSE

WORK.

of

apparatus, conveniently arranged


at

for

noting the

ments measure-

the

stations.

If the

factory day
an ass.

chemist,
with
go

sample

cups

midnight, for example, the and the laboratory helper, provided '^^ant, and a measuring-rule, should at that time
ends
at

through systematically juice, .etc., and


various

the the

factory drawing samples measuring the quantity of material


the
of

of
at

stages
the

manufacture. end

This with
even

stock-taking
sugar, sugar in

should
must

begin with
include

juice and

the the

and the

all material

in process,

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
average accuracy.

composition
If the each from
must

of
are

the

sirup with

fair

degree

of

tanks

of different

sizes,the

quantity
be

drawn The

be varied the

(volume and
to

of

juice in
be
when

accordingly. multiple effects should


a

estimated
from
run

may

considered
the

constant

quantity
use.

run, the

apparatus
may

is in

The when

material

in

multiple effect
tanks the the time
.

be

measured

liquidated into
with of
water at

or

the

apparatus
of

may
season.

be calibrated The

beginning
vessels
to time

the the
a

density
be

the

sirup in
from

of
as

evaporator

should

ascertained
sugar

guide in calculating the


certain tanks of boiler, be omitted
as

value.

By prcfarrangement sirup (meladura) and


the stock and be used Thus in the pans. until the

with

the sugar
may

molasses
to

such

from

complete strikes of massecuite


massecuites need if
not

then

these the

be

measured

they reach
and

or crystallizers

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

molasses

be

BUN

REPOBTS.

333

ugals,hoppers and bins should be noted,ftlsothe last serial


package number. Stock-taking in
if the above
as

largefactory need require but


be followed. the stock taken The
were

few
are

utes mintically prac-

scheme
as

results

accurate

during a shut-down.
a

When the known


or cane a

the of

run

report is called for


may

to include

certain

date,
it be

work

stock-taking
the

be

should facilitated^
a

factory will be shut down day later for cleaning or other reason.
that

day in advance
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
follows: Juice and

Sirup.
"

Since of

the

raw

juicehas

of manufacture be The with

ahead from

estimated

its commercial it, the previous experience of the factory. method


on given.

all the processes sugar value should

available sugar
an

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 loss in manufacture. These remarks

apply

more run

especially to figures are


the

the first run

of the

factory,after which
there is

the

more

accurate, and

further

experience in

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.


and the
as

Massecuites boiled
may

Sugars.
"

^If the of
cases

massecuite

has

been value

without be

addition in the

molasses, its sugar


of the

calculat"ed

juice and

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 from

obtained B

(sugar-value)to be the massecuite;


sugar

""degree Brix of the massecuite;

334

CHEMICAL

CONTROL

OF

SUGAR-HOUSE

WORK.

Let

P"
p=

of the massecuite; polarization


of the commercial polarization
w

sugar; sugar;

fiolidsper unit of the commercial

M
Then

of purity of the final molasses. ssooefficient lOOP-BM


x
=
.

p-SM
V

This

formttla

gives

accurate

results

only

when

the

true

true polarization,

of the estimates

For the purposes it is usuallysufficiently the to use accurate With

Brix and

purity are

used.

apparent
the
at the

etc. polarization,

calculated

results differ but

little from

low-purity massecuites, the actual yield


the

centrifugals.
noted

It will be used the in these

that

the

purity of
gra-de of

final molasses
as

is

estimates. If but
a

This
one

is advisable
sugar

it

simplifies
the

calculations. is

is made,

calculation

simply

substitution
one

of values

in the formula. and

If,however,

more

than

grade is made,
in what

e.g., 96"^ugar

2ds, it is necessary proportions these sugars and made, allotingits proportion to the 96" test sugar are

to know

reducing the remainder In reporting estimates


in addition and
as

to

terms

of the

second

sugar

for the the

to

period or run, it is customary general statistics of the manufacture


to

the

data, analytical

report the

yield of

sugar

follows:
1st sugar
tyj
tt

per
tt

cent
It

of the
It tl

cane.
t(

Total

"

*'

"

"

''

"

1st sugar,
t\J
it

sucrose
H

retained
H

per
ii

cent
It

of
tl

sucrose
tt

in the
tt tt

juice.
tt

Total

*'

*'

"

"

tt

tt

tt

tt

tl

"(

The

sugar

is also
per
it

Ist sugar
nj It

cent
tt

occasionally reported as follows: of sucrose in the juice.


tt tt

^"

f*
*'

""

Total This since the


in

"

"

"

"

**

''

"

is not
order

very be

to

satisfactorystatement comparable with those


to
,

of of

the other

yield,
runs same

figuresmust polarization.
The
statement

be
'

reduced

terms

of sugars

of the

giving the

sucrose

retained in the

conuner-

^
LOSSES OP SUGAR IN THE

MANUFACTtTRE.

335

in the juioe"6ho\vBat a cial sugar per ceht of the sucrose glance, in comparisons, the relative quality of the woric. This form of statement
"

Final
distance
to
waste

molassea, from and

is in very generaluse. In msaiy factories that are

located at
are

favorable the

markets, the final molasses

run

material

pumped
from

this only oheok the chemist has upon Where the molasses is his analytical work. is into lai^ge tanks, from which shipments are made
to

time

time, data
may

of the

total volume

and

average

composition
secure

often for

be

obt^ned.

It is often diflBcultto

this product accurately distributing 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 entirely empty of In the Manufaeture. Losses ^The 203. Sugar information
"

cake, and bagasse,filter-press in the evaporation. through decomposition and entrainment Other sources are by inversion, fermentation,and possible
sources are

usual

of loss

in the

the

so-called mechanical
The
"

or

undetermined

losses.

the

bagasse. ^The loss in the bagasse is calculated from estimated weight of the material and its analysis.

The

weight of the bagasse is


between
the

often

estimated

as

the

ference dif-

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
case

third mill heavier than


if the

it would

be otherwise.

In

this

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
not

known. Fiber
per

In
per

this event
cent
cane.

an

inferential method

mu^t

be

used.
B

cane

XlOO-^ The

bagasse

cent

fiber per cent bagasse uncertain quantity in this


cane.

calculation is the percentage of fiber in the

336

CHEMICAL

CONTROL

OF

BUQAB-HOUSE

WORK.

Cake, FUter-press
the

"

^The loss of

sucrose

is calculated

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
to

time

to

obtain

an

average

weight and

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
cu.

ft. is
a

There filt^

loss of This is

sucrose

in the

juice absorbed
with the

by
unknown

the

cloth. This

usually included

losses.

It will vary
to 0.6 lb.
or
"

methods. quantity varies with the filter-press from almost nothing with double filter-pressing
more

per

filtercloth.
may

Inversion.
on

Inversion

be

estimated

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
page

327, provided no

is 86 per

cent

of its content massecuite 0.5 per


cent

of solid matter the

evaporation to
indicates
or

purity

is sucrose; falls to 84.5. has been


to

after This stroyed debe


a

that

of its solid matter


assumes

inverted.

This

the solid matter

constant.

Glucose

is

usually destroyed
when actual be obtained
as
a sucrose

to
or

some

extent

in the

facture, manu-

therefore materials balance losses.


as can

well

weights of the it is preferable to figurea glucose balance to obtain light on the

calculated

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 of the page 349.) the ash and beaker in the and soluble

throughout the manufacture. {Se^ the the determines He sucrose by Clerget method
salts
as

sulphated ash. He transfers the with ammonium the lime,etc., precipitates


of

ash

to

oxalate soluble

presence

ammonia,

then

washes

out

the

and determines sulphates left in the precipitate

their

quantity

"^Int.Sugar

Journ., 1914, 16, 383.

TEST

BOOKS

AND

RECORDS.

