Laboratory Manual For Queensland Sugar Mills Fifth Edition PDF

BUREAU OF SUGAR EXPERIMENT STATIONS QUT j
Library I
LABORATORY MANUAL
FOR
Q U E E N S L A N D SUGAR M I L L S
FIFTH EDITION
Registered at the General Post Office, Brisbane, for transmission by post as a book.
Wholly set up and printed in Australia by

WATSON, F E R G U S O N AND COMPANY
Brisbane,
1970
PREFACE TO FIFTH EDITION
D u r i n g t h e past eight years the technology of t h e cane sugar industry has changed
considerably. Many new items of apparatus have been introduced i n t o sugar mill laboratories,
and analytical methods and techniques have been modified to take advantage of this improved
equipment.
This new edition of t h e Laboratory Manual has, as far as possible, been brought up to
to date as at the middle of 1969 and, w h i l e t h e f o r m of t h e Fourth Edition has been retained,
each chapter has been subjected to a critical review and changed or completely r e - w r i t t e n
to conform to present day knowledge. The equipment and methods of analysis set o u t are
those w h i c h , in t h e considered opinion of t h e officers of t h e Mill Technology Division, are t h e
most suitable presently available, but t h e r e w i l l doubtless be some sections w h i c h are t h e
subject of diversity of o p i n i o n , and t h e r e are some sections which are in such a state of
rapid change t h a t the procedures set d o w n w i l l be o u t of date in t h e near f u t u r e .
W h e r e v e r possible, descriptions and illustrations of apparatus cover t h e most modern

equipment available, and sections on such new equipment as t h e automatic polarimeter and
t h e spectrophotometer have been included. The chapter on analytical methods has been
broadened to include many new aspects of sugar analysis, and such o t h e r new subjects as
t h e direct analysis of cane. W i t h the increasing importance of boiler w a t e r t r e a t m e n t t h e
section dealing w i t h this subject has been expanded. A new chapter has been w r i t t e n to
cover t h e subject of metrology, w h i l e t h e chapter dealing w i t h soil analysis has been deleted,
as it is felt t h a t this subject is better covered in specialized t e x t - b o o k s .
The Bureau of Sugar Experiment Stations wishes to acknowledge t h e assistance given

by the following organizations and individuals w i t h t h e preparation of this m a n u a l : —
D r . W. H. Steel and Mr. G. A. Bell of t h e National Standards Laboratory.
D r . R. A. M. W i l s o n of t h e Colonial Sugar Refining C o . L t d .
Mr. J. L. Clayton of t h e Central Sugar Cane Prices Board.
The Sugar Research Institute.
The Colonial Sugar Refining C o . L t d .
The Queensland Health Department.
and a number of individuals in t h e sugar industry w h o f o r w a r d e d suggestions f o r this new
Edition.
The following reference books w e r e used freely in t h e compilation of this E d i t i o n : —
The System of Cane Sugar Factory C o n t r o l , Second Edition (I.S.S.C.T.).
Cane Sugar Handbook, N i n t h Edition, Spencer-Meade.
Polarimetry, Saccharimetry and t h e Sugars, Circular C.440, National Bureau of Standards.
ICUMSA Methods of Sugar Analysis, 1964 Edition.
Report of the Fourteenth Session of ICUMSA, 1966.
Various Publications of t h e British Standards I n s t i t u t i o n , and t h e Standards Association of
Australia.
We also gratefully acknowledge t h e provision of illustrations by various d i s t r i b u t o r s
of laboratory apparatus.
N o r m a n J. King, Director
1st February, 1970 Bureau of Sugar Experiment Stations, Brisbane
PREFACE TO FIRST EDITION
The Division of Sugar Mill Technology was created in 1929. One of the early duties of
the Division was to introduce a definite plan of campaign for mill control, which was not
possible at that time due to the confusion of methods employed and the lack of specific
standards. In 1930, Mr. Norman Bennett (then Mill Technologist) instituted the Mutual
Control scheme, which was voluntarily subscribed to by the majority of the Queensland
mills. The International Standards laid down at the Java Conference of 1929 were adopted
as the basis for this work, and a brief statement of standard analytical methods and specifi-
cations foi laboratory apparatus was prepared and issued to the mills participating. It was
most gratifying to find that practically all mills were eager to adopt the new standards in
their entirety, which made possible the present standardised method of reporting mill data
and enabled comparisons to be made of the work of different mills. Doubtless the scheme
has been directly or indirectly responsible for many of the marked improvements in milling
work which have characterised the accomplishments of the Queensland mills during the
past five years.
In order to assist the mills in obtaining accurately standardised equipment, the Division
undertook the calibration of all glassware employed by the industry; at the present time
practically all mills submit their apparatus for checking purposes, and hardly any new appar-
atus is obtained unless accompanied by the Bureau's guarantee.
It is felt that the time is opportune for the publication of a Manual which will provide
the mill chemist with the desired analytical methods, together with the tables employed
in the subsequent calculations, in a readily accessible form. This publication of the Bureau
is therefore presented in the hope that it may fill a long-felt want. Further, it was appreciated
that the student in sugar chemistry often finds it difficult to obtain a work which will pro-
vide him with the fundamental principles of the subject presented in an elementary form.
Chapters, have, therefore, been included in Definitions, Optical Instruments, Balances,
Densimetric Methods, and Calibration of Glassware, with this end in view.
The present work is the result of the combined efforts of members of the Bureau staff,
who would welcome any reconstructive criticism and advice from those engaged in the
industry. The authors wish to acknowledge their indebtedness to those excellent text-books
of C. A. Browne, G. L. Spencer, and J. Reilly and W. N. Rae, which sources have been
freely drawn on in the preparation of this Manual; and also to those manufacturers from
whose catalogues several of the illustrations have been taken.
H. W. KERR,
Director.
Bureau of Sugar Experiment Stations, Brisbane.

14th July, 1934.
CONTENTS
PAGE
CHAPTER I
DEFINITIONS .. .. .. .. .. .. .. .. .. .. 1
CHAPTER II
OPTICAL INSTRUMENTS .. .. .. .. .. .. .. .. 8
CHAPTER III
T H E BALANCE .. .. .. . . .. . . .. .. .. . . 51
CHAPTER IV
DENSIMETRIC METHODS OF ANALYSIS . . . . . . . . . . . . 58
CHAPTER V
VOLUMETRIC EQUIPMENT . . . . . . . . . . . . . . . . 68
CHAPTER VI
T H E BUREAU'S METROLOGY LABORATORY . . .. .. . . . . . . 75
CHAPTER VII
SAMPLING OF SUGAR M I L L PRODUCTS . . .. . . . . . . . . 78
CHAPTER V I I I
LABORATORY REAGENTS . . . . . . . . . . .. . . . . 83
CHAPTER IX
ANALYTICAL METHODS .. . . . . .. . . . . . . . . 94
CHAPTER X
T H E DETERMINATION OF pH . . . . . . .. . . . . .. . . 144
CHAPTER XI
CALCULATIONS INVOLVED IN CHEMICAL CONTROL .. .. . . .. . . 151
CHAPTER XII
T H E BOILER STATION . . . . .. .. .. .. . . . . . . 166
CHAPTER X I I I
FIRST A I D . . . . .. . . . . . . .. . . . . . . 181
R E F E R E N C E TABLES .. . . . . .. . . .. .. .. . . 184
CHAPTER I
DEFINITIONS
Whilst the majority of definitions from the previous Edition have been
carried forward, several general terms which have recently come into promi-
nence and some of the more important definitions associated with the milling
train have been added.
Absolute Juice—All the solids in solution in the cane, together with all the
water in the cane; i.e. Absolute Juice = Cane - Fibre.
Apparent—The word apparent is applied to figures and analyses based on
Brix and pol, as distinct from dry substance and sucrose, for example,
apparent purity. Brix and pol analyses are widely used for factory
control purposes, and unless a specific instance arises where pol and
Brix have to be divorced from sucrose and dry substance, the term
"apparent" is often omitted.
Ash—The residue remaining after burning off all organic matter. In practice
the proportion of residue remaining as "ash" is influenced by the
conditions of combustion, so that ash, as actually determined, is
not an absolute quantity.
Back Roller Juice—The juice expressed between the top and delivery
rollers of any mill of a tandem. The term is synonymous with last
expressed juice only when it refers to the last mill of a tandem.
Bagacillo—A fraction of the fine particles separated from bagasse.
Bagasse—The residue after extraction of juice from cane in one or more
mills. Hence the terms, First Mill bagasse, Second Mill bagasse etc.
and in the case of the last mill Final bagasse or simply bagasse, are
used.
Brix—The Brix of a solution is the concentration (in g solute per 100 g
solution) of a solution of pure sucrose in water, having the same
density as the solution at the same temperature. If refractive index
be adopted as an alternative basis of comparison the value derived
should be termed Refractometer Brix.
Obviously, for solutions of pure sucrose in water, the Brix is
equal to the dry substance, but in the presence of soluble impurities
this may not be, and usually is not the case. Although gases and
insoluble solids in suspension may alter the density of a solution
the term Brix refers exclusively to soluble solids.
Bulk Density—Prepared Cane—The bulk density of prepared cane is used
as a measure of the degree of cane preparation and is defined as the
weight of a prepared cane sample, divided by its bulk volume under
standard test conditions.
Cane—The raw material delivered to the mill, including clean cane, trash
and any other extraneous matter.
C C S . (Commercial Cane Sugar)—That percentage by weight of a quan-
tity of cane which would be recovered as pure sucrose (100 n.t.) if
2 DEFINITIONS
milling and refining operations were conducted at a prescribed

standard of efficiency. The prescribed standard of efficiency is such
that for every pound of soluble impurities in the cane one-half
pound of sucrose is lost in process, there being no other losses of
sucrose.
Impurities per cent cane
Hence C.C.S. = Sucrose per cent cane 2
In the normal application of this formula the following assumptions
are made:—
1. Brix = Total soluble solids (dry substance).
2. Sucrose = Pol.
3. Impurities = Brix — Pol.
4. Brix per cent cane
J . . 100 - (F + 3)
= Brix per cent first expressed juice x 100
5. Pol per cent cane
„ . . 100 - (F + 5)
= Pol per cent first expressed juice X TT^TJ
Hence
C C S . = Pol in cane — | (Brix in cane — Pol in cane)
2 V 109 J 2 V 100 )
where P — pol per cent first expressed juice
B = Brix per cent first expressed juice
F = fibre per cent cane.
Clarified Juice—Juice which has passed through the clarifiers. This juice
is fed to the evaporators and as such can also be referred to as Effect
Supply Juice or E.S.J.
Coefficient of Work—The percentage ratio of the weight of 94 n.t. sugar
produced to the weight of c.c.s. in the cane from which the sugar
was derived. Hence,
jr - ^ r „r , Tons 94 n.t. sugar made x 100
Coefficient of Work = —:
Ions c.c.s. in cane
(A discussion on this formula is contained in the Chapter entitled
"Calculations Involved in Chemical Control").
Compression Ratio (Milling)—The no-void volume of original cane,
divided by the volume occupied by the bagasse (or cane) at the
conditions being considered.
Condensate—Water which has been condensed, either from vapour liberated
from boiling juice, or from steam.
Crystal Content—The percentage by weight of crystalline sugar present in
a massecuite, magma or similar material.
Crystallizer Drop—The decrease in purity of the mother liquor of a masse-
cuite resulting from treatment in a crystallizer.
Cyclone Purity of Molasses—Usually this term refers to the purity of the
mother liquor of a massecuite at the completion of the pan boiling
operation. The term, suitably qualified, is often extended to refer
to the purity of any sample of mother liquor extracted from a
massecuite for examination, and not as part of the normal factory
operations.
DEFINITIONS 3
Dextran—A polysaccharide formed by the action of certain species of
bacteria on sucrose during cane and juice storage.
Dilution Indicator (D.I.)—A factor used to forecast the keeping and hand-
ling quality of raw sugar. It is the ratio of moisture to dry non-
sugars expressed as a percentage.
moisture
Dilution indicator = —— -—— — . X 100
100 — (pol + moisture)
A value of dilution indicator below 40 is considered satisfactory,
for values between 40 and 50 the keeping quality of the sugar is
doubtful, whilst for values above 50 the probability of deterioration
is considerable.
Dilution Water—The quantity of added imbibition or maceration water
which is present in mixed juice. Dilution water is usually expressed
as dilution per cent first expressed juice.
Dry Substance—The weight of material remaining after drying the product
examined under specified conditions, expressed as a percentage of
the original weight. The determination of dry substance represents
an attempt to measure the total solids, both soluble and insoluble,
or, in the absence of insoluble solids, the total soluble solids. The
degree of accuracy achieved depends upon the constitution of the
sample and the drying technique.
Escribed Volume—The volume escribed by a pair of mill rolls in a given
time. Escribed volume is equal to the roller length multiplied by the
work opening multiplied by the surface speed of the rolls.
Extraction (Pol)—The percentage of pol extracted from the incoming
material by a train of mills either individually or cumulatively.
Analogous definitions apply to Sucrose Extraction, Brix Extraction,
and Juice Extraction, the juice, in the case of the last mentioned,
being undiluted juice.
Extraneous Matter—That portion of the material received as cane which,
by arbitrary standards, is considered not to form part of clean cane.
It consists of trash, tops, roots, dirt, etc.
Fibre—Technically, fibre is the dry, water-insoluble matter in the cane. For
commercial purposes a standard method of determination of fibre
per cent cane is specified.
Filling Ratio—A term used in milling calculations to define the ratio be-
tween the no-void volume of fibre passing between a pair of rolls
in a given time, and the escribed volume for the same period of
time. Filling ratio is actually volumetric coefficient divided by fibre
density.
Filterability—The filterability of a raw sugar is measured by comparing the
filtration rate of the sugar with that of a standard sucrose solution
under specified conditions. The result is expressed as a percentage
of the filtration rate of the standard sugar.
Filter Cake—The washed residue discharged from mud filters.
Filtrate—Liquid which has passed through the filtration process.
First Expressed Juice—The juice expressed by the first two rollers of a
mill tandem.
DEFINITIONS
Gravity Purity—See Purity.

Gravity Solids—Synonymous with Brix q.v.
Gums—A general classification given to polymers of high molecular weight
which can be precipitated from sugar products by a strong alcohol
solution. Substances included in this category are pectins, hemi-
celluloses, oligosaccharides, dextrans and solubilised starches.
Hygroscopic Water—The Brix-free water absorbed by cane fibre, the
amount of which varies with the condition of the solution with which
the fibre is in contact. For sugar solutions of low Brix and at normal
temperatures, such as those experienced in bagasse analysis, it
appears that hygroscopic wrater is some 20 to 25 per cent on fibre.
Imbibition—The process whereby water or juice is added to bagasse to
dilute the juice contained therein.
Impurities (Soluble)—A collective term for all substances other than
sucrose present in the total soluble solids contained in a sample.
Sometimes expressed as a percentage of the whole material, as in
the c.c.s. formula, and sometimes as a percentage of the total
soluble solids as in
Impurities = 100 — purity
Frequently based on apparent analyses, in which case it is synonym-
ous with Non sugars.
Invert Sugar—The equimolecular mixture of glucose and fructose which
results from the hydrolysis or inversion of sucrose.
Java Ratio—The percentage ratio of the pol per cent cane to the pol per cent
first expressed juice.
Hence.
Last Expressed Juice—The juice expressed between the top and delivery
rollers of the final mill in a tandem.
Maceration—The process in which the bagasse is steeped in an excess of
wyater or juice, generally at a high temperature. The water added
for this purpose is termed maceration water.
Magma—A mechanical mixture of sugar crystals with a liquid such as syrup,
juice or water.
Massecuite—The mixture of sugar crystals and mother liquor discharged
from a vacuum pan. Massecuites are classified according to descend-
ing purity as first, second, etc., or A, B, etc.
Milling Loss—The percentage ratio of pol in bagasse to fibre in bagasse.
Mixed Juice—The mixture of juices leaving the milling train for further
processing.
Molasses—The mother liquid separated from a massecuite. It is distin-
guished by the same term as the massecuite from which it was
extracted.
Mud Solids—Insoluble matter other than bagacillo in subsider mud, filter
cake and associated materials.
DEFINITIONS 5
Net Titre (N.T.)—An empirical value used as a measure of the percentage
of pure sugar which m a y be recovered from a batch of raw sugar.
Sugars of various qualities are commonly reduced to a common
basis of 94 n.t. as follows:—
Non-Sucrose—The difference between dry substance and sucrose.

Non-Sugars—The difference between Brix and pol.
Normal Weight—That weight of pure sucrose which, when dissolved in
water to a total volume of 100 ml at 20 °C, gives a solution reading
100 degrees of scale when examined in a saccharimeter, in a tube
200 mm long, at 20 °C.
The normal weight according to the International Sugar Scale
is 26.000 g weighed in air with brass weights.
No-Void Volume—The volume of cane (or bagasse) calculated on the basis
that it consists of juice and fibre only i.e. that all air and/or gas has
been removed.
Other Organic Matter (O.O.M.)—The sum of the constituents of raw
sugar other than pol, reducing sugars, ash and water.
i.e. o.o.m. = 100 — (pol + reducing sugars -j- ash -j- water)
Pol—The pol of a solution is the concentration (in g solute per 100 g solution)
of a solution of pure sucrose in water having the same optical rota-
tion at the same temperature. For solutions containing only pure
sucrose in water, pol is a measure of the concentration of sucrose
present; for solutions containing sucrose and other optically active
substances, pol is the algebraic sum of the rotations of the consti-
tuents piesent.
Primary Juice—All the juice extracted without dilution.
Primary Mud—The discharge from the underflow of a clarifier prior to the
addition of bagacillo.
Purity—Three classes of purity—Apparent, Gravity and True purity—are
recognized. Ideally, purity is the percentage of sucrose in the total
solids in a sample. The purities mentioned above are derived as
follows:—-
The term purity alone generally signifies apparent purity.