337

by- difference.
Zimmermann's

The

calculations

are

illustrated by

one

of

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
= s=

unit
cent

of loss

sulphates. Then
on sucrose

33.87

0.32

"

100

:x"0.94,

per

juice. This is evidently a very exaggerated example. The soluble sulphates are much higher than the usual total ash and the
loss is excessive. this class of This

in the

method

is

quoted

to call attention

to

investigations.
"

ErUraininent.

^The loss

by entrainment

may

be estimated

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 AND FACTORT
RECORDS.

204.
a

Test

Books and

and forms

Records. without

"

It is difficult to

plan

set of books

knowing something of the

needs

of the owners, the force of chemists available for con^ trol and whether this control is to be partial or fairly complete.

slip for the Manager, Superintendent and Engineer, giving preliminary data of the the output of mill work and control analyses of the juices,
(1)
A sugar

The

usual

reports include:

and

the fuel

consumption;

this should

by frequent reports to the Engineer on (2) The preliminary report should bagasse.
what include the
may

supplemented the analysis of the


be followed

be

by
and

be

termed

an

which ''operatingreport,''

should

data

covering the entire line of chemical


This should include mill and

control

manufacture. statistics.

ing manufactur-

(3) Run

reports at stated
both and
a

intervals, giving a
run

r^sum6

of all data
a sucrose

collected balance

for the

including
losses.

statement

date, of yield and


to

and

The

data

shot^idbe
and

full

enough
owners

to

indicate
a

the

methods

of manufacture

supply the

permanent

338

CHEMICAL

CONTROL

OF

SUQAR-HOUSE

WORK.

record

of methods. indicate

Working and
what

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

calculating weighted
Printed forms

averages.

should

be A

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 be used each is convenient for these forms
on

routine

work. laboratory

and

sheet

should
or

day.
and
never

All

should be figuring
scraps

the sheets

in

books special

on

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
to

It is advisable

have

of paper. forms for calculatingand

should General

be

tabulated

from

time

to

time

for the

use

of the

Manager and the Chief Engineer. The daily laboratory reports, for a fairly complete 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 polarization the storage qualities must meet market requirements; the ash is an additional check upon the of the juice. (6) Analysis of the final m"^as8es purification
to

meet

ma[rket

conditions

and

to

control

lizers and
to at

centrifugals. (7) Analysis


the loss of sugar.

the pans, crystalof the filter-press cake

control

(8) Analyses of the

bagasse

and sucrose frequent intervals, indudmg moisture, fiber, (9) Frequ^it examination tests, for mill control. of the the for feed-water for sugar, protection of the boilers. (10)
tests in the condenser

Entrainment

water, to protect against carelessness in the evaporationand in the pan-boiling.

SUGAR-HOUSE

CALCULATIONS.*

205. the

Introductory.
are

"

All materials

to be

dealt

with

by
the

composed of sucrose non-sucrose, latter including water, dextrose,levulose, organic non-sugars,

chemist

and

(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
and

by-products, is the
be calculated.

basis

for the

construction

of

with which algebraicequations, etc., may For

quantities,capacities, yields,

in addition the purposes of the usual calculations, to the proportions in which the various constituents are present, certain often
etc.

relations

between
as are

the

constituents

themselves

are

required, such
The

saline coefficient, purity coefficient,


very

constituent of a simple when the original material practicallyunchanged through passes the processes, e. (/.,the fiber in dry milling.

problems

illustrates the principles involved 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
means

percentage
an

of

this dilution
upon

is fact

ascertained that the

by
solids

of

equation

based

the

(Brix) of the extracted normal the diluted juice: m


Let
100
"

(undiluted) juice are

present

6== B"
a;
=

100"

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;)
*

and

a;

100-100fe/B
to

100(B-6)/B.

The

mark

"

"

is used

indicate

division.

340

DBT-MILLINO

FOBHTTLA/

341

This

is the usual dilution formula and is used because it is

the diluted
X

juicethat

is

weighed

or

measured.

The

value of

multiplied by the percentage of dilute juiceextracted from the cane gives the dilution in terms of the weight of the cane.
In
a

of the

similar way, calculations may the dry matter of the cane, of

be based

upon

the fiber
or a

press-cake,the ash
in sugar

constituent Since
are

it,etc.
of the numbers

many

ascertained

analysis

not

absolute,many
upon

of the results of
are

based

them

calculasugar-house tions approximations, but are usually of the

manufacturing These considerations apply especially contnd. to massecuites in whose molasses and be analysis absolute results cannot
expected.
The the full work of

accurate sufficiently

for the purposes

deducing

the formulflQ is
a

followingparagraphs, with
of formulae

view that

to
are

usuallygiven in the beginiier assisting


not

in the construction

given

or

that

are

necessitated
206.

conditions. by special

Dry-milling

Fonnula*"

The

fiber

or

marc

is the

constant: Let 100=

the

weight of the

cane;

B "the F=the F'


2=
s

weight of the bagasse from


percentage of the
marc marc

cane; in the cane;

100

percentage of

in the bagasse;

percentage of juiceextracted; (2) F'S-IOOF;


of J3 in whence

(1)

a;

100-B;

B"100F/F';

substituting the value


X
=

(1)

100

lOOF/F'

100(F'
and

F)ir.
that be for

The

similarityof this formula


(/S07) is noticeable.
the constant This
one

calculating

dilution
in the

should

e2q)ectedsince

(Brix) is diluted and in the other the its percentage relation constant (marc) is concentrated, i.e., increases. to the bagasse as compared with cane
307. Dilution FormulaB." The formula
or

for the dilution mixed

of the mill- juice in terms been

of the diluted To
.

juices has
this number
terms

given in the Introductory (205)


the

reduce

and

followingdilution number

to

percentage

of

342

SUGAI^-HOITSS

CALCULATIONS.

the of
X

weight of the

it vl necessary to multiply the values ively. respectby the percentages of diluted and normal juice, The dilution per cent normal or undiluted juice is
cane,
as

calculated
Let 100 B 6
X

follows: the

"

weight of normal

juice;

juice; the Brix of the diluted juice;


the

the Brix of the normal

percentage of dilution in

terms

of the normal

juice,
then

100+aj=*the

weight
100

of the diluted

and juice, found 100


=

sinc^

all

the solids

(Brix) of the normal


=

juiceare
=*

in the diluted

6(100+ar) juice,
This niunber

B and in

100

B/6-

100(5-6)
indicate

/6.
the

is used

certain

countries

to

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 These derived
Let

formulae in the 100 6 the

are same

similar
way:

to

those

for dilution

and

are

weight of the juice, etc.;


of the

the Brix Brix

juice;
water

B^the
X
=

of the concentrate;

the

percentage, by weight, of
whence

evaporated;

then

100!"
x=

(100-x)B,

100(5 -6)/B.
of

(5ee(311.)
is derived
as

The follows: Let

percentage

evaporation by voliune

100 h

the volume the Brix

of the

juice, etc.;
g

"

of the

juice of

specific gravity;
of G

B
X

"

the Brix of the concentrate the percentage,


=

specific gravity;

by volume, of
volume
of

water

evaporated;
evaporated.

then

GB(lOO-x) x=^lQO"gh/GBf

100^6, and
the
water

(See 312.)
200*

Commercial has
a

Sugar

Formulae."

(A)

This

mula forand

wide

application in the sugar-house control

COMMERCIAL

6U0AB

FORMULA.

313

in

the

estimation of the

required in crystallisers, capacities

etc. :

Let

x=the
p

percentage

yield

of

commercial

sugar
.

of

and S per cent dry matter; polarization 100=: the weight of the primary material (massecuite, and B per cent etc.)of P polarisation molasses,

dry
M=

matter

(Brix);

coefficient of
100
=

then

P"px/ B"Sx/

purity of the residual molasses; in the molasses; the weight of sucrose


weight of dry
matter

100

the

(Brix) in the

mdasses.