Gravity purity is not used in Queensland.
6 DEFINITIONS
Reabsorption Factor—The ratio between the no-void volume of bagasse
leaving a mill opening in a given time, and the escribed volume for
the opening, over the same period of time.
Reduced Extraction—A formula used to express normal mill extractions
on a common basis of 12.5 per cent original fibre in cane. The
formula is usually expressed in the general form,
(100 —extraction) (100— fibre)
Reduced extraction = 100 = ^r
7 x fibre
Reducing Sugars (R/S)—The reducing substances in cane and sugar pro-
ducts calculated as invert sugar. The most familiar examples of
sugars having reducing power are glucose (dextrose) and fructose
(laevulose).
Reducing Sugar/Ash Ratio—The ratio between reducing sugars and ash.
Refractometer Brix—See Brix.
Remelt—A solution of low grade sugar in either syrup, clarified juice or
water.
Residual Juice—The juice left in bagasse after milling.
Seed—Fine sugar crystals, generally suspended in a liquid medium, in which
case the mixture is known as seed slurry. Seed is used either to
provide the crystal surface for deposition of sucrose, or to promote
spontaneous crystal formation from a super-saturated solution. The
latter is referred to as shock seeding.
Set Opening—The distance between the tips of the teeth of a pair of rollers.
Where the roller teeth are set in mesh, this distance will be negative.
Sucrose—The pure chemical compound with the formula C 1 2 H 2 2 O u . This
is commonly referred to in the industry as pure cane sugar.
Sugar—The crystals of sucrose, together with any adhering molasses, as
recovered from the massecuites. The various grades are commonly
identified in terms of the grade of massecuite processed, or in terms
of the avenue of disposal of the sugar—hence, A sugar, C sugar,
Shipment sugar.
Suspended Solids—Solids in juice or other liquid, removable by mechanical
means.
Syrup—The concentrated sugar solution leaving the evaporators.
Total Sugars—The combined percentages of sucrose and reducing sugars
in a sample.
Turbidity—A measure of the material in suspension in a sugar solution as
determined by a spectrophotometer.
Undiluted Juice—The juice expressed by the mills or retained in the
bagasse, corrected for dilution water. For purposes of calculation
the Brix of the undiluted juice is taken to equal that of the primary
juice, or in Queensland, the first expressed juice.
Volumetric Coefficient—A term used to designate the fibre loading of a
mill opening. Using the British system of measurement, it is quoted
as pounds of fibre per cubic foot of escribed volume.
DEFINITIONS 7
Work Opening—The mean opening between a pair of mill rolls. This opening
takes into account the set opening and the allowance for mill
grooving. No allowance is made for juice grooves, but where a dirty-
top roller is employed, this must be taken into account.
Work Ratio—Where a three roller mill has rollers of equal circumference
rotating at a common speed, this ratio is the ratio between the feed
work opening and the delivery work opening. Where openings with
rollers of different diameter or different peripheral speed are to be
compared, it is necessary to calculate the ratio from the two
escribed volumes.
CHAPTER II
OPTICAL I N S T R U M E N T S
The optical properties of sugar solutions afford rapid and convenient
methods for their analysis and the chemist's most important piece of appara-
tus is the polarimeter or saccharimeter. The refractometer is used in a limited
degree for the rapid determination of total solids in juices and syrups. The
introduction of colorimetric methods into sugar laboratory analyses demands
the use of the spectrophotometer, and clarification studies require the use of this
instrument as a turbidimeter. The microscope is used where raw sugars are
examined for grain quality. Each of these instruments will, therefore, be
described in some detail. Recent trends to automation have resulted in the
development of automatic polarimeters; these will be discussed fully while the
principles involved in automatic refractometers will also be mentioned.
Properties of Light
Light is a form of electromagnetic radiation and it consists of trains of
waves vibrating transversely—that is, at right angles to the direction in
which the waves are travelling. The most familiar case of a transverse wave
is probably that which travels along a rope or string when one end is suddenly
jerked sideways. If the end of the rope is moved continuously, a continuous
wave will be produced.
Fig. 1—Illustrating the principle of a light wave.
Fig. 1 represents a wave in which the vibration is at right angles to the

direction of motion, P Q. The distance A B is the amplitude of the wave,
while the distance 0 E, which includes one complete crest and trough, is
known as the wavelength and denoted by the symbol A. For light, wavelengths
are expressed either in nanometers (formerly called millimicrons; 1 nm =
10- 9 metre) or in angstrom units (1 A = 10- 10 metre = 0 . 1 nm). Light of
different wavelengths appears to the eye as different colours; the following
wavelengths have the colours given:
683 nm red
615 nm orange
559 nm yellow
512 nm green
473 nm blue
410 nm violet
These represent pure spectral colours; colours of most objects, however,
are due to light having a range of wavelengths. The intensity of the light
depends on the amplitude of the wave; in fact, it is proportional to the
amplitude squared.
OPTICAL INSTRUMENTS
The number of complete waves passing any point each second is the
frequency, denoted by v. This is measured in hertz (Hz), formerly called
cycles per second. For visible light the frequencies range from 4 x 1014 to
8 x 1014Hz. The speed v at which the wave advances is then given by
v = v X.
In a vacuum, light has a constant speed, no matter what its wavelength;
this is denoted by c. In transparent matter, light has a lower speed and this
speed varies with the wavelength of the light. It is this slowing down of light
by matter that enables optical measurements to give an estimate of, for
example, the total dissolved solids in a solution; the more material in solution
the greater the "slowing down" of light.
In general, the vibration of a light wave occurs in the two dimensions at
right angles to the direction of travel. However, light can be made to vibrate
entirely in a single plane just as a water wave vibrates only up and down.
The light is then said to be plane polarized or linearly polarized. When such
light passes through certain media, the orientation of this plane is changed.
This change is caused only by special materials, said to be optically active, of
which sugars are examples. The amount the direction is changed depends on
the concentration of the optically active material in a solution, so polarimeter
measurements give concentrations of active materials (such as sugars), rather
than total solids.
Refractive Index
In a homogeneous medium light travels in straight lines. If, however, a
beam of light in one medium meets the surface of a second medium, it will
in general be refracted or bent from its original path. The incident ray of
light, denoted by L O in Fig. 2, arrives at the boundary between the media
Fig. 2—Illustrating the law of refraction.

M and M' in a direction represented by the angle LOP between the ray and
the normal (perpendicular) to the boundary. This angle is called the angle of
incidence i. Part of the light is reflected along O L' at the same angle i on
the opposite side of the normal. The bulk of the light, however, is transmitted
into the second medium along O S, which makes an angle SOQ with the
normal. This is called the angle of refraction. If this angle is smaller than the
angle of incidence, the first medium is said to be the rarer medium and the
second the denser. This terminology relates to the effect, discussed earlier,
that as the concentration and hence the density of a medium increases, the
speed of light in it decreases. (This should not be confused with the "optical
density" of a medium, which refers to its light-absorbing properties).
The angles of incidence and refraction are related by the expression
n sin i = n2 sin r
where n and n 2 are constants describing each medium; they are the refractive
indices of the media. For any transparent medium, the refractive index is
the ratio of the speed of light in air to its speed in the medium. Thus, a
"denser" medium, having a lower speed of light, has a higher refractive index
than a "rarer" medium.
For a stricter theory, the refractive index should be defined with respect
to speed of light in vacuum rather than in air, namely
n = c/v.
This is the absolute refractive index and it is 1.000 28 times the refractive
index relative to air, 1.000 28 being the absolute index of air itself. For
practical purposes, however, it is always the index relative to air that is used
and this is what is meant by the simple term "the refractive index".
Another way of writing the relation between the angles of incidence and
refraction is
sin i
-. = n
sin r
where n = n 2 /n 1 and is the ratio of the two refractive indices or the relative
refractive index. This ratio is the same whether absolute indices or indices
with respect to air are used.
Since the speed of light in any medium other than vacuum varies with
wavelength, so does the refractive index. Light of different wavelengths is
therefore refracted by different amounts. When a beam of white light, which
is a mixture of all visible wavelengths, is refracted at a boundary, it is spread
out into a series of colours, known as a spectrum. This is the phenomenon of
dispersion, sometimes called prism dispersion to distinguish it from the rotato-
ry dispersion discussed later. When a refractive index of a material is quoted,
it is therefore desirable to specify the wavelength for which it has been meas-
ured. Certain spectral lines are known by letters, for example, the D line of
sodium and nD denotes the refractive index for this line. Important lines are:
Symbol Wavelength (A) Colour Element
C 6563 red hydrogen
D 5893 orange sodium
d 5876 yellow helium
e 5461 green mercury
F 4861 blue hydrogen
When the line is not specified, it is commonly the D index that is meant.
Although useful for measurements of moderate accuracy, this is really two
lines, close together. The modern tendency, particularly for accurate work,
is to replace the D line by either the helium d line or the mercury e line.
The dispersion of a medium is given by the difference between the re-
fractive indices for the blue and red lines of the hydrogen spectrum, i.e.
nF—nC.
The refractive index of a material also varies with the temperature and
a complete 2description of a refractive index should also include this, as, for
example6
nD 0 °. The rate of variation for glass is small, between 1 x 10- 6 and
6 x 10- per degree Celsius, and is usually positive, the index increasing as
OPTICAL INSTRUMENTS 11
the temperature increases. For liquids, the rate of change is much greater
and in the opposite sense; an increase of temperature by 1 degC decreases
the refractive index of water by 8 x 10-5. For sugar solutions, the te
for organic liquids it may be even greater.
The Refractometer
For the most accurate measurements of refractive index the material,
if a solid, is made into the form of a prism. If liquid, it is poured into a hollow
prism. The deviation of the light through the prism is then measured. For
routine measurements of refractive indices of liquids, however, methods
based on the critical angle are used.
Critical-Angle Refractometers
When light passes from a rarer to a denser medium, the angle of refrac-
tion is smaller than the angle of incidence. Thus, while all values up to 90°
are possible for the angle of incidence, until the incident light grazes the
boundary surface, the angle of refraction has a maximum value that is smaller
than this. This maximum value is the critical angle r c and is the angle of
refraction that corresponds to an angle of incidence of 90°. Then
sin i — 1
and nn1 = n2 sin rc.
Thence an unknown index n 1 can be found by measuring the critical angle r c
for light refracted from the sample into a denser medium of known index n2.
The method is illustrated in Fig. 3, where M 1 is the rarer and M 2 the
denser medium. In Fig. 3(a) the light is incident from the rarer medium and
rays 0x-0b are shown at increasing angles of incidence. A small amount of the
(o) (b)
Fig. 3—Illustrating the measurement of critical angle,

(a) by transmission (b) by reflection.
energy from each ray is reflected at the boundary; the rest is transmitted in
the refracted ray. Since the ray 05 arrives at an angle of incidence of 90°,
it is the critical ray. No light from Mx can penetrate into M2 at a larger angle
of refraction. Hence, if the emergent light into M2 is viewed by a telescope
aimed along the direction 05, the observer will see light on one side of the
field of view, darkness on the other. Obviously, it is impossible for the
telescope to be inside the denser medium M 2 , but this medium can be made
as a prism, the second surface of which refracts these emergent rays into the
air. This second refraction will change the direction of the critical ray but the
final direction will still depend only on the known refractive index of the
prism M2 and the unknown index of the sample M1. The angle of the critical
ray is measured and the index n 1 of the sample found from tables provided
with the refractometer, or the instrument is calibrated to read, instead of
angle, the index n1 directly or a Brix value derived from n1.
The reverse process to that described above is shown in Fig. 3(b). In this
case the light is incident from the denser medium and the rays O1-05 are again
part reflected and part refracted at the boundary, passing into the rarer
medium at a larger angle to the normal until, for 05, the angle of refraction
has reached 90° and the ray leaves grazing the boundary. The angle of inci-
dence for this ray is thus the critical angle. If the angle of incidence is in-
creased further, as in O 6 or 0 7 , no light can be refracted into the rarer medium.
All the energy is reflected at the boundary giving the phenomenon known as
total internal reflection. Again if the light emerging in the denser medium,
now the reflected light, is examined by a telescope aimed along 05, a divided
field of view is seen with one side brighter than the other. The brighter side,
at angles greater than 05, corresponds to rays for which there is total reflec-
tion, while the darker side corresponds to partial reflection. For this case
sin r = 1
and n1 = n2 sin ic.
Fig. 4—The essential parts of an Abbe refractometer.

The critical angle is now an angle of incidence. Since on reflection, the angles
of incidence and reflection are equal in magnitude, the unknown refractive
index is found from a measurement of the angle of reflection that corresponds
to this critical angle of incidence, ic.
For either method of critical-angle refractometry, the solid or liquid
sample M1 is placed on a prism of the material M2. For the first method, the
boundary is illuminated from the sample; for the second, from the prism.
In both cases the illumination should cover a range of angles: in the first case
right up to 90° incidence, and in the second the range must include the critical
angle. The emergent light, refracted or reflected according to the method, is
examined through a telescope, the inclination of which can be altered to set
it in the direction of the critical ray. The field of view of the telescope has a
light and a darker side and the boundary between them is set on a pair of
cross lines in the telescope eyepiece.
In the first method, the darker side of the field would be completely
dark, but for scattered light. In the second method there is only the less
obvious distinction between total and partial reflection. Hence the first
Fig. 5—The principle of the Abbe refractometer.

14 OPTICAL INSTRUMENTS
method is therefore by far the more sensitive method of measurement and
it is the one normally used. The second method is only used when the speci-
men is so strongly absorbing {e.g. a sample of molasses) or scattering, that
insufficient light can be sent through it to the boundary.
One of the most widely used refractometers that is based on the measure-
ment of the critical angle is the Abbe refractometer. An early model made by
Zeiss Jena is shown in Fig. 4 and, in conjunction with Fig. 5, is convenient
for explaining the operating principle. Two prisms A and B of a flint glass of
high refractive index (nD) = 1.75) allow samples to be measured with re-
fractive indices up to 1.7. Each prism is contained in a metal mount, the
mount of the lower prism B being hinged to that of A and held in the closed
position by a clamp. The two prisms are connected through the main bearing
of the instrument to the arm J, which carries a cross line and eyepiece L.
Rotating independently about the same axis is a second arm which carries
the telescope F and the sector S, upon which the refractometer scale is en-
graved. The angle between the prisms and the telescope is read as the position
of the cross line on the a r m / relative to this scale, while this angle is adjusted
to set the boundary line on the cross line in the telescope by turning the
knob T. In Abbe refractometers, the scale is not normally graduated directly
in angle but either in refractive index or in Brix.
In use, the two arms are rotated together until the prism B is uppermost,
the clamp released, and prism B opened away from A. It will be noticed that
the top (hypotenuse) surface of A is polished while the corresponding surface
of B is roughly ground. If a solid sample is being examined, such as the test
piece normally supplied by the manufacturer, a drop of a liquid, such as
monobromonaphthalene (n — 1.658), that is known to have a higher index
than the test piece is first placed on the top of A, which should be horizontal,
and the large polished face of the test piece is pressed down on this, the small
face to the front of the instrument (away from the telescope). This small face
is pointed towards a window or another diffuse source of light and the tele-
scope set on the boundary between the light and dark fields with the instru-
ment in this "upside-down" position. The same position is also used for
absorbing liquids, when the second method of measurement is used. The light
is sent through the window C of prism A (normally closed by a cover) from
the mirror R. In both these measurements, prism B is not used.
For the usual measurements on reasonably clear liquids, a drop of the
liquid is placed on the surface of prism A. Prism B is then clamped into
position so that the liquid forms a film about 0.15 mm thick between the faces
of the two prisms. The instrument is swung back so that the telescope is
upright and light is reflected from a diffuse source from the mirror R into
the open face of prism B. This light is then scattered by the ground face of
this prism which serves simply as a means of giving incident light inside the
liquid at all angles up to 90°. Prism A gives the critical refraction.
The path of the light through the instrument is shown in Fig. 5, with the
light entering through prism B, and being scattered at the ground surface.
In this figure, the thickness of the sample is greatly exaggerated, and in prac-
tice the rays p q and p' q' are almost parallel to the prism surface ef.
These rays enter the prism A at the critical angle and are brought to a focus
along a line at L in the eyepiece of the telescope. Other rays are focussed to
the left of L, so that L represents the boundary between light and dark fields.
This boundary is set to intersect the centre of the cross lines, as shown.
To measure the D index, a sodium lamp may be used as the light source.
When a source of white light is used, the boundary becomes a band of colours
since a different critical angle is obtained for each wavelength. To compensate
for this dispersion, Abbe refractometers are equipped with a pair of compens-
ating or Amici prisms. These prisms are placed on the telescope tube, in front
of the objective and can be rotated simultaneously in opposite directions by
the screw head M. They then act as an adjustable prism that produces no dev-
iation of the light but has a variable dispersion that can compensate for the
dispersion of the critical refraction. Attached to the prisms is a scale z that
can be used to give the dispersion of the sample, that is nF — nC. The Amici
prisms are adjusted until the boundary between the light and dark fields
becomes as sharp as possible. It is then not quite colourless but is seen to
have a narrow band of a magenta colour on one side, yellow-green on the
other.
Unless the refractometer is used in a temperature-controlled room, the
sample should be kept at a constant temperature during the measurement
by circulating water at a constant temperature through the metal mountings
which carry the prisms. The temperature is indicated by the thermometer Th.
When a measurement has been made, the liquid should be removed from
the prism surfaces with absorbent paper, the surfaces washed with a suitable
solvent (usually water or alcohol) and dried with a soft cloth. As the prisms
are made of a soft flint glass, they are easily scratched and great care must
Fig. 6—Abbe refractometer by Carl Zeiss, W. Germany.