Since

the

coefficient of of
sucrose

purity of dry
matter

sugar
we

material

is the

percentage

in its

haye

B-Sx/lOO'
transposing and reducing, clearingof fractions,
lOOP-BM
X-

p-tiSM/100'
the sugar

yield of
of 100"

commercial

sugar.

If the is

product is refined
in

as polarisation/

customarily assumed
to

refinery work, the formula

reduces

^"*

'

100-M

(B) This

formula
from
terms

is

applicable in the calculation

of the

yield

of

sugar

percentages in
Let
X
=

massecuites,. molasses, etc.,and of the primary material.


sugar

gives

the percentage of commercial eoefiicient and 6 per cent of

of P'

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:

344
Then

0nQAR*HonsE

calculations.

BP/IQO
6x/100
1006a?

the
the

weight of

suorose

in the

material;

weight of dry
^^
.

matter

in the sugar;
"

_P'
X-t:^
=

P'bx the
10000
,^^^^, ,^ ^ of wei^t
.

^,

sucrose

the sugar;

100X100

100

B"bx/lQO^the
BP 100 P'hx
=

weight of solids in the mohisses;


the

weight of

sucrose

in the molasses.

10000

precedingsugar formula, an equation the coefficient of purity of the residual molasses


As in the

based

upon

is formed:

transposing and clearing of fractions,

reducing,

we

have

x^lOO P'-M the

X"

(C) This
moisture-free Let x^the

formula

has

same

applications as
way,

the

ceding. preupon

It is derived

in the

same

but

is based

materials:

percentage 3deld of anhydrous


the and
as

sugar

in terms

of

dry
in the the

matter

(Brix) ,in the 4"rimary material,


letters have the
same

let the other

meaning

previous formula
matter

(B),

Then

100

"

dry

(Brix)of the residual molasses;


P 100--M
"

P'a;-M(100-a;)-lOOP,
centage of anhydrous sugar primary material.
The

whence in terms

"

",

the

per-

of the

dry

matter

in the

above
sugar

fonnul"
from

may

be
cane

apphed in the calculation of the


or

yield of
take
a

the

but juice,

into account

the losses in manufacture

it is necessary to in order to make

correct

estimate^

The

''

available sugar'' formulse (185)

CRYSTALLIZEB

CAPACITY.

345

are

more

since they take the losses suitable for sueh estimates,


These formulse find their chief
uses

into

consideration.

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
Let it be

true

solids and

sucrose

in accurate the

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 required
formula

to estimate

(A), 1309,

we

have

100X18-20X60
,^"^

16.39

96-99X60/100
sugar per cent per
cent

of

the

weight
The

of the
cane,

juice. Let the juicebe


then 16.39 X. 80
99 cent per
=

80

per

of the
ceot

weight of the
sugar
=

13. 11

sugar

cane.

contained
12.98 per
per

cent

dry (Brix

matter,
The

therefore contains
cane cane

13.11

X.99

dry
matter

sugar.

juice
on on

20 X. 80*= 16 16
"

cent

dry

solids)
matter
-V-

and

12.98

="

3.02, the percentage


cent

of

dry
of

going into the crystallizer massecuite; 3.02


massecuite
94.4 per
cane.

.94 =3.21, Brix

the

Massecuite

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 94"

weighs

owing
of be diluted

to

the

of its crystallization salts


to cent =0.85

sugar

and

the decomposition also

certain from of 25

(see page
time

98) and
page

it should An

time
per

(see

95).
for

increase

of volume

is safe allowance

alteration, or

0.68+25

per

cent

should time
so we

remain
upon

Further, the massecuite the crystallizer about four days, the ii;L
the size and
=

cubic

feet.

de:"ending
then have

type

of the

crystallizer,
ton

0.85X4

3.4

cubic

feet per

of

cane

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

is 1850

the

size

of

the

vacuum-pans

and

under

the

usual

con-

346

SUGARHttOUSB

CALCULATIONS.

ditions with' pans

of 12 feet in diameter

1000 striking
=

cubic

would be approximately 1000-1-25 per cent 1250 cubic feet, 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 discharging to 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 to a definite purity, lasses depending upon that desired in the mo=
"

to

be

obtained

from

them.

This

formula
same.

assumes

sirupand molasses are the is sufficiently accurate for practical purposes: {A) Let
100
=

that the densities of

This

P=
p=

M
x

100"

"=

weight of massecuite in the strike; purityof the sirup; purityof the molasses to be boiled4n; purityof the required massecuite; 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 be

formula

may
a

be

appliedwith less accuracy


upon

when

purityof

footingor nucleus

which

strike is to

completed with inolasses. be made with greater facility (B) This calculation may ^ method for mixtures,illustrated in the diaby Cobenze's
"

A.

Cobenie,

Vta

Nottrand's

Chemical

der prakt. Photografio., 9th Compendium Annual, 1913, p. 563.

ed., p. 379;

348

SUGAB-HOUSB

CALCULATIONS.

degree Brix of the juiceto that at the temperature of measurement by means table of corrections,page of Gerlach's 489. Apply the Brix gravity number corresponding to this reduced specific perature at the temto the weight of the cubic foot or gallon of water
temperature
of measurement.

of measurement;

reduce

the

Example:
15** Brix
at

Required the wdght of 17.5717.5* C. measured


of the

cubic

foot

of

juice of

at 28** C.

Degree Brix

juiceat U.S'' C (page 489)


for

15.0'' 15** Brix at


7

Hydrometer
28*C

correction

Degree Brix and


28** C

corresponding specific gravity at (Sp. Gr."1.05831)

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
on

Referring to the table

page

of

tank

preferable that all measurements made is be the temperapracticable, at, as nearly as ture of graduation of the hydrometers, thus keeping all errors
measurements.
*

It is

at

minimum. Calculations the Ash and

214,

Based

upon

the etc.
"

Relation These

tween bemethods

Sucrose,

are

used

in

destroyed or example. The


assumed
a

ascertainingwhether sugar or other matters are in a boiling decomposed and removed ])rocess, for
mineral constituents cf the materials
are

to remain of

unchanged
the saline been

during the

process,

therefore show

comparison
sucrose

coefficients

(181) should

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 erroneous

whether

has

destroyed,and

conclusion. in
sucrose

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 50 saline coefficient
was

should be used

evaporated

to

sirupcontain-

r
RELATION BETWEEN THE ASH AND

SUCROSE.

349

ing

50.7

per of

cent 49.71.

sucrose, The

1.02 reduction

per

cent

ash the

and

saline

coefficient

of

saline of

coefficient This is in this culated calthe


case

by
less

50"40.71 in

"0.29,

indicates
terms

decomposition
the
cent
sucrose

sucrose.

percentage

of

in the

the

juice

by
saline 0.68. This

finding

what is of

per

0.29,

decrease

coefficient,

the

original

coefficient

50,

in

method
in

has

long

been

used but

in

beet-

and

cane-sugar
is what some-

manufacture
limited constituents tanks. soluble the salts C. H.

estimating
the the A. fact of

losses,
the

its

application
of and
to
a

by
on

deposition
surface
*

part
in

of the

the

ash

evaporating

storage

Zimmermann of

proposes

utilize

only

the since the the

sulphates
from

the

sulphated they
are

ash formed

in

this

method, through
with

which The

persist
as

manufacture.

material acid.

is The

ashed

usual

addition
ashless
matter

of filter is

sulphuric
or an

ash

is

tran^erred
and the The the of the

to

an

alundum

filtering-crucible
with difference is the hot
water.

soluble residue

removed
and

by

washing
The

is

dri(^

weighed.
ash The pnd this

between

original
soluble

weight sulphates.

of

residue
are

weight
as

calculations

made

before.

Xnt.

Sugar

J.,

16,

(1014),

383^

also

this

work

p.

336.

EVAPORATING
DISCUSSION O^
METHODS.

AND

JUICE
METHODS
BY

HEATING.
OF

CALCX7LATION.

Prop.

W.

H.

P.