be taken not to wipe grit across their surfaces or close them with dust in
between. A scratched or pitted prism will give an indistinct boundary.
The adjustment of the refractometer should be checked periodically on
a sample of known refractive index. This can be the glass test piece provided
with the instrument, freshly distilled water free from air (nD20° = 1-3330) or
another liquid that has been specially calibrated. When making this check,
the telescope is set at the refractive index of the calibrating sample and the
adjusting screw V turned until the boundary is at the cross line. When using
liquids as standards, it is essential to control their temperature to that for
which they have been calibrated.
Fig. 7—High accuracy refractometer by Bellingham and Stanley, London.
Provided the sample gives a clear boundary between the light and dark
fields, an Abbe refractometer should be capable of measuring its refractive
index to an accuracy of about two units in the fourth decimal place (2 x 10-4).
Fig. 6 shows a modern instrument made by Carl Zeiss, Oberkochen, W. Ger-
many.
There are however more accurate critical angle refractometers which will
measure the refractive index of solutions to an accuracy of three units in the
fifth decimal place (less than 0.02° Brix). Figures 7 and 8 illustrate two
types of high accuracy refractometers. The bench model (Fig. 7) is used
with a monochromatic light source and readings may be obtained over
the range 0 to 80° Brix with a single measuring prism. The Dipping or
Immersion refractometer (Fig. 8) is fitted with a compensator for light
dispersion correction, so that it may be used with white light. It is supplied
with a series of interchangeable prisms, each one covering a portion of
the total range of 1.32 to 1.64 refractive index. This refractometer may
be fitted with either non-heatable or heatable prisms. In the former instance
Fig. 8—High accuracy immersion refractometer with temperature controlled prisms by

Carl Zeiss, \V. Germany.
it is used with the measuring prism dipping into the solution to be tested.
The heatable prisms are similar to those of the Abbe type refractometer
and are water jacketed to permit temperature control of the sample.
This heatable prism assembly is usually preferred by Queensland sugar mills.
Flow through cells are also obtainable for these instruments. It must be
stressed that constant temperature control is essential for precision measure-
ment.
With high accuracy refractometers the scale is not calibrated in refrac-

tive index but is an arbitrary scale of equal divisions. As the scale is linear it
may therefore be subdivided by means of a vernier so that readings to one
tenth of one scale division are possible. Tables are provided for conversion
of the scale reading to refractive index from which the degrees Brix may be
determined.
Simpler but less accurate than the Abbe refractometer are the hand
refractometers, an example of which is shown in Fig. 9.
Fig. 9—Hand refractometer by Atago Optical Works, Japan.
Tables have been prepared which show the relationship between the
concentration and the refractive index of sugar solutions. This relationship
varies only slightly for different sugars, so the refractometer is quite satis-
factory for determining the total sugars present in a solution of mixed sugars.
With respect to speed, ease of manipulation, and amount of sample required,
the procedure is superior to specific gravity methods. As recently as 19(H)
ICUMSA has adopted new equations developed by the Physikalisch-Techni-
sche Bundesanstalt in West Germany. These now form the basis of the
International Table of Refractive Indices (1966) of sucrose solutions from 0
to 85 per cent. The new table is very similar to the former table based on
work by Schonrock; however, precise refractive index values can now be
obtained to the fifth and at lower concentrations, the sixth decimal place.
The new table of refractive indices of sugar solutions at 20 0 C in air at
20 0 C, 760 mm pressure and 50 per cent relative humidity is found in Table
VII. Where it is necessary to correct refractometer results for temperature,
this is done by converting the refractometer reading to its corresponding
Brix value and applying the corrections for refractometer Brix shown in
Table VIII. As ICUMSA has not yet studied temperature corrections in
detail, the values shown in Table VIII are still the original ones based on
Schonrock's work.
With impure sugar solutions, such as low-grade molasses, it is found
that the refractive index affords a closer approximation to the actual amount
of dry substance present than does the specific gravity. The percentage dry
matter in massecuites or moist sugars can be determined with the refracto-
meter after dissolving all soluble matter in a known amount of added water.
Since the refractometer indicates the amount of dissolved solids only, any
insoluble matter which is present will introduce an error in the estimation of
dry substance. Where dark-coloured solutions are being examined, it is often
difficult to eliminate completely the effects of dispersion. This may be correct-
ed in some degree by dilution with water, but with impure solutions an error
is introduced just as is the case with specific gravity determinations. A close
approximation is obtained if a solution of pure sugar is used for the dilution.
Most modern refractometers can be obtained with a Brix scale for the
direct determination of the Brix of sugar solutions. The hand refractometer,
of which one type is illustrated in Fig. 9 is useful for the approximate checking
of Brix, particularly for maturity testing in the field. The model illustrated
is of the double prism type and is to be preferred to the single prism instru-
ments which are also available. In both cases, when a sample is introduced,
the eye placed to the telescope will see a division line between light and
dark fields superimposed on a scale of the type shown in Fig. 10. The scale is
read at the junction of the two fields. These instruments are made to cover
various ranges of Brix, e.g., 0-30°, 0-50°, 40-80°.
So long as an adequate number of sticks is suitably sampled, it is possible
to obtain a reasonably accurate estimate of the dry substance present in the
juice from a crop, and the concentration of solids from the several portions
of the stalk of cane provides a useful guide in the determination of the state
of maturity of the crop. The instrument is also of great value in affording a
rapid estimate of the relative sugar content of large numbers of cane seedlings
when these are being selected for further trials.
Fig. 10—Typical field of a hand refractometer.
Automatic Refractometers
Although automatic refractometers are not yet used in the Australian
Sugar Industry, they have found wide use in the sugar industry overseas.
Three methods are commonly used for measuring the effect of a liquid on a
light beam directed at the liquid surface:
(i) the lateral shift, or sometimes the dispersion, of the transmitted
beam as a result of refraction.
(ii) the position of the critical angle (the angle of incidence for which
the emergent beam is tangential to the interface).
(iii) the intensity of the reflected beam for angles of incidence less than
the critical angle.
Measurement of refractive index by the "transmission principle" (i) is
possibly the most precise of the three methods; however it is only suitable
for light coloured solutions. For dark coloured solutions it is essential to use
small measuring cells and this can cause difficulty if any particulate matter
is present. Automatic refractometers using the "critical angle principle" (ii)
of operation are generally the most robust for process control work and are
claimed to be unaffected by aeration, turbidity, and colour. Automatic
refractometers working on the "reflected light principle" (iii) are widely used
as Brix controllers on clear factory streams. They are however usually affected
by aeration, turbidity and colour.
The principle employed by the Waters Inline Refractometer which works
on the critical angle principle is described as follows:
A light beam from an incandescent lamp is directed through a lens to a
glass prism in contact with a liquid sample. The beam is refracted at the
interface between the prism and the process fluid and directed back through
a beam deflector to two cadmium sulphide photocell detectors. As the re-
fractive index changes the critical angle changes causing more or less light
to fall on one photocell detector. The other photocell (comparison cell)
remains in the full intensity portion of the beam. As the light changes on the
detector cell, a signal is generated by the photocells and amplified, causing
a servo motor to drive a glass restorer plate in the beam. The amount of
movement of the glass required to restore the beam to a null balancing posi-
tion is a measure of the process stream concentration. Prisms covering
different refractive index ranges are available.
There are many automatic refractometers currently available from well
known manufacturers throughout the world.
Polarized Light
Linearly polarized light, in which the vibration occurs entirely in one
plane, is one type only of polarized light. The vibration may be in two dimen-
sions, at right angles to the direction of travel. Thus it can be a circular
vibration around the direction of travel, and, in the most general case, vibra-
tion in an ellipse. If all the light in a beam has its vibrations following the
same figure (straight line, circle or ellipse) the light is polarized, either
linearly, circularly, or elliptically. Natural light is not polarized, but consists
of a random mixture of all polarizations.
In practice, linearly polarized light is the most important. It is obtained
from natural light by means of a polarizer, a system that transmits vibrations
in one direction only. Since the random vibrations of natural light can be
resolved into two components along two directions at right angles and these
two components are, on the average, equally intense, a perfect polarizer will
transmit half the intensity of natural light.
The light reflected from the boundary between twro transparent media
is linearly polarized for a certain angle of incidence, but only a small part of
the intensity is reflected. A more efficient polarizer is made from dichroic
films. A dichroic material is one that transmits light linearly polarized in a
certain direction (with respect to the orientation of the material molecule)
and absorbs that polarized in the direction at right angles. The early experi-
ments on polarized light used the dichroic crystal tourmaline as polarizers.
As it proved difficult to produce large dichroic crystals artificially, later
polarizers have been made from small crystals embedded in a plastic sheet,
all aligned in the same direction by stretching the sheet. This is the original
form of Polaroid, the crystals used being herapathite or iodosulphate of
quinine.
These microcrystalline sheet polarizers are now quite obsolete. The
present-day polarizers made by the Polaroid Corporation use a molecular
dichroic material. A sheet of polyvinyl alcohol is stretched to align the
molecules and then its surface converted into a dichroic material by treat-
ment either with iodine or oxygen to give two types of Polaroid, called H or K
sheet. For use in optical instruments, the sheet polarizer is cemented between
discs of glass. Other manufacturers such as Zeiss in Germany and Barr and
Stroud in Scotland also make sheet polarizers.
The properties of sheet polarizers vary somewhat, depending on the
dichroic material used and how much of it there is on the sheet. All absorb
some of the linear polarization that they should transmit and transmit a
small amount of the polarization they are intended to absorb. Good sheet
polarizers, however, are now as good as the polarizing prisms described later
and are gradually replacing these prisms in polarimeters and other optical
instruments.
Prism polarizers are made of transparent crystals that have the property
of being birefringent or doubly-refracting. The crystal commonly used is calcite
or Iceland spar, a clear form of calcium carbonate that cleaves readily into
rhombohedra. If an object is viewed through such a crystal, a double image
is seen. Both images are found to be linearly polarized with their polarizations
at right angles. The crystal thus splits natural light into two linearly polarized
rays and refracts these rays in different directions. (A dichroic crystal does
the same splitting, but it absorbs one ray).
Each crystal has a direction known as the optic axis, fixed with respect
to the rhombohedral planes, in which both rays have the same refractive
index, 1.658 for calcite. In other directions, one ray still has the same re-
fractive index; it is called the ordinary ray. The other ray, however, the
extraordinary ray, has a refractive index that varies with direction from
1.658 to 1.486 and so does not obey the simple law of refraction. In Fig. 11 the
effect of sending a beam of light through a crystal of calcite is illustrated.
Fig. 11—Illustrating double refraction of light in calc spar.
The natural light is split into two polarized beams that leave the crystal
with a slight separation, about 1/9 of the thickness of the crystal. This separa-
tion is usually too small to be useful for making a polarizer, and before such
a crystal of calcite may be utilized for this purpose, one set of emergent rays
must be eliminated. One method is to use the phenomenon of total internal
reflection. This is usually accomplished by the method devised by Nicol.
A crystal is selected (Fig. 12) of which the length is about three times the
width. Wedge shaped sections are cut or ground from each end of the crystal
so as to reduce the acute angles GBC and FDA from 71° to 68°. The crystal
is then halved in the direction AC, at right angles to the modified faces. The
cut surfaces are next polished and reunited with Canada balsam which has a
refractive index about 1.54. A beam of light PR entering such a crystal
Fig. 12—Illustrating the principle of the Nicol prism.
(Fig. 12) is resolved into two rays, RO and RE. That which is the more
highly refracted (the ordinary ray, RO) meets the film of Canada balsam AC
at such an angle that it is completely reflected and is thus eliminated. The
e x t r a o r d i n a r y r a y R E i s less h i g h l y r e f r a c t e d , a n d e m e r g e s a s p l a n e p o l a r i z e d
light from t h e e n d surface o f t h e c o m p o s i t e p r i s m .
It should be noted t h a t the separation of the two rays and the elimination
of the ordinary r a y a r e a c h i e v e d b y t h e half p r i s m A B C a n d t h e film o f
Canada balsam. T h e o t h e r half p r i s m A D C s e r v e s o n l y t o r e s t o r e t h e e x t r a -
ordinary ray to i t s original d i r e c t i o n , a n d t o p r o t e c t t h e film o f C a n a d a
balsam.
T h i s early t y p e o f Nicol p r i s m d o e s n o t n e e d t o b e g r o u n d a n d p o l i s h e d
o n t h e o u t s i d e faces, o n l y a l o n g t h e d i a g o n a l — w h e r e t h e t w o half p r i s m s a r e
c e m e n t e d w i t h t h e C a n a d a b a l s a m . I t h a s t h e d i s a d v a n t a g e s o f a s m a l l useful
angle a n d o f d i s p l a c i n g t h e b e a m o f l i g h t t o o n e side. I t i s n o w r e p l a c e d
e n t i r e l y b y r e c t a n g u l a r p r i s m s , w i t h all faces p o l i s h e d . T h e s e a r e , h o w e v e r ,
still s o m e t i m e s called " n i c o l s " .
A s calcite i s a m u c h softer m a t e r i a l t h a n glass, c a l c i t e p r i s m s s h o u l d b e
c l e a n e d o n l y w i t h e x t r e m e c a r e o r t h e y will s c r a t c h . T h e y a r e difficult t o h a v e
r e c o n d i t i o n e d a s t h e p o l i s h i n g o f c a l c i t e i s h i g h l y specialized o p t i c a l w o r k
and each prism m u s t be separated then re-cemented with a cement of index
s u i t a b l e to t h e p r i s m a n g l e . A s i m p l e r class of m a i n t e n a n c e is s o m e t i m e s
r e q u i r e d , h o w e v e r , i f t h e b l a c k p a i n t o n t h e side o f t h e p r i s m b e c o m e s d e -
tached. This paint is important as it absorbs the ordinary ray and so prevents
i t b e i n g s c a t t e r e d b a c k b y t h e g r o u n d surface.
A c o m b i n a t i o n of t w o p o l a r i z e r s in series is t h e b a s i s of a p o l a r i m e t e r .
W h e n l i g h t from t h e first p o l a r i z e r (Fig. 13 I) p r o c e e d s to a s e c o n d p o l a r i z e r ,
k n o w n as an analyser, it is c o m p l e t e l y t r a n s m i t t e d if t h e p o l a r i z i n g d i r e c t i o n s
of t h e t w o a r e p a r a l l e l , losses in i m p e r f e c t p o l a r i z e r s b e i n g n e g l e c t e d . If,
h o w e v e r , t h e a n a l y s e r i s r o t a t e d a b o u t t h e l i g h t b e a m (Fig. 1 3 I I ) , t h e i n t e n s -
i t y o f t h e e m e r g e n t l i g h t will d e c r e a s e u n t i l t h e t w o p o l a r i z i n g d i r e c t i o n s a r e
a t r i g h t angles, w h e n t h e light i s e x t i n g u i s h e d . I n t h e first p o s i t i o n , t h e p o l a r -
izers a r e s a i d to be parallel: in t h e second, t h e y a r e s a i d to be crossed.
I. Parallel Nicols.
II. Crossed Nicols.