Creighton,

Dean

op

Department

op

Technology,
215.
"

Tulanb

University,

New

Orleans,

La.

General
the
on

Conslderattons."
used in sugar

-^tyipora^n
house work

of Water.
the tables

At

low

pressures

based

Regnault's

formula
or

H=1091.7+0.305(r-32)B.t.u.,
U^
are

605.4 -fO.305 T for used. of


use.

calories,
tables such
as

too 377

inaccurate
should be

Only Sugar
at

Table

A,

page

216.
to
assume

Boiling
that of the

Point
the
water

Solutions." which
any

It is usual

temperature

portion of
to

given

mass
on

will boil is that


of the entire
to

pressure solutions the

surface

corresponding In liquid mass.


of

the

sugar
as

this

assumption
of

leads
a

serious
a

inaccuracies
mass

temperature
will

boiling of
upon

portion of

sugar

solution absolute This

depend
on

its

density,its viscosity and


the
to

the

pressure

the
that

surface. of the
on

portion considered.
of the of entire the
mass

pressure

will be the

surface the

increased
considered 217a.

by

pressure

due

depth
with

portion
and tions solu454.

below Variation

the

surface. liquid's of

Temperature
in the

Density
sugar

Purity.
In

"

The

variation

boiling-point of
in Gerlach's

with

density

is indicated is
as

table, page

general, the variation

in the

following table:

^^^

jj

Degree / Degree \ Degree

Brix

60 5.4 3.0

Fahrenheit

Centigrade

217b.

The

boiling point of
of

sugar

solutions

is also

enced influ-

by their purity.
218. Elftect have increase the

Viscosity. mucilages
the 350

"

In

the other

raw

juice

we

times some-

gums,

and

compounds
As

which
which

viscosity of

fluid.

anything

EFFECT

OP

VISCOSITY.

351
from

Impedes
surface
to

the tends
see

escape
to

of the
a

steam

bubble

the

heating
it is

produce
gummy

local rise of temperature,


a

easy

that

sirups will have


puce sugar

higher temperature
The

of

boiling than
Vaiiatioii
low in than
pressures

solutions.

difference

is uncertain. 219. At the

with
used

Depth
far

Below house

the

Surface."
small ferences dif-

in sugar

work

pressure tmder

produce
at

larger temperature
For small head

ferences difWhat

high pressures.
which
a a

example:

wiU

be the temperature

portion of sirup of
is 26 inches?

50.6'' Brix will boil if it is under

of 2 feet of solid (no


vacuum

bubbles) sirup in the third effect if the


A

head

of 2 feet of

sirup of specific gravity 1.236


of 2 "^

will change the pressure


to

pounds
to water

per 3.4

square

(50.6*') inch, corresponding


per

26

inches

vacuum

pounds
of vacuum,
we

square

inch. 3.4
at

At

26 inches vacuum,

boils at 125.5**

F.; imder
it boils

pounds
141.8* of

per square inch, or 23.8 inches Add for density 4* F. and F. F.

have

ture tempera-

145.8"

solution, without
As

'produce boilingin the sugar considering at all the effects of viscosity. required
from
to

transfer of heat
upon

the of

heating

to

the heated
we see

liquid
that in

depends
this in
case
case

difference is
as
a

temperature,
"*"

there

loss of 145.8"125

20.3*"

F., difference
in the

temperature
of water.

compared

to

similar lost

condition

We

shall call these their effect.

degreesin temperature
The relation

and

later will discuss

21d0. between is

Specific Heat
the

of
a

Sugar
sugar
a

Solutions."
and

density of
the values

solution

its specific heat

expressed by

equation of
to those

straight line and


be

hence
"

intermediate

below

may

readilyfound:

Degree Brix of 10 solUitioii


....

20 .03 .86

30 .79

40 .72

50 .65

60 .58

70 51

80 .44

90 .37

Specific heat.

2I^1"

Heat

of tlie

Liquid."
is

To

raise TF
a

pounds of

sugar

solution whose tu to
a mean

heat specific

C, from

mean

temperature,

requires temperature, tt, TrC("j-"i) B.t.u.

362

EVAPORATING

AND

JUICE

HEATING.

Thus,
would

to

raise 10 leO**

pounds of sirup at 60" Brix from


F.,
to
a mean
=

mean

temperature,

temperature,

180**

F.,

116 B.t.u. require 10X.58(180-160) and Sohitioifts 22^. Heat To Sugar


"

Evaporate
a

Water.
sugar water

The

temperature
will be
same

of the vapor
same
as

risingfrom
from
pure

boiling boiling
heat

solution
imder the

the

that the

pressure.

When

superheated bubble
excess

reaches and

the surface

of

boiling sirup it loses all

to at

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
a

temperatiure, tst corresponding to the .presaire at the surface, requires WiC(ti-ti)-^WiLiy where Lt is the latent
heat In is of water
cases

correspondingto
must

h-

where

h is greater than

fe,the

quantity WiC(ti"ti)
in evaporators

negative and
223.

be subtracted. In

Condensate."

condensing

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
up
a

number
in

of thermal condensate
of steam

units

equal

to

the its

loss in temperature

the

multiplied by
vessel, and
steam is
up

weight. give
at up

Thus,
WLi
is led

if W

pound
another

is condensed
own

at "i, it will

thermal
to

units in its vessel

if the

condensate
a

where

condensing W(ti-U)
Heated.

lower

temperature; fe,it will there give


224.

B.t.u.
"

Amount
cane

of

Liquid
must

to be
be

The

amount of
water

of normal

juice
milk

maceration
used There tanks in is and

water,

by the of lime, wash-waters, and

increased

amount

the

diluting the
a

defecator-bottoms

(mud

or

oachaza).

removal

of water

by evaporation in the various experiments, weight of the purified juice to


that of the
as raw

cake. with the filter-press


to

In careful

it is usual be

calculate the
or

evaporated
The

heated the of

from

juice,taking by
the sities. den-

into

consideration

dilution the

indicated

juice varies with the milling and the manufacture; methods also, with the equipment total weight of liquid to be heated of the factory. The
dilution
or

concentrated

usually

ranges

from

about

90

to

110

per

HEAT

LOSSES.

353

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 called the Specific Thermal heat transfer, is Conductivity,
cent

of ihe

"

the

number

of

thermal

units

transferred

per

hour

from

the steam
for each

Uirough the heating surface to the sugar solution tween bedegree difference of temperature, Fahrenheit,
and the solution for each
square

the steam

foot of

heating surface.
The formulas for heat transfer have
are

simple, but they all


value

involve this unit which


B.t.u.
are

may

any

between

1500

B.t.u. per hour. Experience and judgment Some of the variables to select a proper value. required and 50

the value of this imit are: effecting of the steam past the heating surface; (1) The velocity the o f solution the The surface ; velocity past heating (2) sugar (3) The presence of air or other incondensible gases; either on (4) T^e character and thickness of the deposits both sides of the heatingsurfaces; or and composition (5) The surface pressure and the depth, density of the sugar solution being boiled. The transfer of heat is the transfer of vibration and
thing any-

deadening
which
rate

the vibration

results in less. and lowered

Steam

cules mole-

have strudc the Rurf ace

their vibration
new

should On

be swept aside to allow the the


sugar must

impact of
away

cules. mole-

solution be moved is
as a

side of the
or

heating surface,
from the There

steam

bubbles

swept
heat existence

steam as heating surface,

poor

conductor. and

is

no

longer any

doubt

to

the

enormous

importance of surface films of gases, where the heating fluid is a gas, or of a vapor having air-containing films,as in
condensers
to

the resistance magnify incalculably the transfer of heat through the metal plate. Smith
or

which effects,

hJ

354

EVAPORATING

AND

JUICE

HEATING.

found of

that at 90" in. mercury

F. the presence reduced


mercury

of air heat

producing
cent.

pressure

1/20

the reduced varies


power

transniission

25 Orrok

per
*

cent, and
says water

3/20 in.

it 50 per with and the

that heat

transmission
to the

Telocity of the

in the tube

6/10

with and

(p^) where
,

Ps
of

represents the
the

partial steam
and air

pressure
pressures.