Fig. 13—Illustrating the principle of polarizer and analyser.
W h e n linearly polarized light passes t h r o u g h a birefringent crystal, it

also c a n b e split i n t o t w o r a y s w i t h different r e f r a c t i v e i n d i c e s . I f t h e c r y s t a l
is thin, these rays are not noticeably separated and recombine as t h e y leave
t h e c r y s t a l . B e c a u s e o f t h e i r different s p e e d s , h o w e v e r , t h e y d o n o t r e c o m b i n e
in s t e p a n d , i n s t e a d of l i n e a r l y p o l a r i z e d l i g h t , e l l i p t i c a l l y p o l a r i z e d l i g h t is
obtained.* E l l i p t i c a l p o l a r i z a t i o n c a n also b e o b t a i n e d i f l i n e a r l y p o l a r i z e d
light passes through strained glass. Glass is not ordinarily doubly refracting
but, when strained, because of poor annealing or a mount that introduces
strain, it becomes slightly birefringent.
Optical Activity
Quartz is also a crystal that is birefringent with about one-twentieth the
birefringence of calcite. As with calcite, this effect is greatest in directions at
right angles to the optic axis. Along the optic axis, however, a new effect
occurs; if linearly polarized light is sent through a crystal of quartz in this
direction, the angle at which the light is polarized is changed. The amount of
change depends on the thickness; the direction of polarization can be
imagined as rotating around the ray like a corkscrew as the light proceeds
through the quartz.
This property of rotating the plane of polarization is known as optical
activity. It is possessed by certain crystals and also by some liquids and
solutions, including sugar solutions. Materials such as glass that are not
ordinarily optically active, can rotate the plane of polarization when they
are placed in a magnetic field; this is known as the Faraday effect.
The amount of rotation depends directly on the thickness of the sample
through which the light passes and, in the case of a solution, on the concentra-
tion of the optically active substance in the solution. It also depends on
temperature and wavelength, so these must be specified. An active substance
in solution is characterized by its specific rotation a, i.e. the rotation of a solution
of unit concentration and 1 decimetre length. For the D line at 20 °C this
20
is written ay-. If a sample has a concentration c (in g per 100 ml, weighed in
vacuo) and a length / (in dm), the angular rotation will be
20
0 = a ^ C //100,
6 being measured in degrees. In the case of the Faraday effect, the amount
of rotation depends on the field strength and its length, and therefore for an
electromagnetic coil, on the current in the wire and the number of turns.
A normally non-optically active substance, such as glass or air, when placed
in an electromagnetic coil is characterised by its Verdet constant V, i.e. the ro-
tation caused by the substance in unit field strength and 1 decimetre long. As
20
above the angular rotation can be expressed as 6 — V — H Z/100, where H
is the field strength in gauss. The measurement of this rotation is the tech-
nique of polarimetry; it is a method of measuring the concentration of a
substance of known specific rotation when placed in a tube of known length.
Sucrose +66.54 Laevulose —92.5

Dextrose +52.5 Invert —20.0
A solution of sucrose or dextrose, which has a positive specific rotation,
rotates the plane of polarization in a clockwise direction when viewed towards
the light source, and is said to be dextrorotatory. Laevulose, on the contrary,
rotates the plane in an anti-clockwise direction and is said to be laevorotatory.
Crystals of quartz occur in two different forms that are either dextro- or laevo-
rotatory. They are called right-handed and left-handed quartz. In the case
of the Faraday effect, the direction of rotation depends upon the direction
of the magnetic field and therefore for an electromagnetic coil on the direction
of the current in the coil.
In any method of polarimetry, the solution is placed in a cell of known

length between two polarizers. In a polarimeter, these are set crossed with
the cell empty and the extra rotation of the analyser, required to restore
extinction after the sample is introduced, measures the rotation of the sample.
In a saccharimeter, the analyser is not rotated, but the rotation due to the
sample is compensated by the rotation in a plate of quartz of variable thick-
ness. In certain automatic polarimeters, the same principle of balancing is
used, but instead of quartz, a rod of glass in a variable magnetic field gives a
Faraday rotation; the current used to produce the field indicates a measure of
the sample rotation.
The variation of rotation with the wavelength of the light used is known
as rotatory dispersion. It has the practical result that measurements of rota-
tion must be made with monochromatic light, as are measurements of re-
fractive index. Traditionally, the D line of sodium has been used, but there
is a modern tendency to use the e line of mercury (5461 A) for very accurate
measurements; it must be remembered that the specific rotations for these
two lines are quite different. Thus a polarimeter is used with either a sodium
or mercury lamp. In a saccharimeter, the quartz and sugar solution have
similar rotatory dispersions, at least in the red-to-yellow part of the spectrum,
so that white light that has been passed through an orange filter can be used.
The Polarimeter
The essential parts of a visual polarimeter are shown in Fig. 14. An
aperture B is illuminated by a source of monochromatic light C, either directly
or through a lens which focuses C on B. The light passes on through a fixed
polarizer P, with a field stop F, and the analyser A which may be rotated;
Fig. 14—Showing the essential parts of the simple polariscope.

the latter is fitted with a scale S on which the rotation can be read. It is
usually graduated so that the crossed position of the analyser corresponds
to the zero of the scale. The light is viewed by the eye E of the observer.
If a cell X containing an optically active solution is now placed between the
polarizer and analyser, it will be found that the light is no longer extinguished
by A, which will have to be rotated to a new orientation to restore extinction.
The angle through which the analyser is rotated is the rotation of the speci-
men. The scale 5, as well as being marked in angular degrees, is often also
marked in terms of the International Sugar Scale discussed later.
A simple polarimeter of this type would not be very accurate, for setting
an instrument to extinguish light cannot be done with high precision. It is
well known in the technique of measurement that a setting to a maximum
or a minimum, such as this, is less precise than a balancing of two quantities
to equality or coincidence; for example, setting a needle on a scale division,
aligning a line to a crosswire, or matching the intensity of two adjacent fields
of view. Settings of this last type are known as null settings.
The eye looking through the polarimeter has a field of view located at
the stop F near the fixed polarizer. To convert the instrument into an
instrument with a null setting, this field is split into two parts as shown in
Fig. 15 or in some cases into three parts. The polarizations of these two regions
are in directions that differ by a small angle (when three regions are used, the
two outer ones are polarized in the same direction and the centre one is
different) so that, as the analyser is rotated, first one field, then the other is
extinguished. When the analyser is crossed with the direction midway between
the two polarizations, the two fields have equal intensity. A setting to this
position is thus a null setting and is much more accurate than a simple
setting to extinction.
I II III
Fig. 15—Illustrating the principle of the Lippich polarizer for double field.
The three-field alternative has an even greater sensitivity but, if the

two outer fields are not polarized exactly in the same direction, it loses its
advantage, since two balance-points are obtained. Under ordinary laboratory
conditions, the simpler two-field balance is preferable.
The angle between the polarizations of the two fields is known as the
half-shadow angle. Theory shows that, the smaller the half-shadow angle used,
the greater is the sensitivity of the instrument. However, the smaller this
angle, the closer the two sides of the field are to extinction at the balance
point, and the less light there is available to judge the balance. Since the
sensitivity also depends on the light intensity, when the light source is as
bright as can be obtained, a compromise is required on the half-shadow angle
between the loss of sensitivity due to too large an angle and the loss due to too
little light. In practice angles of 1° to 10° are used. In the saccharimeter
described later an angle about 7° to 8° has been found a good compromise
for accuracy and available light.
There are several methods used to make polarizers that give a split field.
The simplest to understand are forms of the Jellet-Cornu polarizer. Imagine
a polarizing prism with a narrow-angle V taken longitudinally from its centre.
The two separate prisms are then cemented together to give two adjacent
polarizers with a fixed half-shadow angle, the angle of the V cut. Another
polarizer with a fixed half-shadow angle is made from two long natural
rhombs of calcite; this is one example of the use of the rhomb itself, instead
of a prism, to separate the ordinary from the extraordinary ray.
The most common method of obtaining the split field is the Lippich
polarizer, shown in Fig. 16. In front of the main polarizer is placed a smaller
polarizer covering half the field. This is rotated through the half-shadow
angle from the main polarizer. This rotation changes the direction of
polarization across this half of the field and also slightly reduces the
intensity. The reduction of intensity affects the posit-

ion of the setting slightly; it is no longer exactly
midway between the angles at which the two fields
extinguished. The small polarizer is also tilted slightly
so that the observer does not look along its face (and
hence see a broad band separating the two fields) but
sees only a sharp edge. When the triple field is used,
two such small polarizers are employed.
The Lippich system has the advantage that the
half-shadow angle is adjustable and can be altered to
suit the intensity of the illumination. When it is
altered, however, there is an alteration of the zero
point of the analyser. But, in the Bates Fric sacchar-
imeter a special set of gears is fitted so that, when
the large polarizer is rotated to change the half-
shadow angle, the analyser is rotated by the amount
required to correct for the change in zero point.
The need to use monochromatic light with a
polarimeter was a great practical disadvantage when
it had to be obtained by feeding metal salts into a
flame. Now spectral lamps, such as sodium and
mercury, are readily available and easy to use. Most
of the visible light from the sodium lamp is in a pair
of orange lines, called the D line, and it is usually
used with a yellow filter to cut out the light from a
fainter pair of green lines. Sodium lamps have a fixed,
rather low brightness.
Mercury lamps can be obtained with a wide
range of brightness. The bright, high-pressure lamps,
however, give broadened spectral lines and this can
cause errors. Thus for polarimetry, a low-pressure Fig. 16—Showing the
construction of
mercury lamp is required with a filter to separate out Lippich polarizer for
the green e line. double field.
The Saccharimeter
Formerly a saccharimeter was considered to be a polarimeter graduated
not in angular degrees but in relative concentration of sugar or degrees of
sugar o S. However some polarimeters today have both angle and sugar scale
graduations and modern automatic polarimeters can be arranged to display
the rotation in any chosen unit. This applies equally whether the sample
rotation is compensated by turning the analyser prism, or by placing a suit-
able amount of optically active substance, such as a piece of quartz, or a
glass rod in a magnetic field, immediately before a fixed analyser.
Therefore it seems best to describe a polarimeter with a sugar scale
merely as a sugar polarimeter and to confine the term saccharimeter to an
instrument which by virtue of its principle of operation should be used only
on sucrose solutions.
As a result, it is becoming common, therefore, to reserve the name
saccharimeter for an instrument that uses quartz wedges for compensation.
When a polarimeter is designed specifically for use with sucrose solutions,
that is, as a saccharimeter, it becomes possible to adopt an alternative means
of eliminating the ill-effects of rotatory dispersion and the need to use rather
low intensity spectral lamps. (When white light is used with a simple polari-
meter, no extinction is obtained since different colours are rotated different
amounts.) By chance, quartz has practically the same rotatory dispersion as
sucrose solution. The rotation produced by the sugar is balanced out by a
quartz compensator, wavelength by wavelength, and extinction can now be
obtained with white light. The extinction is improved further if the blue end
of the spectrum, where the dispersions match worst, is not used. The light is
therefore filtered through a bichromate filter (15 mm thickness of a 6 per cent
solution of potassium bichromate) or a plate of glass having similar trans-
mittance characteristics.
The quartz compensator consists of two wedges of quartz of equal angle
mounted so that one can be moved past the other, as shown in Fig. 17. The
pair of wedges then acts as a parallel-sided plate of quartz of adjustable
Fig. 1 7—Showing the construction of single wedge quartz compensation.

I Dextrorotatory system. II Laevorotatory system.
thickness and it gives a controlled rotation to the light going through it.
This rotation is never zero, since the plate formed by the two wedges can
never be zero thickness. To obtain zero rotation, the wedges are "backed off"
by a fixed plate of quartz of the opposite hand; i.e. if the wedges are made of
left-handed quartz, this plate is right-handed. This system, known as a
single-wedge compensator, is the one most commonly used in commercial
saccharimeters.
The optical system of a saccharimeter is shown in Fig. 18. The lens a
condenses white light from a clear filament lamp, with a ground glass disc
in front of it, on the aperture in b; the light is brought to a focus at the objec-
tive of the telescope by a lens c; d is the polarizer (with fixed half-shadow
angle); e is a stop to limit the size of the light beam and / a glass protecting
Fig. 18—Illustrating the parts of a saccharimeter.
plate. The sugar solution under examination is contained in the cell g; h is a

second protecting plate; i and m are stops for cutting out stray light; j, k,
and I make up the single-wedge compensator; n is the analyser; o the objective
of the viewing telescope; p a field stop in the focal plane of the eyepiece;
and q and r form the eyepiece of the telescope.
Two separate optical parts of the instrument are thus in dust-proof
enclosures, protected from juice splashes by the optically inactive protecting
glasses. The whole system is mounted in a rigid metal tube which is held
horizontal on a stand. Formerly, saccharimeters were supplied for both
200 mm and 400 mm sample cells but the former has almost disappeared
from the modern sugar-mill laboratory; the longer cell is needed for such
solutions as bagasse extracts, which are of low optical activity. On the
latest models (Fig. 19) the lamp housing is built on as an extension to the
instrument so that the light source is fixed in relation to the instrument and
is held in its correct position. With the Schmidt and Haensch instrument a
small focusing disc is provided. This is placed at the end of the trough
towards the analyser, and if the light be correctly placed, a sharp image of
the filament of the lamp will coincide with the horizontal diameter marked
on the disc. The ground glass disc with which the lamp is fitted should, of
course, be removed when making this test.
The scale is usually graduated from —30 °S through zero to +105 °S
(with extended graduations at both ends), or occasionally, from —150 °S
to +150 °S. The angular rotation that corresponds to 100 °S depends on the
length of cell used, the normal weight specified for the instrument, and on the
wavelength for which the rotation is measured.
Fig. 19—Illustrating a Schmidt and Haensch saccharimeter.

The scale is viewed through a low-
power microscope, being illuminated by
some of the light that has been deflected
from the main path. Two types of scale
are now in common use. The type em-
ploying a vernier is illustrated in Fig. 20.
It will be observed that the main scale is
graduated at intervals of one degree of
sugar. A centre-zero vernier is provided,
one side for positive readings and the
other for negative, both divided to read to
0.1 °S. In Fig. 21 is illustrated the scale
employed in the current Schmidt and
Haensch saccharimeter. The scale moves
vertically as opposed to the former hori-
zontal scale and the main scale is divided Fig. 20—Illustrating the double
into 10 °S divisions. A fixed engraved scale vernier scale of a saccharimeter.
Reading 73.4° S.
Fig. 21—Direct reading scale employed in the Schmidt and Haensch saccharimeter.
Reading 66.3° S.
of 10 °S subdivided into 100 divisions is also provided whereby the reading

may be made directly to 0.1 °S and estimated to 0.02 °S. The zero adjustment
for each scale is carried out as follows:—
In the vernier type scale the field is set to the balance position with the
trough empty and the zero of the vernier is adjusted, with the key provided,
to the zero of the main scale. With the direct reading scale the zero on the
movable scale is set to the zero on the fixed scale first and the field is then
balanced for equal intensity by the knurled knob situated at the base of the
analyser housing. At the balance point the two halves of the field should
appear identical. The appearance of a difference in colours at the balance
point, one side appearing yellowish and the other nearly white indicates the
need for internal adjustment. This should not be attempted by unskilled
technicians.
Effect of Illumination
As stated earlier, the rotatory dispersion of sucrose solution is close, but
not exactly equal to that of quartz, the sugar having the greater dispersion.
Since the difference in the two dispersions is greatest for blue light, the
quartz-wedge saccharimeter is designed for use with white light filtered to
remove the blue end of the spectrum. A movable glass filter, that approx-
imates closely to the characteristics of a six per cent potassium bichromate
solution of 15 mm thickness, is now usually built into the saccharimeter.
This filter transmits red, orange, and yellow light but absorbs the rest of the
spectrum; the transmitted radiation has a mean wavelength of about 6000 A.
If white light is used without a filter, a saccharimeter will give readings
that are in error by about +0.12 °S at the 100 °S point. Only when the
solution is coloured and acts as its own filter should the filter be omitted.
If a sodium lamp is used with a quartz-wedge saccharimeter, there is again a
small error, now about 0.03°S at 100 °S, whether a filter is used or not.
Automatic Polarimeters
The modern tendency in optical measuring instruments is to replace
the eye by some photoelectric detector. Such instruments do not require as
highly skilled an observer and are less fatiguing to use. In addition, the
results obtained are more reliable and often more accurate and, being in the
form of an electrical signal, can be recorded by means of the large variety
of data-recording equipment now available. If calculations are made on the
results, this is done by connecting in the appropriate calculating circuits
and the result is obtained with very little delay. An automatic polarimeter
is normally used with a flow-through cell so that samples can be readily
introduced and flushed away; many installations use an automatic sample
feeder which introduces samples to the instrument at regular intervals of,
say, 60 seconds and actuates the read-out device. Certain instruments allow
the polarisation to be recorded continuously as the sample flows through the
cell. However, the precision of the measurement usually surfers seriously as
a result of striations.
A photoelectric polarimeter could be made by using a conventional
split-field polarizer and taking the light from each half of the field to a
separate photocell. At the balance point, the two electrical signals from the
photocells would be equal. Such a system would give continuous d.c. signals
from the photocells and would require d.c. amplifiers, which are notoriously
more unreliable and more unstable than a.c. amplifiers.
Modern automatic polarimeters, therefore, use a.c. balancing. Instead
of a field split in space and two photocells, one photocell is used with a field
"split in time". The plane of polarization changes backwards and forwards
between the two positions it would have for the split field, either in jumps
or continuously. The electrical signal from the photocell then consists of a
d.c. background superimposed on which is an alternating current of the
same frequency as that at which the polarization is being switched. This
a.c. component of the signal is an error signal: it becomes zero at balance.
The instrument balances itself by using the error signal to drive the
balancing system; when the error signal vanishes, this drive stops. It is thus
a servo-system.
To oscillate the direction of polarization one of three methods is used.
The first, employed by Schmidt and Haensch and also by Perkin Elmer in
their automatic saccharimeters and polarimeters, uses a synchronous motor
coupled to the polarising prism, which is caused to rotate backwards and
forwards so that the direction of polarisation oscillates. The second, used
by the National Physical Laboratory (N.P.L.) in the standard polarimeter
that they use to calibrate quartz control plates and also by Jobin-Yvon,
has a rotating plate, around the edge of which is a series of holes, each
covered by a quartz plate. These plates are of equal thickness and alter-
natively left- and right-handed. As the plate rotates, these quartz plates
pass in turn in front of the polarizer to give a direction of polarization that
switches first to the left, then to the right. Hilger and Watts use a similar
system consisting of a vibrating reed supporting and oscillating two pieces
of quartz side by side, one left-handed and the other right-handed, and
oscillating them across the light beam.
The third method makes use of a Faraday cell and is employed by Zeiss
and Jouan. It is also used in the polarimeter designed by N.P.L. which is
made by Thorn Bendix. As stated earlier, if a glass rod with light passing
through it is placed in a magnetic field, the field being in the direction of the
light, the plane of polarization of the light is rotated by an amount that de-
pends on the type of glass and the strength of the magnetic field. Very dense
flint glasses give the largest rotation. The sense of rotation depends on the di-
rection of the field and, if this is alternated, the rotation alternates. To give an
oscillating direction of polarization the glass rod is enclosed in a solenoid
through which passes an alternating current.
The polarimeter is balanced in one of three ways, corresponding to the

above methods of modulation: Either a conventional analysing prism is
rotated (Hilger and Watts, Zeiss, Perkin Elmer), or compensating quartz
wedges are driven up and down (Schmidt and Haensch, Jobin-Yvon), or a
d.c. Faraday cell is used as a compensator to balance the rotation due to the
sample (Bendix, Jouan). The rotating analyser is turned to balance by a
motor that is driven by the amplified error-signal, and the rotation can be
read from an angle scale by an electrical method e.g. by using a potentiometer.
In the Hilger and Zeiss instruments a digital output of the rotation in sugar
degrees is obtained using a shaft encoder. The compensation quartz wedges
are driven to balance by a motor in a similar fashion to the rotating analyser,
and the sugar value of the rotation of the sample is read from a linear scale.
(The Schmidt and Haensch instrument uses moire gratings, for example).
In the Bendix polarimeter, the current in the compensating Faraday cell is
a measure of the rotation.
In the Hilger and Zeiss instruments, the servo motor drives the rotating
analyser at a constant rate, and so the time taken to reach a balance depends
on the range to be traversed: for instance if a cane juice sample reads 90 °S,
the instrument will take twice as long to give a reading if the previous sample
read 70 °S than if it had read 80 °S. In the Bendix instrument the balancing
is done electronically, not mechanically, and equilibrium is approached at an
exponentially decreasing rate. Therefore the time taken to reach balance
depends only slightly on the range to be traversed. The accuracy of the final
setting depends, however, on the time allowed for the equipment to reach a
balance; the longer the time permitted, the higher the accuracy that can be
obtained, until the instrument's limit of accuracy is reached. To be precise,
the accuracy increases as the square-root of the time, so that, to double the
accuracy, the instrument would take four times as long to reach a balance.
The Hilger M560, Zeiss OLD 3 and Bendix-NPL 700 A automatic polari-
meters have been built to comply with the Australian Standard Specification
for an Automatic Sugar Polarimeter, AS K157 - 1968. Australian Standard
Specification AS K157 - 1968 "Automatic Sugar Polarimeter" covers the
requirements which are considered desirable for an automatic sugar polari-
meter suitable for use in the analysis of cane juice and sugar products
in Australian sugar factories. It was approved by the Standards Association
of Australia in 1968. They have a range of —120 °S to +120 °S with a digital
readout to 0.01 °S, and are suitable for cane juice, raw sugar and molasses.
Most of the other commercially available automatic polarimeters are built
for the European beet sugar industry, and have a range of 0 to 30 °S or 0 to
100 °S, with a readout to the nearest 0.05 °S or 0.10 °S.
The Hilger and Zeiss instruments are basically automated verisons of
conventional polarimeters. Their components are shown in Figs. 22 and 23,
respectively.
The Hilger M560 polarimeter normally uses a mercury vapour lamp
and an absorption filter to provide monochromatic radiation of 546 nm.
However, it can be fitted with a sodium light source. The light is linearly
polarised by a calcite prism of the Lippich type. A small oscillating biplate
of left- and right- rotating quartz modulates the beam, which passes through
the sample, normally contained in a 200 mm tube, and on to the analyser
prism and the photomultiplier. Jacketed flow-through cells are available,
and the tube trough is also provided with a water jacket for more effective
temperature control. The "out of balance" signal from the photomultiplier
is amplified and used to drive a servo motor which rotates the analyser prism
until balance is reached. The shaft of the servo motor also drives the electro-
SCHEMATIC LAYOUT OF
M560 AUTOMATIC
POLARIMETER
Fig. 22—Schematic layout of Hilger M560 automatic polarimeter.
mechanical digitizer disc; this consists of a number of miniature commutator

type brushes which touch contacts on an opposing fixed disc. This instrument
is not being commercially produced.
The Zeiss OLD 3 polarimeter uses a mercury spectral lamp and an
interference double-band filter for a wavelength of 546 nm. The light is
polarised by a prism of the Glan-Thompson type, and then passes through a
Faraday modulation coil. The modulator rod is made of special stress-free
glass, 50 mm long; the modulation is at 50 Hz and the angle is about ± 2 ° at
Fig. 23—Diagram of Zeiss OLD digital polarimeter.

546 nm. The modulated beam then passes through a sample cell, 98.13 mm
long; this length being chosen so that 100 °S is equivalent to 20° of angle.
Jacketed flow-through cells are available, and the sample space is also pro-
vided with a water jacket for more effective temperature control. From the
cell the light passes through the analyser prism to the photomultiplier. The
Zeiss is a full circle polarimeter; the analyser is permanently coupled to an
analogue-digital convertor (shaft encoder) with 5 decades and a transmitting
potentiometer. The two decades representing the most significant figures
(tenths and hundredths of a sugar degree) are photoelectric: the other three
decades are electro-mechanical with suitable reduction by epicyclic gears.
The components of the Bendix-NPL polarimeter are shown in Fig. 24.
Since the instrument uses a magnetic field to give the balance, it is itself
sensitive to the earth's magnetic field and, if horizontal, the reading given
Fig. 24—Diagram of Bendix-NPL automatic polarimeter Type 700.
would change if the instrument were turned around on a table. It is therefore

made upright so that it always stands vertical at a constant angle to the earth's
field (at one place). In addition it is made of non-ferrous metals. It should be
kept away from large pieces of iron or steel during use since, if these are
moved near it, the field through the Faraday compensation coil could be
changed in the middle of a measurement. Road traffic closer than 15 ft may
also affect the reading.
The light source, a filament lamp with a stabilized electrical supply, is at
the top. This light is passed through an interference filter to give a band of
mean wavelength corresponding to the mercury e line (546 nm), with a band
width at 50 per cent transmission of about 20 nm. An interference filter can
be fitted to give a mean wavelength corresponding to the sodium D line
(589 nm). The light then passes through two stops and a condenser lens,
which control the beam size, the polarizer (a sheet polarizer), and the first
Faraday cell (the modulator cell). An alternating current through the coil of
this cell provides the required oscillation of the direction of polarization
about the direction given by the polarizer. A modulation frequency of 380 Hz

is chosen because it is not harmonic with either 50 Hz or 60 Hz.
Below this Faraday cell is the compartment for the sample cell. This is
much shorter than those used with visual polarimeters and saccharimeters.
The Faraday cell type of automatic polarimeter is much more precise than
the visual type instrument for the measurement of angle; it can therefore use
a shorter sample and still achieve the same precision in terms of the sugar
scale. The shorter cell is really forced on the instrument; a large range of
rotations cannot be covered because of the limitation in rotation imposed
by the Faraday compensator cell.
Below the sample chamber is the compensator which is followed in turn
by the fixed analyser and photomultiplier. The polariser and analyser are
normally in the crossed position, and when modulation is applied the intensity
of light reaching the photomultiplier varies sinusoidally. In one period of
oscillation the plane of polarisation passes twice through the null position,
and the light intensity at the photomultiplier therefore has a frequency of
760 Hz. The output signal from the photomultiplier includes a 760 Hz in-
balance component, and a 380 Hz out-of-balance component when a sample
is introduced.
The signal is fed to the input of a selective amplifier in the electronic
unit. The amplifier only accepts a narrow band of frequencies centred on
380 Hz. After passing through a phase sensitive detector, followed by recti-
fication and amplification, the out-of-balance signal is fed back to the
Faraday compensator cell until null balance is restored. The current in the
compensator is then a measure of the rotation, which can be read from a
meter on the electronic unit, recorded on a separate chart recorder, or fed to
and displayed on a digital voltmeter from which a print-out or punch-out can
be obtained.
The small Bendix Model 143 C polarimeter covers a range of rotations
of ±.5° and has a sensitivity of 0.0001°. Thus, if the sample cell were 2 mm
thick only, it would allow measurements on solutions up to about 120 °S
(with the mercury e line) to an accuracy of about 0.025 °S; such a thin cell
is very difficult to make accurately. The angular range has been increased
in the large Model 700 A polarimeter by providing water cooling on the
compensator cell so that larger currents can be used without generating too
much heat, and ±.5° of rotation is covered.
In use, the amplifier must be switched on at least 30 minutes before use,
so that it can stabilize. When used frequently, it should be left on continu-
ously, that is 24 hours a day seven days a week. With each set of readings,
it is advisable to check the zero of the instrument with the sample cell
containing distilled water. The coarse adjustment to the zero is done by
rotating the polarizer. An additional Faraday cell between the compensator
and the analyser allows fine control of the zero to be made electrically (see
Fig. 24).
Effects of Birefringence
As stated earlier, materials such as glass become doubly refracting if
they are strained. If linearly polarized light passes through such strained
glass, it may come out elliptically polarized. If it is now followed by an
analyser, the intensity seen varies as the analyser is rotated, but it no longer
drops to zero at any position; the extinction is only partial, not complete.
At the position of minimum intensity, the analyser is crossed with the direc-
tion of the longer axis of the ellipse of polarization. This may not be in the
same direction as the original linear polarization, so that the strained glass
has i n t r o d u c e d a n e r r o r i n t o t h e m e a s u r e m e n t . I t i s n o t possible t o e l i m i n a t e
this e r r o r b y r e - a d j u s t i n g t h e z e r o o f t h e p o l a r i m e t e r since t h e d i r e c t i o n o f
the ellipse a n d h e n c e t h e e r r o r c a n c h a n g e w h e n t h e s a m p l e i s i n t r o d u c e d
and rotates the polarization.
T h e s e e r r o r s d u e t o birefringence c a n b e c a u s e d b y s t r a i n e d glass i n t h e
e n d p l a t e s o f t h e s a m p l e cells o r i n o t h e r p r o t e c t i v e p l a t e s b e t w e e n t h e
polarizer a n d t h e analyser. In visual polarimeters a n d saccharimeters t h e y
a r e n o t u s u a l l y l a r g e e n o u g h t o b e serious, b u t i n a u t o m a t i c p o l a r i m e t e r s ,
w h e r e t h e a c c u r a c y o f angle m e a s u r e m e n t m u s t b e g r e a t e r t o allow for t h e
s h o r t e r s a m p l e , t h e y c a n b e significant. T h e e r r o r s i n t e r a c t s o t h a t s t r a i n i n
glass p l a t e s before a n d after t h e c o m p e n s a t i o n cell c a n g i v e rise t o t w o sets
o f e r r o r s , o n e fixed, t h e o t h e r d e p e n d i n g o n t h e s a m p l e . T o a v o i d birefringence
e r r o r s i n a u t o m a t i c p o l a r i m e t e r s , n o t o n l y m u s t all glass u s e d b e v e r y well
a n n e a l e d , b u t i t m u s t also b e m o u n t e d w i t h o u t s t r a i n a n d c l e a n e d c o r r e c t l y ;
w i p i n g w i t h a c i r c u l a r m o t i o n i n t r o d u c e s less b i r e f r i n g e n c e t h a n w i p i n g
always in the one direction.
Standardization of Polarimeters
J u s t as t h e reading of a refractometer is checked periodically by m a k i n g
a m e a s u r e m e n t on a t e s t piece, a p o l a r i m e t e r s h o u l d be c h e c k e d r e g u l a r l y
w i t h a s t a n d a r d of k n o w n r o t a t i o n . F o r v i s u a l p o l a r i m e t e r s , t h i s is a q u a r t z
c o n t r o l p l a t e , a p l a t e of q u a r t z of k n o w n r o t a t i o n m o u n t e d in a t u b e t h a t
f i t s i n t o t h e p o l a r i m e t e r i n p l a c e o f t h e s a m p l e cell. T h e s e c o n t r o l p l a t e s a r e
n o r m a l l y m a d e close t o 2 5 °S, 5 0 °S, 7 5 ° S a n d 100 ° S a n d t h e l a s t t w o a t
least s h o u l d b e a v a i l a b l e for use. T h e q u a r t z c o n t r o l p l a t e s a r e t h e m s e l v e s
checked by a standardizing laboratory. In Australia, t h e recognized
standardizing laboratories are the National S t a n d a r d s L a b o r a t o r y a n d those
registered by t h e N a t i o n a l Association of Testing Authorities.
Q u a r t z p l a t e s a r e n o r m a l l y u s e d t o s t a n d a r d i z e t h e H i l g e r a n d Zeiss
a u t o m a t i c p o l a r i m e t e r s . T h e a c c u r a c y r e q u i r e d for B e n d i x p o l a r i m e t e r s i s s o
h i g h t h a t q u a r t z c o u l d n o t , i n t h e p a s t , b e g r o u n d a n d p o l i s h e d sufficiently
flat a n d p a r a l l e l for v a r i a t i o n s o f r o t a t i o n t o b e negligible. T h e N a t i o n a l
P h y s i c a l L a b o r a t o r y ( L o n d o n ) h a s recently- o v e r c o m e t h e s e p r o b l e m s , a n d
have a suitable plate available.
The International Sugar Scale

A t t h e 1932 m e e t i n g o f t h e I n t e r n a t i o n a l C o m m i s s i o n for U n i f o r m
M e t h o d s o f S u g a r A n a l y s i s , t h e following r e s o l u t i o n s w e r e a g r e e d t o : —
(1) T h a t t h e C o m m i s s i o n a d o p t a s t a n d a r d scale for t h e s a c c h a r i m e t e r
a n d t h a t t h e scale b e k n o w n a s t h e " I n t e r n a t i o n a l S u g a r S c a l e " .
R o t a t i o n s e x p r e s s e d i n t h i s scale shall b e d e s i g n a t e d a s d e g r e e s
s u g a r (°S).
(2) T h a t t h e p o l a r i z a t i o n of t h e n o r m a l s o l u t i o n (26.000 g of p u r e
s u c r o s e d i s s o l v e d i n 100 m l . , a n d p o l a r i z e d a t 2 0 ° C i n a 2 0 0 m m t u b e ,
u s i n g w h i t e light a n d t h e d i c h r o m a t e filter a s defined b y t h e C o m m i s -
sion) b e a c c e p t e d a s t h e b a s i s o f c a l i b r a t i o n o f t h e 100° p o i n t o n t h e
I n t e r n a t i o n a l S u g a r Scale.
(3) T h a t t h e following r o t a t i o n s s h a l l h o l d for t h e n o r m a l q u a r t z p l a t e
of the International Sugar Scale:—
N o r m a l Q u a r t z P l a t e = 100 °S = 4 0 . 6 9 0 ° ± 0 . 0 0 2 ° (A = 5461 A) at 20°C
N o r m a l Q u a r t z P l a t e = 100 °S = 3 4 . 6 2 0 ° ± 0 . 0 0 2 ° (A = 5892.5A) at 20°C
T h i s definition o f t h e " I n t e r n a t i o n a l S u g a r S c a l e " d o e s n o t h o w e v e r
m a k e mention of t h e rotations of t h e normal sugar solution, at t h e n o r m a l
Fig. 25—Polarimeter tubes, a
Fig. 25 b
Fig. 25 c
Fig. 25 Id
Fig. 25 lid
Temperature Effects.
When a sugar solution is made up and polarized at temperatures other
than 20 °C, the reading obtained will be influenced by the temperature
difference on the instrument, the apparatus used and the substance in solu-
tion. Therefore the reading obtained must be corrected to 20 °C to give the
true polarization in °S of the solution under consideration and in addition
this corrected polarization reading must be corrected further if the solution
was not made up at 20 °C.
R. A. M. Wilson (1965) of the Colonial Sugar Refining Coy. Ltd. has
classified the corrections for temperature effects into the "polarization reading
Tr = T e m p e r a t u r e of s o l u t i o n or q u a r t z p l a t e w h e n r e a d i n g t h e p o l a r i z a -
t i o n (°C)
N = N o r m a l i t y of s o l u t i o n . A n o r m a l s o l u t i o n c o n t a i n s 26g of s a m p l e
in 100 m l
5 = W e i g h t p e r c e n t s u c r o s e in t h e s a m p l e
R = W e i g h t p e r c e n t r e d u c i n g s u g a r in t h e s a m p l e
Tp = T e m p e r a t u r e of p o l a r i m e t e r (°C)
Tm = T e m p e r a t u r e of s o l u t i o n w h e n m a k i n g to t h e m a r k (°C)
T] = C o n s t a n t e q u a l to 1 for q u a r t z w e d g e s a c c h a r i m e t e r s a n d e q u a l to
0 for o t h e r t y p e s of p o l a r i m e t e r s a n d s a c c h a r i m e t e r s
F o l l o w i n g on t h e w o r k of W i l s o n a n d a s u b m i s s i o n to I C U M S A in 1966
b y t h e A u s t r a l i a n N a t i o n a l C o m m i t t e e o f I C U M S A , t h e following simplified
f o r m u l a e w e r e a d o p t e d a s u s u a l l y sufficient for t e m p e r a t u r e c o r r e c t i o n s t o
t h e p o l a r i z a t i o n o f r a w s u g a r . F o r o t h e r p r o d u c t s , for q u a r t z c o n t r o l p l a t e s
a n d for h i g h p r e c i s i o n w o r k , a p p r o p r i a t e f o r m u l a e m a y b e o b t a i n e d b y
suitable combination of the equations above.
F o r quartz wedge saccharimeters the temperature correction to be m a d e
t o t h e observed polarization shall b e : —
(t r — 20) (0.00033 S — 0.004 R)
where
t r (°C) is t h e t e m p e r a t u r e of t h e s o l u t i o n as r e a d in t h e s a c c h a r i m e t e r
S is t h e a p p r o x i m a t e per cent sucrose in t h e s a m p l e
R i s t h e a p p r o x i m a t e p e r c e n t r e d u c i n g s u g a r s (as i n v e r t s u g a r ) i n
the sample.
For sugar polarimeters (without q u a r t z wedge compensation) the correc-
t i o n t o b e m a d e t o t h e o b s e r v e d p o l a r i z a t i o n s h a l l be:-—
(tr — 20) (0.00019 5 — 0.004 R)
w h e r e t h e s y m b o l s a r e a s defined a b o v e .
For accurate work it is desirable t h a t control of t e m p e r a t u r e to 20.0-^
0.5 °C be o b t a i n e d for all p o l a r i m e t r i c a n a l y s e s of n o r m a l s u g a r s o l u t i o n s t h u s
eliminating a n y major t e m p e r a t u r e corrections.
I C U M S A h a s r e c o m m e n d e d t h a t for t h e p o l a r i z a t i o n o f r a w s u g a r t h e
t e m p e r a t u r e of p o l a r i z a t i o n s h a l l be as close to 2 0 . 0 °C as p o s s i b l e a n d in
a n y case i t shall n o t b e o u t s i d e t h e r a n g e 1 5 t o 2 5 °C.
The Spectrophotometer
Q u a n t i t a t i v e m e a s u r e m e n t s based on t h e colour of solutions h a v e been
e m p l o y e d b y c h e m i s t s for m a n y y e a r s . T h e s e m e a s u r e m e n t s , w h i c h a r e
covered by t h e general t e r m colorimetric analysis, m a y be carried out in a
n u m b e r of different w a y s .
T h e simplest m e t h o d s of colorimetric analysis are visual methods, which
m a y i n v o l v e m a t c h i n g of an u n k n o w n c o l o u r w i t h a series of s t a n d a r d c o l o u r s ,
d i l u t i o n of an u n k n o w n colour in a p a r a l l e l - s i d e d t u b e u n t i l it m a t c h e s a t u b e
filled w i t h a s t a n d a r d c o l o u r a n d t h e n c a l c u l a t i n g t h e s t r e n g t h o f t h e u n -
k n o w n s o l u t i o n from t h e h e i g h t s of t h e l i q u i d s in t h e t u b e s , or by t h e use of a
colour c o m p a r a t o r s u c h a s t h e D u b o s c q . A m o r e a d v a n c e d f o r m o f c o l o u r
m e a s u r e m e n t i s o n e w h e r e t h e h u m a n e y e i s r e p l a c e d b y a p h o t o e l e c t r i c cell,
t h u s largely eliminating t h e errors due to t h e personal characteristics of each
observer. I n s t r u m e n t s based on this principle are k n o w n as photoelectric
colorimeters, or, more correctly, photoelectric absorptiometers. These instru-