Pt

the

sum

partial

steam

See

'^Vacuum air

In the steam belt shown in Fig. 93, any Pumps," 246. in the heating steam is positivelyforced to the outlet incondensible
gases.

for

High
the

ciurent

velocity then
To
steam
as

is desirable

on

both

sides

of

heating surface.
of the decrease

secure

high
at

cross-section

current

velodty the right angles to its


steam

path should
is decreased

rapidly as

the volume

of the

steam

by condensation. is increased culation by securing a positive fluid cirEconomy in a predetermined path. In the ordinary standard
is
no

effect there

definite

path of either the


is erratic.
a

steam

or

the

juice. The
transfer
to

juice circulation
is

In
to

some cause

spots the
the

of heat

high, with
steam

tendency
but the

juice

largest part of the heating surface is not used efficiently.In the steam heating there are in which the incondensible large volumes space
space,

spout into the

efficiencyby bkmketing is eddying with cyclonic the heating surfaces. As the steam are constantly changing position. velocity, these volumes
gases

accumulate

and

lower

the

Eddy
When

currents

indicate inefficiency.
steam

exhaust contain

is used oil from

for the

heating
the

purposes,

it is

liable to

much of

engines. The
lime used

presence

of this oil and

scale,arising from
to

in the

impede the transfer of heat. defecation,


As the metal used

separate the heated


or

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 juices are evaporated to the saturation distinct stages. The or crystallization first point in two
"

either copper is generally

brass and

"Proportioning

of

Surface

Condensers,"

tions of the American

Society of Mechanical

G. A. Orrok, TransaoEngineers, 1917.

356

EVAPORATING

AND

JUICE

HEATING.

Operation is practically continuous


a.

while several

the second
times 12.5"

involves If
a

cyde

of

operations
cubic

repeated

daily.
Bnx
is will be
lo

unit to
a

of 10

feet of

juice of about
a

sent

serieB of vesaels called

multiple effect,it
therein cubic feet.

orated evap2

about

This

thickened
its

juice is called simp and density


is about 53" It b pumped

Brin.

from

tiple the mul-

eEfect and

is stored
to

in the
ond sec-

tanks,
next

preparatory
unit

operation.
stage
our

In the of

two

cubic
drawn and

feet of into
a

sirup will be
vacuiun

pan

evaporated
foot
will

to

about

1 cubic

of tnasseeuite be half about half

which
sugar

and

molasses.
water

Besides

evaporating
the

from
to

sirup

to

bring

it

the saturation

point,

the

I operations

in the pan

include
sugar

graining or forming the


crystals and
Fia.Ol.

the
of

subsequent
the crystak size.
This

enlargement
to

commercial

operation
governs

is called

boiling to grain. Efficiencyof evaporation


of

the
more a

design

while the multiple effect,


upon

vacuum

pan

design is
228.

dependent
mass

efficiently handling and


In

charging dis-

thick viscous

quickly.
Louisiana the

Multiple
of four
are

Effects."
two
or

multiple effect
three
or

usually consists

three

vessels;
while in

in Cuba

usually
even

used been
the

ordinarily;
used. of

Europe
far

five and

six

have with

Properly
vessels in
are on one

operated,
so

efficiency
fuel coste heaters affords
on

increases
are

number

as

concerned.
the

These

vessels
of steam

simple
side

steam

whN"

condensing
necessary
to

of

tube

the heat other

evaporate the

water

from

the juice and

the of

side.

Necessarily

t"mperature

pressure

DISPOSAL

OF

CONDENSATE.

357
those the

the

steam
or

on

the heating side


side. The

are

higher than
arising from

on

the

juice

heated

vapor

boiling

juice in the first efifector vessel passes through a pipe to the steam Fig. 91, and will evaporate space of the second effect,
water

from

the
a

juice if the

pressure

maintained

on

this

the two fall of temperature between proper The vapor sides of the heating surface. arisingin each effect

juice allows
does the

evaporativeduty
last which is sent

in the
a

followingone, except

that

from

to

condenser.

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 descends either in

through adjacent
the
center.

tubes

or

through the large


inay
as

down-take omitted
Note

The

large down- take


as

be

and several largertubes used


the

down-takes

desired.

followingconditions

in

Fig. 90:

Effect.

IV differences
40" -16.2 -24.7 8.6
""

Temperature

PresBurea:,
side Steam side Juioe Differences Densities, Briz: in.
in.

in.

Entering
In

effects effect)!

12** 470

These either 229.


steam
as

data maximum

were

obtained
or

on

test

and

do

not

indicate
in the be used

capacity
of

maximum

economy

necessarily.

Disposal

Condensate."

The

condensate

belt of the first effect is free of sugar The older condensate from

and

may

boiler feed water.

the other

effects,
to

especiallyin the
contain
sugar steam

types
over

of

evaporators,

is liable

carried
from in modem

by entrainment

in the

rapidly

moving

the

entrainment

is rarely preceding effect. There and well-operated well-proportioned condensates

multiple effects.
of
sugar
were

If the

containing

even

traces

used In

in the the

start

foaming.
93

boilers,these would ultimately modem the confactory, in which


by
E. W.

Figs. 90
American

to

are

from

paper

Kerr
1916.

in

Transactions

of

the

Society of Mechanical

Engineers.

358

EVAPOEATINQ

AND

JUICE

HEATINQ.

contain

no

sugar,

this water

ia used

in

feeding the
tanks. The

boilere, in
(mud
or

saturating
and

the

bagasse, in diluting tank-bottomB


various

cachaza)

in wfkshing the

Gondensat"
effect the the
may

from be and

the second

passed

into

third fourth

the total into then of


to
a

effect and

be removed pump. the from

by

means

It is usual condensate each

pump

separately
the
belt of the

calandria, as
or

heating section
effect 330. is often

termed.

Disposal
"

of

Gases.
gaaea
are

Incondeosible

bteught into the


steam

multiple effect [in the


or

juice

and

are

given

off

under

the reduced
to

pressures
less un-

and t"nd

accumulate,
as

removed
enter.

fast

as

they

Certain

nitrogenous
pose juice decomammonia

bodies

of the and

form

during

the

heating. positive

The

path
should

of the beating steam be


are so

that

the gases

forced
to

to move

continuously
where

the

exit

they
In

are

removed
the
case

by the pipes which


or

connect for the

eaolt
pose. pur-

calandria

with the

condenser,
of the
vacuum

air pump
pans

using high
but

pressure

steam,
steam

the air ia removed traps.


steam.

by

valves

in connection
pass,

with

the

The
The
steam.

steam

traps

let water will

neither
escape

air but
air

nor

air relief valve

let the of the the

air

not

the

Advantage
and will sink

is t"ken below

fact

that After

cools

readily

steam.
to

the

air has
a

escaped, the
stem

steam,
so

in attemptii^ the valve

follow,
allowed

heats

valve

and

oloaes

that

air to escape.

TCBEB.

359

231.

Jnlce

Height."

In

the

ordinary standard
capacity
the
cany

vertical

multiple
when
to

effect. Fig. 92, the

greateet

is secured exterior

the juice height, as the

indicated
to

by the glass gage


tube

effect, is one-third
the effect the s'^eam

oae-fourth
may

height.

Inside the lite

bubbles
not

the juice over the

tube

sheet,
is

but
at
or

this does the


same

indicate

juice level, by handfrom

sirup

kept

height

in all effects amount

controlled the into

valves

auhMuatically, the gaged by the


Types
of amount

pumped

last liffect being

of thin juice drawn

the first.
Different

232.
are

Multiple

Effects."