ments usually employ light consisting of a comparatively narrow range of
wavelengths, and this is achieved by passing white light through filters.
The most modern instruments employed for colorimetric analysis operate
with light of a definite wavelength, with a very narrow band-width, and these
instruments are called spectrophotometers. A spectrophotometer, as its name
implies, is a combination of a spectrometer and a photometer. The spectro-
meter portion of the instrument provides light of any selected colour, by
employing a prism or a diffraction grating, and is usually termed a mono-
chromator, while the photometer portion of the instrument measures the
intensity of the monochromatic light produced.
The spectrophotometer most commonly in use in Queensland mills is
the Bausch and Lomb Spectronic 20, which is shown in Fig. 26. A schematic
diagram of the optical system of this instrument is shown in Fig. 27. The
Fig. 26—The Spectronic 20, Bausch and Lomb
operation of the instrument is as follows:—White light emanating from the

tungsten lamp passes through the entrance slit, being focused by the field
lens onto the objective lens. The objective lens is of such a focal length as to
focus an image of the entrance slit at the exit slit, the reflection-type diffrac-
tion grating being interposed before the exit slit in order to reflect and
Fig. 27—Schematic optical diagram of Spectronic 20.

d i s p e r s e t h e light. T o o b t a i n t h e v a r i o u s w a v e l e n g t h s a t t h e e x i t slit, t h e
grating is rotated, by m e a n s of an a r m which rides on t h e wavelength cam.
In setting the wavelength, the cam rotates t h e grating so t h a t light of t h e
d e s i r e d w a v e l e n g t h p a s s e s o u t t h r o u g h t h e e x i t slit. T h i s m o n o c h r o m a t i c
l i g h t w h i c h p a s s e s t h r o u g h t h e e x i t slit c o n t i n u e s o n t h r o u g h w h a t e v e r
sample m a y be contained in a test t u b e or c u v e t t e placed in t h e light p a t h , a n d
finally t e r m i n a t e s a t t h e m e a s u r i n g p h o t o t u b e , w h e r e t h e l i g h t e n e r g y i s
c o n v e r t e d i n t o a n electric signal. W h e n e v e r t h e s a m p l e i s r e m o v e d f r o m t h e
i n s t r u m e n t , a n o c c l u d e r a u t o m a t i c a l l y falls i n t o t h e l i g h t b e a m s o t h a t t h e
zero m a y b e set w i t h o u t f u r t h e r m a n i p u l a t i o n . A l i g h t c o n t r o l i s also p r o v i d e d
in order t h a t t h e i n s t r u m e n t m a y be set at zero absorbance with a b l a n k or
reference s o l u t i o n i n t h e s a m p l e c o m p a r t m e n t . V a r i o u s o t h e r s p e c t r o p h o t o -
meters are available, some with a wider range of light wavelengths t h a n is
o b t a i n a b l e w i t h t h e S p e c t r o n i c 20, b u t all w o r k o n t h e s a m e p r i n c i p l e o f a
p r i s m or diffraction g r a t i n g m o n o c h r o m a t o r p r o v i d i n g a s o u r c e of m o n o -
c h r o m a t i c light for a light s e n s i t i v e p h o t o t u b e . A c t u a l l y , t o refer t o t h e s e
instruments in terms of "light" is rather misleading, because even the simple
S p e c t r o n i c 2 0 i n s t r u m e n t h a s a scale r a n g e f r o m 3 2 5 n m ( t h e u l t r a v i o l e t
region) u p t o 9 7 5 n m , w h i c h i s well i n t o t h e i n f r a - r e d r e g i o n .
Colorimetry
The operation of such instruments for colour determination is relatively
simple, but several points must be borne in mind, in the interests of accuracy.
Firstly, for the instrument to be stable, the light output from the lamp must
be constant. This requires a stable power supply, and voltage stabilizers may
have to be installed to ensure this, or in some instances battery operation of
the lamp must be reverted to in order to overcome line voltage variations.
Secondly, for accurate results, scrupulous cleanliness must be practised with
the handling of the delicate and expensive glass cuvettes used as sample
containers, and, whenever possible, these cuvettes should be kept in their
matched sets. This last factor will avoid errors caused by standardization of
the instrument with a blank in one cuvette and reading the unknown in
another cuvette which does not have a precisely equal cell width. When using
spectrophotometers for colour measurement the manufacturer's instructions
should, of course, be adhered to, but the procedure basically consists of
setting the wavelength to that specified for the determination, setting the
zero of the instrument, setting the optical density to zero with a blank solu-
tion as sample, and then reading the optical density of the unknown sample.
The concentration of the unknown solution is then read off a standard graph
prepared from solutions of known concentration.
Turbidity Measurement
Spectrophotometers are also used to measure the turbidity of such mill
products as clarified juice. For this determination the wavelength is set to
975 nm, well into the infra-red region, to avoid the effect of juice colour, and
the amount of "light" absorbed, read as an optical density, gives a measure
of turbidity. For convenience, turbidity is usually recorded as one hundred
times the optical density.
The Microscope
In sugar factory operations the most important use of the microscope
is for the examination of proof samples withdrawn from vacuum pans and
for the determination of the sizes of crystals in sugar, massecuite, magma,
seed, etc. For these purposes a comparatively low order of magnification is
required. The microscope also enters essentially into the determination of
saturation temperature by the optical method and has numerous other casual
ACTUAL PATH OF LIGHT.
RAY PATH OF VIRTUAL IMAGE.
i Fig. 28—The essential parts of a microscope.

uses for w h i c h a fairly h i g h d e g r e e of m a g n i f i c a t i o n is r e q u i r e d . H e n c e , w h i l s t

t h e p r o v i s i o n of a s i m p l e low p o w e r e d m i c r o s c o p e for u s e on t h e p a n s t a g e
is u n i v e r s a l l y a c c e p t e d , t h e r e is also n e e d for a m o r e v e r s a t i l e i n s t r u m e n t of
b e t t e r q u a l i t y for l a b o r a t o r y use.
The Structure and Operation of the Microscope

T h e e s s e n t i a l p a r t s of t h e t y p e of m i c r o s c o p e in g e n e r a l u s e in t h e
laboratory are illustrated in Fig. 28. T h e h e a v y b o x of cast metal A s u p p o r t s
a s h o r t rigid u p r i g h t pillar B to w h i c h t h e a r m or l i m b D is h i n g e d at C.
T h e a r m w h i c h i s c o n v e n i e n t l y c u r v e d for e a s y g r a s p i n g b y t h e h a n d w h e n
t h e m i c r o s c o p e h a s t o b e m o v e d f r o m p l a c e t o p l a c e , i s also o f h e a v y m e t a l
a n d t h e h i n g e C s h o u l d allow o n l y a stiff m o v e m e n t in a v e r t i c a l p l a n e a n d
no m o v e m e n t whatsoever sideways. At the upper end the a r m bears the
t u b u l a r b o d y E , w h i c h carries t h e m a g n i f y i n g lenses, a n d j u s t n e a r t h e h i n g e
t h e s t a g e F i s r i g i d l y a t t a c h e d t o it. B e n e a t h t h e s t a g e a n d fitted t o i t i s t h e
condenser G, commonly known as the substage condenser, a n d below t h a t
t h e d o u b l e m i r r o r H , w h i c h i s flat o n o n e side a n d c o n c a v e o n t h e o t h e r .
M o v e m e n t o f t h e b o d y d o w n to, a n d u p from, t h e s t a g e i s p r o v i d e d b y a
coarse a d j u s t m e n t o p e r a t e d b y t u r n i n g t h e milled h e a d I a n d a fine a d j u s t -
m e n t working t h r o u g h a smaller head J. At t h e t o p t h e tubes of most micro-
scopes are fitted w i t h a g r a d u a t e d d r a w t u b e s o t h a t t h e d i s t a n c e b e t w e e n t h e
eye-piece K a n d t h e nose-piece M in w h i c h t h e o b j e c t i v e s N are m o u n t e d ,
c a n b e v a r i e d t o suit t h e r e c o m m e n d a t i o n s o f t h e m a n u f a c t u r e r o f t h e lenses.
T h e eye-piece fits easily i n t o t h e t o p o f t h e t u b e . T h e o b j e c t i v e s d o n o t lit
d i r e c t l y i n t o t h e t u b e , b u t a r e s c r e w e d i n t o a r e v o l v i n g p l a t e called t h e nose-
piece. T h i s m a y h o l d from o n e t o four o b j e c t i v e s . F o r p u r e l y r o u t i n e use a t
t h e o n e m a g n i f i c a t i o n a s i n g l e - o b j e c t i v e nose-piece is q u i t e s u i t a b l e , b u t
w h e n a r a n g e of m a g n i f i c a t i o n is r e q u i r e d t h e m u l t i - o b j e c t i v e nose-piece is
e s s e n t i a l in t h a t it allows t h e r e a d y c h a n g i n g of o b j e c t i v e s w i t h o u t risk of
damage to the object a n d with a m i n i m u m of delay. The substage condenser
is n o t n e c e s s a r y w i t h l o w - p o w e r o b j e c t i v e s (when t h e c o n c a v e side of t h e
m i r r o r p e r f o r m s t h e s a m e f u n c t i o n ) , b u t i t i s e s s e n t i a l for h i g h - p o w e r
o b j e c t i v e s w h i c h m u s t h a v e a c o n c e n t r a t e d b e a m o f i n t e n s e light. T h e
c o n d e n s e r m u s t b e u s e d o n l y w i t h t h e p l a n e m i r r o r , o t h e r w i s e i t loses m u c h
of its efficiency. T h e r a c k a n d p i n i o n g e a r O is u s e d for m o v i n g t h e c o n d e n s e r
u p a n d d o w n a n d t h e r e i s u s u a l l y s o m e p r o v i s i o n for s w i n g i n g t h e c o n d e n s e r
o u t o f t h e o p t i c a l axis w h e n n o t r e q u i r e d . T h e v e r t i c a l m o v e m e n t o f t h e
c o n d e n s e r i s v e r y i m p o r t a n t b e c a u s e t h e s y s t e m o f lenses f o r m i n g t h e
c o n d e n s e r h a s to be focused j u s t as carefully as t h e o b j e c t i v e s if a h i g h -
q u a l i t y i m a g e o f t h e o b j e c t i s t o b e o b t a i n e d . T h e iris d i a p h r a g m P u s e d t o
r e g u l a t e t h e a m o u n t o f light c o m i n g i n t o t h e c o n d e n s e r , i s a n i n t e g r a l p a r t
of it a n d is o p e r a t e d by a s m a l l l e v e r facing t o w a r d s t h e front of t h e i n s t r u m e n t .
General Principle of Operation: By s u i t a b l e p o s i t i o n i n g of t h e m i r r o r in
r e l a t i o n t o t h e c o n d e n s e r a n d t h e s o u r c e o f light, r a y s o f light a r e reflected
from i t a n d i n t o t h e c o n d e n s e r w h e r e t h e y a r e c o n c e n t r a t e d i n t o a m o r e
intense b e a m a n d so pass through the object under examination. This is
m o u n t e d on a glass slide, u s u a l l y m e a s u r i n g 3 x 1 in h e l d firmly by s p r i n g
clips t o t h e s t a g e , a n d for s a t i s f a c t o r y e x a m i n a t i o n s h o u l d b e e i t h e r c o m -
p a r a t i v e l y t r a n s p a r e n t , o r consist o f s m a l l p a r t i c l e s s e p a r a t e d b y clear liquid.
T h e light p a s s i n g t h r o u g h t h e m o u n t e d o b j e c t e n t e r s t h e o b j e c t i v e , t h e
f u n c t i o n of w h i c h is to form an e n l a r g e d i m a g e of t h e o b j e c t for f u r t h e r
m a g n i f i c a t i o n b y t h e eye-piece. T h e front lens o f t h e e y e collects t h e light
r a y s c o m i n g t h r o u g h t h e eye-piece a n d p r o j e c t s a n i m a g e o n t h e r e t i n a w h i c h
t h e b r a i n r e c o r d s a s a n o b j e c t s i t u a t e d a b o u t 1 0 i n a w a y from t h e e y e . T h e
a c t u a l p i c t u r e seen by l o o k i n g d o w n a m i c r o s c o p e is in r e v e r s e a n d if o n e
wishes to move an object from, say, the left edge of the field of view to the
centre, one must move the stage (and slide) from right to left and not left to
right. The same reversal, of course, occurs for other movements also.
Lenses and Magnification: The objectives are the most important com-
ponents of the microscope since on their perfection depends the efficiency of
the instrument. They each consist of a series of lenses in a brass cylinder
and are made to give various degrees of magnification: the higher the magni-
fication the more lenses have to be incorporated, and so the more expensive
the objectives become. The lower powered objectives are known as "dry"
lenses, but objectives giving a magnification of 80 of more are always "oil
immersion", i.e., they can only operate when a film of special oil, having a
refractive index the same as glass, makes contact with both the front of the
lens and the top of the glass slip covering the object. Oil immersion lenses
represent the peak of the lens maker's skill and are essential for critical work
at high magnifications, but they are quite unnecessary for practical sugar-
house control, and the special conditions for their satisfactory use will not be
considered here. Two types of dry lens are obtainable, viz., achromatic and
apochromatic. The aprochromats are more corrected for colour errors in-
herent in any glass magnification system, but their advantage is only appa-
rent in critical work at the higher magnifications and for the practical
requirements of a sugar mill the much cheaper achromats are quite suitable.
Objectives are designated by a number—expressed in inches or milli-
metres, and engraved on the objective—which represents the "focal length"
of the particular lens and indicates its magnifying power. The common
objectives are the 2/3 in (16 mm) or lower power, the 1/6 in (4 mm) or high
power and the 1/12 in (2 mm) which is an oil immersion. The focal length is
measured from a point within the objective so that when the object is in
focus the distance between it and the front lens of the objective is always
less than the focal length. This reduced distance is called the working distance
of the lens and becomes quite an important factor in the use of super-
saturation apparatus.
The table below shows the approximate magnification obtained with
various objectives and eye-pieces:
Objective focal Objective or initial |

length magnification Final magnification
in mm
!
! x 6 eye- piece | X 10 eye-piece
2/3 16 10 ! 60 100
1/3 8 20 120 200
1/6 4 40 240 400
1/12 2 80 480 800
An objective is always designed to be used with a certain tube length,

usually 160 mm, but objectives for a 200 mm length are also obtainable.
Increasing the tube length by withdrawing the sliding drawtube L increases
the magnification of the object, but it does not increase the amount of detail
that can be seen; in other words, the resolution, which is a function of the
objective alone, is not altered. Like the objectives the eye-pieces are also
compound lenses. Their function is to pick up the enlarged image of the
object formed by the objective and magnify it still further. The total magnifi-
cation thus obtained is the product of the objective magnification multiplied
by the eye-piece magnification. Eye-pieces are made with various powers of
m a g n i f i c a t i o n ; x 6 a n d X 10 a r e t h e m o s t c o m m o n , b u t for c e r t a i n w o r k
i n t h e mill i t m a y b e d e s i r a b l e t o o b t a i n o n e w i t h a h i g h e r m a g n i f i c a t i o n .
The a d v a n t a g e of t h e high magnification in t h e eye-piece c o m p a r e d w i t h t h a t
obtained with a higher powered objective a n d a low power eye-piece is t h a t
w i t h t h e former a r r a n g e m e n t t h e w o r k i n g d i s t a n c e i s m u c h t h e g r e a t e r .
Source of Light: W h i l e o r d i n a r y d a y l i g h t , n o t d i r e c t s u n l i g h t , is often
u s e d as a s o u r c e of i l l u m i n a t i o n for m i c r o s c o p i c w o r k , artificial l i g h t is g r e a t l y
t o b e preferred. I t s use allows t h e g e n e r a l l i g h t i n g i n t h e r o o m t o b e r e d u c e d
t o a c o m f o r t a b l e level for m i c r o s c o p e w o r k a n d s o e x t r a n e o u s a n n o y i n g g l a r e
c a n b e e l i m i n a t e d . I t also gives t h e o p e r a t o r c o m p l e t e c o n t r o l o v e r t h e
i n t e n s i t y o f t h e i l l u m i n a t i o n a n d allows t h e m i c r o s c o p e t o b e s i t e d w h e r e v e r
convenient. There are various types of microscope lamps on t h e m a r k e t , some
of t h e m very expensive, b u t a cheap a n d quite satisfactory l a m p can be
easily m a d e b y m o u n t i n g a b u l b , p r e f e r a b l y w i t h p e a r l glass, i n a s m a l l b o x
o r t i n . S o m e v e n t i l a t i o n i s n e c e s s a r y a n d t h e light s h o u l d c o m e o u t t h r o u g h
a piece of g r o u n d glass s e t at t h e s a m e level as, or s l i g h t l y below, t h e f i l a m e n t
of t h e b u l b . A s m a l l h o o d a r o u n d t h e g r o u n d glass will confine t h e light to a
b e a m not m u c h wider t h a n the microscope mirror.
Operation: T h e m i c r o s c o p e m u s t be set on a firm t a b l e or b e n c h at a
c o m f o r t a b l e h e i g h t for t h e o p e r a t o r , a n d v i b r a t i o n f r o m m a c h i n e r y , p e o p l e
w a l k i n g o n t h e floor, e t c . , e l i m i n a t e d a s far a s possible. A n eye-piece a n d t h e
objectives having been placed in position, t h e operator p u t s the microscope
s q u a r e l y i n front o f h i m w i t h t h e m i r r o r facing d i r e c t l y t o w a r d s t h e s o u r c e
o f light. T h e d i a p h r a g m P i s o p e n e d t o i t s fullest e x t e n t a n d t h e p l a n e
m i r r o r a d j u s t e d s o t h a t t h e m a x i m u m a m o u n t o f l i g h t i s reflected t h r o u g h t h e
c o n d e n s e r a n d t h e w h o l e field of v i e w is i l l u m i n a t e d as e v e n l y as possible.
I t i s c o n v e n i e n t a t t h i s j u n c t u r e t o focus a n o b j e c t o n a slide w i t h t h e low
p o w e r o b j e c t i v e e v e n t h o u g h t h e light m a y n o t b e s a t i s f a c t o r y . When bringing
an object into focus never rack the tube downwards with the eye looking through
the eye-piece; always rack down carefully as close to the object as possible with
the eye on a level with the stage and then rack upwards until the object is in focus.
M a n y e x p e n s i v e lenses a n d i r r e p l a c e a b l e o b j e c t s h a v e b e e n r u i n e d b y failure
t o o b e y t h i s s i m p l e rule.
W i t h t h e o b j e c t i n focus t h e c o n d e n s e r i s t h e n b r o u g h t i n t o focus also.
T h i s i s d o n e b y m o v i n g t h e c o n d e n s e r u p w a r d s t o w a r d s t h e slide a n d c o n -
c u r r e n t l y m o v i n g t h e m i r r o r s l i g h t l y from t i m e t o t i m e u n t i l t h e edge o f t h e
l a m p or t h e filament of t h e b u l b or, if d a y l i g h t is b e i n g used, a p o r t i o n of t h e
w i n d o w f r a m e o r a m a r k o n t h e w i n d o w glass, c o m e s i n t o view. T h i s i m a g e
is t h e n m a d e to disappear by m o v i n g t h e condenser d o w n w a r d s slightly,
a n d t h e illumination restored to its previous uniformity by m a n i p u l a t i o n
of the mirror. The condenser is then transmitting t h e m a x i m u m a m o u n t of
light, w h i c h i n g e n e r a l will b e t o o m u c h for u s e w i t h t h e low p o w e r s a n d
s h o u l d be r e d u c e d by use of t h e d i a p h r a g m , or a screen of g r o u n d or c o l o u r e d
glass i n s e r t e d b e t w e e n t h e s o u r c e o f light a n d t h e m i r r o r .
T h e coarse a d j u s t m e n t i s o p e r a t e d b y t h e m i l l e d h e a d s I a n d i s all t h a t
i s n e c e s s a r y for t h e lower p o w e r s . F o r t h e h i g h e r p o w e r s t h e fine a d j u s t m e n t
/ i s n e c e s s a r y t o b r i n g t h e o b j e c t i n t o s h a r p focus. T h e low p o w e r o b j e c t i v e
s h o u l d a l w a y s be e n g a g e d first a n d s h o u l d it be d e s i r e d to v i e w a s e c t i o n of
t h e field i n g r e a t e r d e t a i l , t h e s e c t i o n i s m o v e d i n t o t h e c e n t r e o f t h e field,
a n o b j e c t i v e o f h i g h e r p o w e r t u r n e d i n t o p o s i t i o n , a n d t h e focus carefully
a d j u s t e d . T h e l o w p o w e r i s t h e r e c o n n a i s s a n c e lens a n d t h e e x a m i n a t i o n o f
a n y o b j e c t s h o u l d c o m m e n c e w i t h t h i s before u s i n g t h e h i g h e r p o w e r .
O b j e c t s m o u n t e d on t h e u s u a l 3 X 1 i n c h g l a s s slides m a y b e s t be o b s e r v -
ed by s u b m e r g i n g t h e m in a t h i n film of a colourless l i q u i d a n d c a r e f u l l y p l a c -
ing a coverslip over t h e whole. F o r pan-stage observations w i t h v e r y low

p o w e r s , e.g., i n c h focal l e n g t h l e n s m a g n i f y i n g four t i m e s , a c o v e r s l i p is n o t
n e c e s s a r y , b u t c r y s t a l s a r e seen m u c h m o r e c l e a r l y i f m o u n t e d i n a c o u p l e o f
d r o p s o f a s a t u r a t e d s o l u t i o n o f refined s u g a r . M a s s e c u i t e s m a y b e t h i n n e d
d o w n for e x a m i n a t i o n b y m i x i n g w i t h a d r o p o f t h e s a t u r a t e d s o l u t i o n . B l a c k
circular air bubbles m a y interfere with t h e observation of some preparations,
b u t a d r o p o f a l c o h o l e i t h e r n e a t o r s u g a r - s a t u r a t e d will u s u a l l y c a u s e t h e m
to disappear.
Direct Measurement of Objects: It is f r e q u e n t l y d e s i r e d to m e a s u r e
accurately t h e dimensions of an object u n d e r t h e microscope. It is manifestly
i m p o s s i b l e t o p l a c e a fine r u l e r i n t h e s a m e field a n d m a k e d i r e c t r e a d i n g s a s
o n e w o u l d d o w e r e t h e o b j e c t o f a size e a s i l y m e a s u r a b l e b y c o m p a r a t i v e l y
gross i n s t r u m e n t s s u c h a s calipers a n d rules. R e c o u r s e h a s t h e n t o b e m a d e
to an eye-piece m i c r o m e t e r . T h i s is a glass disc on o n e surface of w h i c h a r e
a c c u r a t e l y e t c h e d lines o r s q u a r e s o f u n i f o r m s p a c i n g . T h e t o p o f t h e eye-piece
is unscrewed a n d t h e micrometer dropped in to come to rest on a ledge within
t h e eye-piece. T h e t o p i s t h e n r e p l a c e d a n d t h e e y e - p i e c e l o o k e d i n t o while
held v e r t i c a l l y o v e r a s o u r c e o f l i g h t . T h e m i c r o m e t e r r u l i n g s s h o u l d n o w b e
i n s h a r p focus: i f t h e y a r e n o t , t h e m i c r o m e t e r m a y b e f o u n d t o h a v e l a n d e d
upside down on t h e ledge or it m a y be necessary to screw t h e t o p out slightly
t o give a s h a r p focus. I t will b e f o u n d t h a t w h e n p r o p e r l y p o s i t i o n e d a n d i n
s h a r p focus t h e m i c r o m e t e r r u l i n g s will lie i n t h e s a m e p l a n e a s t h e i m a g e
of t h e o b j e c t a n d t h e size of t h e o b j e c t in t e r m s of divisions c a n be r e a d
d i r e c t l y . T h e a p p a r e n t size of t h e s e divisions in m i l l i m e t r e s or f r a c t i o n s of an
i n c h is, h o w e v e r , n o t k n o w n a n d m u s t b e a s c e r t a i n e d b y reference t o a s t a g e
m i c r o m e t e r . T h i s c o n s i s t s o f a s t o u t 3 x 1 i n c h glass slide w i t h a p o r t i o n i n t h e
c e n t r e r u l e d a c c u r a t e l y w i t h lines a k n o w n d i s t a n c e a p a r t . A c o m m o n t y p e
h a s lines s e v e r a l m i l l i m e t r e s l o n g 0.1 m m a p a r t w i t h o n e 0.1 m m s e c t i o n
s u b d i v i d e d i n t o 0.01 m m . B y focusing o n t h i s m i c r o m e t e r o n t h e s t a g e t h e
eye-piece r u l i n g s c a n b e s u p e r i m p o s e d o n t h e scale r e a d i n g s a n d t h e v a l u e o f
t h e eye-piece m i c r o m e t e r divisions easily m e a s u r e d . T h i s m e a s u r e m e n t o f t h e
a p p a r e n t a c t u a l size o f t h e eye-piece m i c r o m e t e r division i s t e r m e d " c a l i b r a -
t i o n " of t h e eye-piece m i c r o m e t e r a n d v a r i e s w i t h t h e m a g n i f i c a t i o n , so a
s e p a r a t e d e t e r m i n a t i o n m u s t b e m a d e for e a c h c o m b i n a t i o n o f eye-piece a n d
objective at a particular t u b e length. Eye-piece micrometers are not expensive
a n d s h o u l d be p a r t of t h e e q u i p m e n t of e v e r y m i c r o s c o p e : as a m a t t e r of fact
t h e y c a n b e k e p t p e r m a n e n t l y i n t h e eye-piece a n d s o r u n n o risk o f b e i n g
m i s l a i d . T h e s t a g e m i c r o m e t e r s a r e m o r e e x p e n s i v e b u t officers o f t h e B u r e a u
will b e p l e a s e d t o c a l i b r a t e a n y m i c r o s c o p e s a n d eye-piece m i c r o m e t e r s u p o n
request.
T h e c a l i b r a t i o n d o e s n o t p r o v i d e a m e a s u r e of t h e m a g n i f i c a t i o n , i.e,.
t h e size o f t h e o b j e c t a s seen b y t h e e y e t h r o u g h t h e m i c r o s c o p e c o m p a r e d
w i t h i t s a c t u a l size. T h i s c a n often b e o b t a i n e d b y a k n o w l e d g e o f t h e
m a g n i f i c a t i o n p r o v i d e d b y t h e o b j e c t i v e a n d t h e eye-piece, b u t s o m e t i m e s
t h i s i s n o t a v a i l a b l e . A r o u g h a p p r o x i m a t i o n c a n t h e n b e m a d e w i t h low-
p o w e r e d o b j e c t i v e s b y t h e following m e t h o d : —
P l a c e an o b j e c t of k n o w n s u i t a b l e size, e.g., a d i v i s i o n on an e n g i n e e r i n g
rule, o n t h e s t a g e a n d b r i n g i t i n t o s h a r p focus. T h e n h o l d a s h e e t o f w h i t e
c a r d or stiff p a p e r at a d i s t a n c e of 10 in f r o m t h e e y e a n d close to t h e l i n e of
t h e microscope body. By looking i n t o t h e microscope with one eye a n d
focusing t h e o t h e r o n t h e w h i t e p a p e r a t t h e s a m e t i m e , a n i m a g e o f t h e
o b j e c t will b e seen t o b e s u p e r - i m p o s e d o n t h e p a p e r . T h e e n d s c a n b e m a r k e d
with a pencil as one watches a n d then t h e distance m e a s u r e d between t h e
t w o p e n c i l lines. T h e r a t i o o f t h i s d i s t a n c e t o t h e a c t u a l size o f t h e o b j e c t
gives the magnification of the particular optical set-up of the microscope.

The method sounds rather complicated but after a little practice it is found
possible to reproduce the measurements quite readily.
The Projection Microscope
A projection microscope is of value when a large image is to be thrown
on a screen for demonstration purposes or on to a table for the purpose of
making a drawing.
Outfits are available for converting a standard microscope into a projec-
tor, the main requirements being a stand to provide rigid mounting and an
efficient illumination train of high intensity. Complete projection microscopes
may also be obtained. Various models are available ranging from expensive
high power units to much simpler ones when only low to medium magnifica-
tion is required. A projection microscope of medium cost is shown in Fig. 29.
This microscope is of a type suitable for use in the examination of proof
samples withdrawn from vacuum pans etc. The slide with the sample to be
examined is placed on the stage and brought into focus on the viewing screen
Fig. 29—A projection microscope of medium cost (Maruzen).

of nearly 7 in diameter. The standard lens supplied (x 10) is of sufficient

power for pan stage operation, however, other objectives up to x 40 are
also available. A squared grid may be placed over the screen and calibrated
for size depending on the objective used.
Photomicrography
Photomicrography is the process of recording on film the image produced
by the microscope. The fact that a real image of the microscopical object is
projected, without the aid of any equipment other than a brilliant source of
illumination, by the eye-piece onto a screen located above it, makes photo-
graphic reproduction possible.
If a light-sensitive plate or film is substituted for the screen and all
extraneous light excluded a negative can be secured.
The simplest form of equipment consists of a light-tight box with a ground
glass screen fitted into the top, which can be exchanged for a film pack or
plate holder. The box is arranged over the microscope so that the image can
be focused onto the screen, which is then exchanged for the film. The
exposure can be made by turning the microscope light on for the required
period.
Another simple method involves a camera with the lens removed,
connected in a light-tight manner to the microscope tube. A single-lens reflex
camera or one with a ground glass focusing screen is required so that accurate
focusing on the focal plane of the camera can be done, for the point of best
focus for the camera will not be identical with the best visual focus through
the microscope. If a camera with a focal plane shutter is used this can be used
for making the exposure, otherwise the microscope light can be used.
Complete photomicrographic equipment, ranging from extremely simple
to very elaborate, is available from microscope manufacturers. If serious
work is contemplated these commercial products are to be preferred, however
very good results can be obtained with improvised outfits.
The Care of Optical Instruments

All too frequently optical instruments are treated as though they were
a piece of laboratory furniture and not as delicate instruments built by
the manufacturers to a degree of high precision. If treated and used carefully
the life of a good instrument is practically unlimited.
Optical instruments should be set up in situations which are not exposed
to dampness or corrosive fumes, or subjected to jarring or vibration. In
tropical conditions dampness favours mould growth which etches the polished
surfaces of prisms. It has been found in practice that mould growths on calcite
prisms will render a saccharimeter useless within a short period of time from
when they first become visible. The instrument should be forwarded for
attention to an instrument maker who is thoroughly conversant with it.
If the instrument is subjected to vibration or jarring the optical system
may be thrown out of adjustment. Where it is not practicable to build the
laboratory sufficiently far from the mill to avoid all vibration, the instrument
should be mounted on a suitable anti-vibration table.
The instrument should be examined regularly and kept scrupulously
clean. This applies, in the case of saccharimeters, to splash glasses and the
trough. If juice is allowed to accumulate in the trough thus penetrating to
the threads of the screw caps holding the splash glasses, great difficulty will
be experienced when an attempt is made to remove them. In some sacchari-

meters the splash glass holder is held in position by means of a tension spring
and is constructed for ready removal by the fingers. It should be maintained
in such a condition.
The prisms of a refractometer should always be thoroughly cleaned and
dried after use and a piece of lens tissue placed between the prisms before
closing them. This assists in keeping the polished face of the measuring prism
in good condition.
A microscope, even one in the cheaper range, is an instrument of precision
and as such should be treated with every care, if it is to give satisfactory
results over a long period. The operation and manipulation should be
entrusted only to people who have shown themselves capable of handling it
with the respect it deserves. Special precautions should be taken to ensure
that dust is kept out of the lenses at all times and they should never be
exposed to direct sunlight, for this will quickly result in permanent fogging.
When not in use, objectives should be placed carefully in the small plastic or
metal cans provided by the manufacturers. There should always be an eye-
piece in position otherwise damaging grit is likely to enter the draw tube,
body, nose-piece and objectives. Eye-pieces should never be left dismantled,
for dust inside the eye-piece will spoil the image. The condenser remains
attached to the microscope permanently and should be wiped over from time
to time with a dust-free silk or cotton cloth or cigarette paper, care being
taken that the top lens surface is not scratched. The diaphragm and mirrors
should be quite dry and dust-free. While a very small amount of lubrication
is required for the adjustment threads and racks, oil or grease elsewhere is
to be avoided at all costs. Not only is it unnecessary, but it damages lenses
and specimens and in removing it permanent harm can easily occur to the
instrument.
Care in the actual use of the microscope is also of importance in main-
taining the instrument in a good working condition. It should never be
subjected to sudden jolts or bumps and never allowed to get sticky or dirty.
The under side of the slides should always be dry and clean before being
placed on the stage and no liquid should be allowed to run off the. mounted
slide. The technique for avoiding the fouling of the front lens of the objective
when bringing the object into focus has been explained and it should be
followed at all times.
When not in continuous use, all optical instruments should be kept under
a cover. At the end of the season they should be cleaned and stored away in
a dry atmosphere.
REFERENCE
Wilson, Robert A. M. (1965), Polarization Temperature Corrections. Int. Sug. J. 67,
234-6, 265-8.
CHAPTER III
THE BALANCE
A sugar laboratory should be provided with three balances of the follow-
ing general types—
(1) An analytical balance for accurate work;
(2) A sampling balance for work of moderate accuracy;
(3) A balance of higher capacity for coarse weighing of large masses.
The Analytical Balance
This balance is required for all analytical purposes, for determination
of specific rotations, for calibration of small items of volumetric glassware,
Fig. 30—-A modern single pan constant load balance (Sartorius).