There

many

diSet^ot
of the

styles of multiide efiects made

of difierrat

modifications
same

few most is

elements.
couunon

The

fault

too

large
so

juice
that

capacity,
the
too

mains juice re-

long in
Home

the types

effect. lack

in

the

poaitiveness of the
circulation
steam
or

of
or

the in cS

juice

the the
gaaes.

withdrawal incondenuble

The

beating
is made
up

face sur-

of
^^ ^

straight tubes
horizontal.

usu-

ally either vertical


or

Usually the
the the To

steam

Eontal tubes well-known

and type

juice through permit air


a

passes through the vertical ones.


over

the
In

horione

juice is sprayed

inclined the closed

tubes upper

taining con-

steam.

to escape

end

of the 333.
are

tube

contains
"

pin hole.
the vertical standard
or

Tabes.

In

effect the

tubes

about
40
to

ft inch
54

thick, 1} inches long.


The

2 inches

in diameter and the the


more

and
more

inches
a

longer these
of them

tubes

intensely

small

number

is heated

360

EVAPORATING

AND

JUICE

HEATING.

certain
steam.

wiU

they spout juicehigh up in the rapidly moving efficient the heating surface, the The more more
will be the

uniform

boilingover
Intense

the

entire

top sheet
should

and the be

the smaller

will be the
steam

temperature difference between


localized

juice and
avoided.
The diameter

sides.

heating
or

tuTjes in horizontal

effects
14

are

f inch

inch

in
are

and

about unless

12

or

feet

long.

Longer tubes
These may

liable to sway
are

supported
in nests

in the middle. of

tubes

generallyarranged
as a

eight, which
Each
not

be

moved re-

unit

(Fig.91).
of Eff eets
to
are

234.

Relations

effects will operate when All the steam

they

Multiple operating efficiently.

Other."

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
had its heating surface
the
amoimt

covered

with

scale.

It

could

not

transmit
steam

of heat

it transmitted in its steam

before, so
belt
to

the

and temperature pressure transmitted heat the was rise till the
steam
now

would all But


steam

sufficient

condense
effect. the

coming
less than belt
or

over

from

Ihe

second

this would\be pressure in

formerly,as
calandria
the of

the the

rise in third

the

effect

has

increased the |)ressure The

on

juiceside of the second

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

difference of the

between

the

temperature
the

in

the

steam of the

calandria
vapor

first effect

and from

temperature

going
vacuimi

to the condenser

apparent
as
a

range

of

temperature.

the last effect is the total For a single effect,such in into


a one

the
a

double

pan, this total range occurs effect this range is divided in

vessel.

In

two

parts, in
effect
a

triple effect into three parts and


four

quadruple
in

into

parts.

For

the
are

causes

enumerated

ceding pre-

paragraph,
These of
are

there

of temperature. lost-degrees
a

tabulated below

for

tnple and

quadruple effect
under three

the

standard

type, for usual

conditions

heads.

(1) The

boiling temperature

loss is due

to

the

fact that

TEMPERATUBE

DIFFERENCES.

361

we

are

dealing with
water

sugar

solution rather

than

with

dis-

tiUed

(217) ;
static head loss takes in the loss due
to the

(2) The
of the

depth
sity den-

boilingliquid(216), (219).
third includes loss

(3) The
and To Obtain

(assumed) due (218).

to

the

of the solution viscosity the Pressures the

to he Carried

in the Vessels

of the
is

r^ln Multiple Effect of

table

below, the total loss degrees


F. The
steam

temperature
to

are

5.4*'-|-9' +15.4** =29.8''


the first vessel at 227.2^ 125.4" F. The

assumed
to

enter

F. and

the vapor
range

leave

the last vessel at

apparent

is

227.2** -125.4''
=

and

the

real range
can now

is 227.2** -125.4" be with

-29.8**
a

72** F.

This

real range

divided, for

triple

effect,into three parts in accordance


the heat coefficients that have scale of
range
or

conditions affecting,
as

been

considered

for instance In the table Tha

expected
the
ranges

oil

on

the

heating surfaces.
26** have is the

22**,24** and
in. each its

been
sum

assumed. of the

apparent
real range To

vessel

assumed

in it and

obtain

expected lost degrees of temperature. the temperature of the vapor rising in the first
the

vessel, subtract F., from


belt. in the The

apparent
steam
so

range

in

temperature,
in the
steam

27.4**

the assiuned 199.8** F. belt.

temperature
is the

first steam

obtained

temperature
199.8**

second

Subtracting SS"* F. from

gives

166.8** Fiom

F., the temperature of the vapor tables (page 377) we the steam

in the second
can

vessel.

readDy find the

pressures

correspondingto
DISTRIBUTION

the temperatures.

IN

TRIPLE

EFFECT.

362

EVAPORATING

AND

JUICE

HEATING

DISTRIBUTION

IN

QUADRUPLE

EFFECT.

Sugar Factory/' Abraham, translated by Bayle, the following table is given, illustrating
losses in temperature
LOSS IN

In

"Steam

Economy

in

the

in evaporators of beet sugar


DIFFERENCE
FAHRENHEIT. IN

factories:
DEGREES

TEMPERATURE,

Evaporation

System.

Single effect.
Double
....

effect Triple effect effect. Quadruple Quintuple effect.


. .

Hausbrand^

gives
in the The

even

greater differences
the

in the

fall of
are

temperature

effects when

heating surfaces

of

equal
him
are

area. as

ratios of the

fall of temperature

given by

follows: effect
1 1 58
.

In the double
In the

1 effect triple In the quadruple effect. .1

1 .44 1
.

3.44 1 48
.

105

2
.

175

Applying

these

ratios

in

the

preceding
as
1JI

cases

would

give

apparent temperature
In

differences
O

follows:
o

1?

op*
"

op.

the

tripleeffect quadruple
effect.
. .

17.3 17.7

24.9

59 26
.

In the The

19.5

38.4

discussion of

of the difference between has


and

real and

apparent
to largely
E.

differences
1

temperatures
Condensing

been Cooling

introduced
Apparatus,"

"Evaporating,

Ha\is-

brand, Eng.

Ed., 113.

364

EVAPORATING

AND

JUICE

HEATING.

did
to

not

build

m^ and
up

if

bring the
the

pressure

liad been enough steam supplied to 18 pounds per square lute, inch, absoper

evaporation enormously increased.


was

rate

square

foot

would

have

been

In

this test the

total range

of temperature

53.8" F., that in the first effect

being 7.6" F.
before

The

original papers
as

by Prof. Kerr should be consulted


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
"

drawing conclusions

approximately 3 pounds of water from 4 pounds of juice in a triple effect and that it will evaporate 4 pounds of water from 5 pounds of juice in a quadruple
effect in the
us same

unit of time

will evaporate

unit

of

time.
on

To
page

show 361

this, let
a

assume

the

steam

temperatures
the

for

triple
0

effect and

density of the entering juice is 12 Brix, the temperature being 180" F.


Distribution First Effect.
1 lb. per
in a

also that

Heat

Triple

Effect. Heat. lb. Juice, B.t.u.


4
.

steam,

5 lbs. pressure

Latent

=960.7

000

sq. in.

Heat

juiceat 180" F. to 199.8" F.,specific heat =0.9, 72 (199.8-180) X4X0.91


= =
.

requiredto raise

4 lb.

Total Latent

heat liberated heat


at 199.8" =977.7

888.7 B.t.u. .909 3.091 ^"x=i5-5".

Evaporation No.
Juice transferred

1 =888.7-^977.7= to No. 2 effect

BS^tooSecond
Heat liberated
as

*"

Effect.

follows:
1 effect

Vapor from

No.

888.7

Sensible heat from

condensate:
=

(227.2-199.8) Xl
Sensible heat from

27.4

juice:
86.7 1002.8

(199.8-166.8)3.091X0.85=
Total heat liberated

INCBEASING

EVAPORATIVE

EFFICIENCY.

366

Juice Intent

transferred to No. 2 effect


heat
at 166.8
=

3.091

998
=

Evaporation
Juice

No.

1002.8 ^998 3 effect

1.005 2.086
"

transferred to No.

15,5_2J086
Brix'"3.09r
Third
""

^ _^^o "r"-^3.

Effect. 1002.8

Vapor

from

No.

2 effect condensate:
=

Sensible

heat

from

(199.8-166.8)(0.909+1.005)
Sensible

63.2

juice: (0.75) (166.8 -125.4) (2.086)


heat
=
'

from

the

64.7
. .
. .

Total
Latent

heat

liberated
=

1130.7

heat at 125" F. in No. 3 23

1021 1130.7
'^

Evaporation
Sirup from
238.

1 107
.

0 979
=

0.979
"*"

No.

3, gg^

g^*
on

^"

^^'

Increasing

Evaporative
the
to heat

ally Efficiency." Theoreticscore

it is
use

always advisable

of steam

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
solutions and solutions in
a can

be

raised

to

high temperatures

series of

operations.
in the
steam
a

Thus, all the heat


from be its used
owi

the last effect is wasted, yet


to

going to the condenser portion of that heat could

the vapor the

ten degrees of juices to within some In other heaters, steam taken from temperature. pipes of the third,second, or first effect could raise

raise cold

juiceto highertemperatures. to the scheme the increased are The objections practical complexity of the apparatus, its initial cost and upkeep.
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

the

366

EVAPORATING

AND

HEAT

JCHCING.

used
or

in any

singleeffect heater, such


steam

as

the

vacuum

pan

the defectator,

used will be

"

h^.

being sent from the last effect to the condenser were it is evident that we of high enough grade, 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 to the second pipe leading effect, then the evaporation has been reduced 50 per cent, as only has been evaporated. By removing h 1 pound of water of the firsteffect we send must pounds from the vapor pip)e
steam
X

Suppose that the

h
steam sent to

to the first effect

^ +"

pounds of steam, thus saving ^ pounds.


a

Every pound of

effect should triple


a

orate evap-

3 pounds of water.
GAIN
IN PER

By
BY

taking off
ROBBING

pound
EFFECTS.

of vapor

CENT

from

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 first effect
we

lose the

second

effect

we

evaporate

out

of 3

pounds

of water

or

gain 663
239.

per cent.

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 fur-

General

the firstvessel with

(a)
This

( expression may
We
may

-j +hi pounds of

steam.

be considered to consist of two


a

tors. facact

imagine

weight
so

of steam

(
\n
n

-] to
/ /

normally in

vessels and

evaporate

n(
\n
n

^j =x"h

SAVING

IN

PER

CENT.

367

pounds
essary

of water.

The of water

other

hi, evaporated the factor,

neo-

^i
to

pounds

from

the firsteffect and this vapor


of

is sent

heating. perform the auxiliary t^ken from only the second of If ^2 pounds steam are
amount

vessels,the

of steam

that must

be sent

to the first

vessel will be

(6)
As
" "

("-^)+A,.
before,we
may

imagine

the steam

representedby
times its value

to

act

normally and

supply

additional evaporation, or (x"2ht) pounds. The will evaporate /is pounds from each pounds of steam
in
two

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, the first, then the total from second, third, will be, on consumption of steam rearranging expressions (a) and (6)above
. . . . . . "

rnx-T'H'rni-r*

.-[-An
n
"

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.
. . .

Savliig in

Per

Cent."

The

for direct

effect evaporation would multiple

be

"

+Pi-f-pa

Pn

and

the

percentage saving would be (pi4-2p2+3p8


. . .

npn)-^n.
of 0.15x,

In

quadruple effect

the

first effect is robbed the third of

the second

effect of O.lOx and

0.05z,the saving is
or

(.15X.254-.10X.50+.05X.75)x
or

12.6%. j?|a;

(238.)

(.16+2X.10+3X.05)-*-4"12.6%.
In
a

quadrupleeffect if,in
are

one

the first, second instance,

and

third effects

robbed

of

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_
"

~'^'^

however, Practically,
makes the

the reduction

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
from the boilers into the steam
steam

belt of the first effect and

or

of

sending the resulting belt. If P pounds of steam into the steam sent to are vapor it will deliver P pounds of steam to the first the preheater,
in
a

using this live

heater

effect, and
twice. The

care

must

be

taken
proper

not
must

to
now

count

this steam

multiple effect

evaporate x"P

pounds

of steam, and
,
,

this will
,

requireeither
(^1+2^2+3^3+.
n
. .

x-P..
n

nhn)

pounds of steam,
n

according as the effects are robbed or not. If the effects are robbed, then the firsteffect
X

must

receive

(n+l)P.,
n we

-|-/ii+/i2-r
"

,.

,
. .

(/ii-f2/i2+3/i3+...n/in)1
+P,
n

hn

simplicityS^-f P pounds of exhaust steam, llE being the quantity enclosed by the brackets.
which If the ( effects
are

shall call for

not

robbed, the first effect will receive


steam,
I

-PJ pounds
preheater or
a

of exhaust

and

pounds

from

the

total of (

(x"P\

pounds.
exhaust
steam to

The
the

total amount

of boiler and

supply
the the

various
use are

auxiliary machines
Ha^ Hi,, He
robbed
. " "

and

the

effects when of
steam

former effects will be

Hg pounds
. . .

and

of hu

hz, hz

hn

pounds

of steam

2^+P
^
I
"

+ f/a + H6+
|-/2a~r"6"r
Z7
1

Ho-{lh+h,-\^
n
'

17

.
" " "

u'
"^

hn)^ (Ai4-2/t2+3/i3 4... . .

nhn)
"

HEATIiNG

SURFACES.

369

242.

Steam

Consumption
of
cane

In
sugar

Cane

Sug^ar

Honse.
not
use

In the

manufacture do

most

factories 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

preevaporator

is also used

to

increase

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
steam
a

quantity of heat in
of
a

pound of high-pressure

and of

in that

pound
a

water

from
vacuum

that

that pound of low-pressure steam; in condensing will evaporate a pound of steam the juice; that a preheater may be used and for heating is steam using low-pressure pan

feasible. In
a

house is 78

provided with
per cent

quadruple effect,the
cane

oration evap-

of the

weight

and

the

exliaust The

steam
vacuum

supplied the firsteffect is therefore


pans
use

78/4

per

cent.

22 per cent

and

is used.

weight of steam (1) Straightevaporation,no


The
7Q
=

heating 16 per cent steam used is then, for, no preheater, robbing of effects,

for

57.5%. -^+16+22 (2) If


a

preheater receiving10

per

cent

steam

is

used,

55%. "^^^^^+16+22
=

(3) If
the

preheaterreceiving 10
pan,

per

cent

steam

is used
a

and

first effect is robbed


vacuum

of 10 per cent steam the second effect is robbed the fourth

for

sure low-prescent cent

juiceheating and for heating purposes,


for
4

of 10 per of 6 per effect is robbed

If the effects are the


are same

not

robbed
This
mass

it is usual to
cannot

give each vessel


if the effects
one

heating surface.
be robbed
as

be done
sent

to

the

of steam

from

effect

to the next

diminishes

greatly. Thus,

370

EVAPORATINQ

AND

JUICE

HEATING.

The 78
4 IB,..
Steam from

exhaust

steam

sent

to the firsteffect

S^"

5X10_^^^^^^_^^_ )^,, ^^^ (10X1+10X2+6X4^


4
19.5

10%
10.0-

10%

T,
in"

-29.6%"

I"

19.5%"

n-i".5%"

fl.5%"

IV-L3.6%

Eeater
10%

re-

i
29.5% 19.5% 9.5%

i
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, extra enlarged to provide the necessary a new
Where
a
'*

heating surface. 343, Heating


378,
one

Surfaces."

By referringto Table

B,

page

is struck in the

by the wide

disparityin temperature

fall also

allowed

different

effects in different

houses,and

conductivity by the disparityin the coefficients of thermal in the different effects in houses of the same capacity.
It is evident
are new

that

the

results

obtained

when
are

the

effects

and

free of oil and

and incrustation, in each

with

the

proper

fall of temperature these economic

operated vessel, will be


obtain.
may
assume

different when Under that


water
we can a

conditions

do not
we

average

conditions, for example,


effect will evaporate

quadruple
per

6.5 to

7.5

pounds

of

square foot of heating surface per hour and hence the heating surface obtain by dividing necessary
to

the

water

be

evaporated

in each

effect per

hour

by 6.5
\

to 7 5.
-

Thus,

if

quadrupleeffect is to evaporate
hour, the

100,000 pounds
effect will be

of water

per

heating surface
sq.

of each

100,000 -5- (6.5X4) =4000


If the effects surface
cane

ft., approximately.

of any

of vapor, the area of the heating effect is found by multiplying the weight of
are

robbed

ground

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

JUICE

HEATING,

fall of temperature

in them

and

those

in the

first two

creased de-

the fall of temperature by increasingcorrespondingly in them. Example: Find


a

the

area

of

the
tons cent

heating "vurface of
of cane, of the

juice heater for capacity;


cane

factory of 1000

steam

equal
from of

to

per

daily grinding weight of the


effect

to
a

be

taken

the

vapor

pipes of the second weight of the


transfer is 250
two

at

temperature
of the
cane

183.5^

F., the
of heat

juice is
is B.t.u. sides. that

that lOO"*
per

and

its temperature

entering the heater


the

F.y assumed
steam

coefficient

degree Fahrenheit

difference

between

Aspume'the

to lose 1000

B.t.u. per The

pound and

the
in

heat of the juice is 0.9. specific the

rise in temperature

juice
1000X2000X0.06X1000
1000X2000X0.9 B.t.u.
^^ wo

^o

p *"

The steam

mean

difference

of

temperature

between

juice and

sides of the heater


too
=

loo.o

c
"

/100+100+66.6
I
rt

=50.2"

F. the losses,

Allowing

10

per

cent

for radiation

and

other

heating surface
-

will be
.,

,,1000X2000X0.9X6G.6_^^o
^"^

1.1 X

250X24X50.2

^'

"*

The
must

originaljuice temperature
be
ten
or more

plus its rise in temperature


the assumed
steam tem-

degrees below
Pan. A
vacuum

perature.
244.

Vacuum

"

pan

is

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 and than
economy
a

of steam

is

sought in its design.


To boil

boil

drop

strike

quickly is desired.

required properly clarified sirup, good quickly there are and air and coils free of condensate steam sirup circulation, the heating steam as great difference in temperature between
and the massecuite
as

is

practicable. To
must not

drop
the

strike

quickly the heating


the massecuite.

surfaces

impede

free fall of

CONDENSER.

373

Boiler

steam,
Inside 4-inch

passing a reducing valve, is


having
the
pan 6
or

admitted

to

vertical manifold the


pan.

8 branches

or

nozzles into

entering
2
or

these

nozzles

divide
not

4 40

helical feet.

copper pans

tubes there

preferably
may

longer than
on

In sides

large
of
a

be

two

manifolds

site oppo-

diameter be
so

having similar

nozzles

and

tubes.

These

tubes and

culation arranged as to give the best cirthe quickest drop possible.


must

No

tube

must

contain the

steam

unless
of the

it is covered

with
mass

massecuite. in is the
pan

In

first part thin and

operation the
in volume

is rather

diminishes

till it

the building grain. After that period dui*ing 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^

ready

to form

Sugar is often boiled ivith exhaust tube at high velocity,as enters a


of the
process,

steam.

When in the

this steam first part


siderable con-

it does

when

the

sirup is thin, and


results that

condenses,
sets up

unbalanced

pressure

excessive

vibration, unless the tube is restrained by collars fastened soft coils must to rigiduprights. The not rub against their
collars and
In 450

produce pin holes in the tube. 0.55 boiler horsepower designing the pan, about
of steam
must

or

pounds

be

allowed

per

ton

of

cane

per

day.
245.

Condenser.
or

"

By
pan

condensing the
the pressure
steam

steam

from below

the that air

last effect of and the

vacuum

is reduced is

atmosphere.

As

the

accompanied
the

by

other

incondensible

juices or sirup,or through leakage, an air


them
so

gases, formed
pump may

either

dissolved

in the

inal origor

during
must

be

heating process provided to remove


The

that

the

vacuum

be

maintained.
on

metric baroa

condenser

is
at

condenser
may

when
open

ground so that it discharge by gravity against the atmospheric pressure the bottom of its discharge pipe is submerged in an
tank the filled with modern
water.

placed

preferredtype height above a

plantations. It is

the

In
enters

type

the vapor
at

pipe from
near

the effect bottom

or

pan
a?

the

condenser

the side

the

and

374

EVAPORATING

AND

JUICE

HEATING.

the suction
the

pipe of the air

pump

is attached

at

the

top,

water path of the gases is toward the top. The injection the top of the condenser enters and is broken into near up sprays
on
or

thin

sheets
to

through
air pump

which

the vapors

must

pass

their way
move

water
a

and opening. As the vapor in opposite directions,it ia sometimes called

the

counter-current The

condenser. the condenser.


It

discharge pipe usually supports


be about 34 feet

should
in

high.

To

find the minimum

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
the

weight of
1 square

column

of the

discharge water
To this add the

1 foot

and

inch

in cross-section.
to

the

of water

in feet necessary

produce
be

assumed

high height velocity


cone

of efflux of the Fins


or

discharge water. placed


on

projectionsshould
proper to

the

bottom from

of the condenser

prevent the
level.

water

whirling
second,

and

so

risingabove
"

the normal

Example.

If 5 cubic

feet of cubic

discharge foot, are

water to

per

weighing
from
a a

pounds per discharge pipe of


60

be

discharged

condenser

carrying
at
a

foot cross-section from 0.5 square of 2 pounds, absolute,into pressure of 14.7


as

the

atmosphere

pressure

pounds

per

square

inchithe minimum

height will be found


(14.7-2)

follows:

-^^=30.5
ion

ft.;

V^=2gh;
Minimum

/.

^1

^^^ 1.56
=

ft.;
ft.

=30.5 height

+1.56

=32.06

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

pans

should

be

heated

gently

painted with
pores.

close these The

paraffincor other paint which will Joints of all descriptions may leak air.
a

length

of time

vessel

will hold

vacuum

indicates its

VACUUM

PUMP.

375
two

air

tightness. Air leakage


of air that must office of the
gases
as a

may

be

or

more

times

the

amomit

be handled is to

unavoidably.
pump

The

air pump rather


so

air and The


some

other

in-

oondensible
oome

than that

vapor.

air and
vapor

vapor

off

mixture this
can

pumping
to
a

is

avoidable, un-

but if the of the

be
a

reduced

very not

small

amount

air is cooled

to

temperature

exceeding
than
10^
or

that 15*

by more incoming injectionwater To do this bring the vapor, Fahrenheit.


the suction

just as it is
into contact

ing enter-

opening of the air

pump^

with

surfaces
water.

having the temperature


in the

of the

incoming injection
same

The

parts
vapor

pressure the but


mass

condenser
of

is the

nearly the
we

in all the
perature temsponding corre-

temperatures
and

different parts of
take find the tables

may

differ considerably. If
vapor
we

of the
pressure

from

the

the

actuaUy

shall find this pressure less than that The difference of these existingin the condenser.

due is the pressure to the incondensible gases. pressures the less the amount of steam in lower we cool the vapor The
any

given

mass

and

the

greater the

amount

of air

as

the

The constant. total pressure remains proportion of vapor of air present is in proportion to the pressures and they exert. Thus
as

This

is Dalton's that
gauge

law the
was

of mixed

gases.
a a

suppose shown by the shows that table

absolute
102

in pressure and th