52 T H E BALANCE
for the weighing of pycnometers and all other operations where precision
weighing is required. It should have a capacity of at least 160 grammes and
a sensitivity reciprocal of 0.1 rnilligramme per scale division or less. The great
majority of balances of this class utilise the two knife edge, constant load
principle, employing built in weights, critical damping of the swing of the
beam and an optical projection system for reading the beam deflection. A
modern balance of this type is shown in Fig. 30 while the diagrammatic
representation in Fig. 31 shows the components.
1 Compensating stirrup
2 Front knife edge
3 Pan brake
4 Weight carriage
5 Built-in weights
6 Pan
7 Weight control mechanism
8 Recording disc
9 Projecting scale
10 Micrometer mirror
11 Weight shaft
12 Arrestment shaft
14 Bulb
15 Arrestment
16 Objective regulator
17 Scale and objective
19 Damping
19 Sensitivity adjustment
20 Zero adjustment
21 Beam
22 Center bearing plate
23 Center knife edge
Fig. 31—Diagrammatic representation of a single pan constant load balance (Sartorius).
The sensitivity of a balance is defined as the deflection produced by the

addition of unit mass to the pan and is usually expressed in divisions per
milligramme. The more useful term sensitivity reciprocal, S.R., is the mass
which must be added to the pan to change the reading by one scale division.
The value of the sensitivity depends on the position of the centre of gravity
of the moving system in relation to the axis of rotation of the beam. For
stability, the centre of gravity of the beam must lie below the axis but the
smaller the separation the more sensitive the balance becomes. In a three
knife edge equal arm balance the sensitivity varies with the load being
weighed unless the three knife edges are accurately co-planar. The two knife
edge balances, in which weighing is made by substitution, operate at constant
load and the sensitivity remains constant irrespective of the value of the
load being weighed.
A small weight moving on a vertical screw fixed to the beam is provided
to vary the vertical distance of the centre of gravity from the main knife and
hence the sensitivity of the balance. A constant load balance having a
sensitivity reciprocal of 0.1 mg per division should be adjusted so that the
error in reading at the full deflection of the beam is less than 0.2 mg. A three
knife edge balance should be adjusted, with half full load in each pan, to the
same order of accuracy.
T H E BALANCE 53
In all balances provision is made for poising the beam and adjusting
the zero reading by means of poising nuts carried on horizontal screwed rods
parallel with the beam. In all balances with optical projection reading, fine
adjustment of the zero is made by moving the reading index of the balance.
All precision balances are equipped with an arresting mechanism which
supports the pans, stirrups and beam of the balance, so protecting the knife
edges and bearings from damage when the pan or pans are loaded and un-
loaded. When loading has been completed and the case closed the balance is
released and the pan, stirrup and beam are released, preferably in that order.
Weights: The majority of modern balances have the weights built in to
the balance, the weights being applied and removed by the manipulation of
controls external to the case. Balances of the older type require to be used
in conjunction with a set of standard weights.
Irrespective of which type of weights is used they must conform with
certain basic requirements. To ensure both long and short term stability the
weight must be constructed in one piece from a hard inoxidisable material,
the surface must be smooth and free from sharp edges and the material must
be non-magnetic. These requirements are met by well made weights of non-
magnetic stainless steel containing approximately 25% chromium, 20%
nickel, which has a density between 7.8 and 8.0 g c m - 3 a t 20°C. Weights of
this material are far superior to those of brass, either plain or with a protective
plating of gold, chromium or any other material.
It is customary for precision weights to be adjusted to their nominal
value on the assumption that they are all of uniform density—8.0 g cm - 3 .
That is, the weights are adjusted to balance a standard weight of true
nominal mass and of density 8.0 g c m - 3 when in air of density 0.0012 g cm - 3 .
This practice is followed by N.S.L. Australia, and by most national standard-
izing laboratories.
It follows from this that in weighing of the highest precision, where air
buoyancy corrections must be applied, they should be calculated on the
basis that the density of the weights is 8.0g cm~3 and using the actual value
of the density of the air in the balance case.
Weights must never under any circumstances be touched with the
fingers. They should be manipulated only with plastic-tipped or chamois
covered forceps.
Setting up the Balance: In the case of a new balance it is most desirable
if possible to have the balance set up and adjusted by the maker's re-
presentative.
The balance must be set up on a firm bench, free from vibration and in
a room in which the temperature is reasonably constant or varies only slowly
during the day. A good criterion for an acceptable level of vibration is the
appearance of the image of the optical scale. This should, of course, be focus-
sed until the lines appear quite sharp, and the balance then released. The
appearance of the lines is closely observed and any slight blurring is a good
indication of the presence of excessive vibration. If this occurs, steps should
be taken to isolate the balance from the bench by means of anti-vibration
mountings.
The balance should be placed on the bench and the inside of the case
thoroughly cleaned. The case should be levelled using the circular level bubble
or plumb bob provided and the rest point adjusted to zero. The sensitivity
should be adjusted to its nominal value by placing on the pans a weight
which should give full scale deflection of the reading index.
54 THE BALANCE
After these adjustments have been made the balance case should be
closed and (he balance left to stand for at least one hour to settle down.
After this period the zero reading and sensitivity should be re-checked and
any further minor adjustments made if required.
General Precautions in Weighing
Objects should never be weighed until they have attained the temper-
ature of the balance case. Hot bodies should never be placed on the balance
case but should be allowed to cool, preferably in a desiccator, until they are
approximately at ambient temperature. The time taken by a body to cool
to room temperature depends on its initial temperature, its size, and the
material from which it is made.
Hygroscopic materials can only be weighed when contained in an air-
tight vessel. Under no circumstances should any chemical come into contact
with the scale pan. All material to be weighed should be placed in a clean
dry tared container of suitable material such as platinum, glass, aluminium
etc. In the case of non-hygroscopic crystals a piece of clean dry paper may be
used.
Method of Weighing: The operator must first make sure that the pan
and the interior of the weighing compartment are clean.
The operation of weighing with a direct reading balance with weight
loading facility is very simple. With the weight selector dials set to zero,
release the balance, and when the image comes to rest adjust the balance to
read zero. Arrest the balance. Place the object to be weighed on the balance
pan, and close the balance case. Select a weight which is judged to be close
in value to the mass of the object being weighed. Release the balance and
note whether the object is heavier or lighter than the weight selected. Arrest
the balance and select the appropriate greater or smaller weight and read
again. Repeat the process until a reading on the scale is obtained. Allow the
beam to come completely to rest and read the weight of the body.
Some balances of this type have a partially released position of the beam
in which it is possible to change the dial settings and watch the change in
scale reading without having to arrest the beam between settings.
In making weighings with an equal arm three knife edge balance the
following procedure is observed. The pans are wiped with a small camel-hair
brush, the case is closed, and the beam is carefully released. The pointer will
now swing slowiy over the scale, and when the amplitude has fallen to about
five scale divisions, the readings of the extremities of the swing are taken for
five successive swings. Care should be taken to avoid parallax in the readings.
It is best to number the scale continuously from left to right rather than to
call the centre division O and those to the right positive and to the left
negative. Suppose the central point to be numbered 10, and that the following
numbers represent observations: —
THE BALANCE
The beam is then arrested, taking care that this is done when the pointer
is at the centre of the scale, so as to avoid damaging the knife-edges.
The object to be weighed should be removed from a desiccator in which
it has been placed in order that it may be free from moisture, and at the same
temperature as the balance. The object is placed on the left-hand pan. A large
weight should then be put on the right-hand pan, and the beam released just
sufficiently to determine the direction in which the beam will move. The beam
is again arrested and a larger or smaller weight applied as required. Each
weight is tried in turn until equilibrium has been obtained as closely as
possible. The balance case is then closed, and the further adjustments made
by means of the rider.
It is not necessary to adjust the weight so that the resting point is
identical with that initially found, provided the precise sensitivity of the
balance is known. Suppose the following turning-points were determined
with a mass of 21.682 g on the right hand pan:—
Right
Mean 9.53 12.05
The weight is, therefore, insufficient and should be increased by an amount

which would change the resting point by 10.79-10.03 or 0.76 division. If, from
a previous determination, it has been found that the sensitivity at 20 g load
is 4.0 scale divisions per mg the correction to be added is:—-
It will be observed that the average of the last left-hand and the last
right-hand swing of the balance gives a result which would be indistinguish-
able on the scale from the true resting point. A skilled operator makes use
of this fact to determine when the correct mass is on the scale pan. By a
careful release of the mechanism he may confine the first deflection to one
or two divisions and observe if the next two are at equal distances from the
centre of the scale.
Testing a Precision Balance
The essential attributes of any precision balance are:—
(1) The reading of the balance must be consistent for any given condition
of loading.
(2) The balance must give weighings which are closely reproducible.
In the case of balances fitted with optical projection reading and inbuilt
weights the following are additional requirements.
(3) The sensitivity must be close to its nominal value and must be
constant over the full range of the scale.
56 T H E BALANCE
(4) T h e e r r o r i n a n y w e i g h t o r c o m b i n a t i o n o f w e i g h t s s h o u l d n o t e x c e e d
t h e c o r r e s p o n d i n g Class A t o l e r a n c e specified b y t h e N a t i o n a l
Standard Laboratory.
(5) I n t h e case o f t w o p a n t h r e e knife e d g e b a l a n c e s t h e effective l e n g t h s
o f t h e b a l a n c e a r m s s h o u l d b e e q u a l t o w i t h i n 1 0 p a r t s i n a million.
Methods of Test: (1) T h e g e n e r a l c o n d i t i o n of a b a l a n c e c a n n o t be c h e c k e d
q u a n t i t a t i v e l y b u t a n i n s p e c t i o n s h o u l d s e r v e t o c h e c k t h e following p o i n t s .
T h e b a l a n c e s h o u l d b e c l e a n a n d all p a r t s s h o u l d b e free f r o m c o r r o s i o n .
The arrestment should operate smoothly and should not cause a n y un-
wanted motion of the pointer or pans.
M a n i p u l a t i o n o f t h e b u i l t i n w e i g h t s s h o u l d n o t c a u s e a n y significant
j o l t i n g or s w i n g of t h e p a n .
(2) R e p r o d u c i b i l i t y o f r e a d i n g s . T h i s i s c h e c k e d b y t a k i n g t w e n t y c o n -
s e c u t i v e r e s t p o i n t r e a d i n g s , t h e b a l a n c e case b e i n g k e p t closed a n d t h e
balance arrested between each reading.
T w o c r i t e r i a of s t a b i l i t y a r e u s e d :
(a) T h e m a x i m u m difference b e t w e e n a n y t w o c o n s e c u t i v e r e s t p o i n t s a n d
(b) T h e s t a n d a r d d e v i a t i o n of t h e r e s t p o i n t s .
(a) is a m e a s u r e of e r r a t i c v a r i a t i o n in t h e r e s t p o i n t a n d
(b) gives a m e a s u r e of drift or slow c h a n g e in t h e r e s t p o i n t .
If S is t h e a c c u r a c y of e s t i m a t i o n of t h e r e a d i n g e i t h e r by v e r n i e r or by
v i s u a l e s t i m a t i o n , b o t h c r i t e r i a (a) a n d (b) s h o u l d be less t h a n 2 8 for a g o o d
balance.
(3) T h e s e n s i t i v i t y of t h e b a l a n c e is m e a s u r e d by s e t t i n g t h e o p t i c a l scale
to zero and t h e n adding to the p a n a weight equivalent to the m a x i m u m
deflection of t h e scale. T h e d e p a r t u r e of t h e full scale deflection f r o m i t s
n o m i n a l v a l u e s h o u l d n o t e x c e e d 2 S in t h e case of a c o n s t a n t l o a d b a l a n c e
a n d 10 8 in t h e case of t h r e e knife edge balances with optical projection.
(4) T h e l i n e a r i t y of r e s p o n s e of t h e b a l a n c e is t e s t e d by u s i n g successive
r a n g e of t h e scale.
(5) T h e t e s t i n g of t h e a c c u r a c y of t h e i n d i v i d u a l w e i g h t s is a m o s t in-
v o l v e d process b u t a n i n d i c a t i o n o f t h e p r e s e n c e o f a n y gross e r r o r s c a n b e
obtained by checking the sum of various groups of weights against approp-
r i a t e s t a n d a r d s . F o r e x a m p l e if a b a l a n c e h a s an o p t i c a l r a n g e of 0.100
g r a m m e and groups of weights
0, 0 . 1 - 0 . 9 g
0, 1 - 9 g
0, 1 0 - 9 0 g
check 0.9 + scale a g a i n s t 1 g
9.9 + scale a g a i n s t 10 g
99.9 + scale a g a i n s t 100 g
A m e t h o d of c a l i b r a t i o n of i n b u i l t w e i g h t s , u s i n g all a v a i l a b l e d a t a , h a s
b e e n d e s c r i b e d ( H u m p h r i e s , 1961), w h i c h y i e l d s self c o n s i s t e n t r e s u l t s of an
accuracy comparable with the discrimination of the balance.
T H E BALANCE 57
Balance for Coarse Weighing

For general approximate work at heavier loads a speedier balance of
more robust construction is used. A balance having a maximum load of 3 or 4
kilogrammes and a discrimination of 0.1 gramme is suitable for this purpose.
Single pan balances with optical scale and taring facility are available and
they are very suitable for this purpose.
Although these balances are robust they should nevertheless be kept
clean and their accuracy periodically checked with known weights.
REFERENCE
Humphries, J. W. (1961). The calibration of the weights built into a balance.
Aust. Jour, of Ap. Sci. 2, 3, 360
CHAPTER IV
DENSIMETRIC METHODS OF ANALYSIS

The quantity of mass in unit volume of a substance is known as the
density of that substance, and is expressed in such units as grammes per milli-
litre, or pounds per cubic foot. Mathematically where d is the dens-
ity, m the mass and v the volume of the substance. The volume of a given
mass may, and almost invariably does, vary with temperature and pressure.
For liquids and solids the change of volume with temperature is quite
significant, but the effect of variation in pressure is usually negligible, so t h a t
it suffices to specify the temperature to which any statement of density is
related.
At any given place the mass of any body is proportional to its weight
in vacuo. The ratio of the masses (weights in vacuo) of equal volumes of a
substance and some standard material is known as the relative density of the
substance. Customarily, when the standard material is water, the ratio is
known as specific gravity, so that specific gravity (s.g.) may be defined as a
number which indicates how much heavier or lighter a material is than
water.
The derivation of specific gravity involves two densities each of which
must be qualified by a temperature and so the ratio
Since one ml of pure water at 4 °C (the temperature at which the density

of water is a maximum) weighs one gramme in vacuo* and thus has a density
of 1 g per ml, the temperature of 4 °C is frequently adopted as a basis for
expression of specific gravities. It follows that the density of a substance at
ts in g per ml and its specific gravity are numerically the same.
For convenience it is customary to adopt a standard temperature for
which the density of the test material is specified. In the Queensland sugar
industry the accepted standard temperature is 20 °C and specific gravities
are usually quoted as s.g
By reference to tables showing the density of water at various tempera-
tures it is possible to derive a factor for the conversion of specific gravities
based on water at 4 °C to values based on water at some other selected
temperature, e.g., s.g. 20 °C.
The relationship between two masses is correctly expressed by the ratio
of their weights in vacuo. When a weighing operation is conducted under
normal laboratory conditions, the buoyant effect of the atmosphere is exerted
on both the sample and the weights, and as these usually differ in volume,
the resultant force creates a difference between the weight of the sample in
air and its weight in vacuo. A weight "in air, with brass weights" is con-
*This follows from the old definition of the millilitre, i.e., the volume occupied by
1 g of water at the temperature of its maximum density.
DENSIMETRIC METHODS OF ANALYSIS
vertible to the weight in vacuo if the density of the test sample is known.
Hence, densities and specific gravities may be expressed in terms of weight
in air with brass weights, and as most weighings are conducted under these
conditions, tables of density on this basis have great practical value. Great
care should be taken to avoid confusion between density figures based on
weight in vacuo and those based on weight in air with brass weights.
The determination of specific gravity is one of considerable importance
in sugar analyses. This is due to the interesting fact that solutions of different
sugars of equal concentrations have almost identical specific gravities. The
following values for 10 per cent solutions of nine distinct sugars illustrate
this fact:—
Further, the mean value for all sugars approximates closely to that
for sucrose. It is possible, therefore, to determine very closely the percentage
of dissolved substance in any solution of sugar or mixture of sugars simply
by determining its specific gravity.
While the application of specific gravity tables established for sucrose
may be applied with reasonable accuracy for the estimation of dissolved
substance in a solution of mixed sugars, this is not the case where other
dissolved substances are present. The errors resulting from this cause are
at times very great as, for example, with final molasses. The influence of
the salts present in such a solution may be gauged from the following data
showing the concentration of solutions of sodium-potassium tartrate and
potassium carbonate in comparison with sucrose solutions of equal specific
gravity.
When the specific gravity of such solutions is determined after dilution

with water, the error is still further intensified, owing to the difference in
contraction between sugar and dissolved impurities in aqueous solution,
as is seen from the above table. Concentrations determined by this method
for other than pure sugar solutions must, therefore, be regarded as rough
estimates only.
60 DENSIMETRIC METHODS OF ANALYSIS
The Pycnometer
A highly accurate instrument for the determination of specific gravity
is the pycnometer or specific gravity bottle (Fig. 32).
Fig. 32—Illustrating the types of pycnometer in use in Queensland.
It is simply a glass vessel which is designed to contain an accurately

reproducible volume of liquid at any particular temperature. The best
pycnometers are vacuum jacketed for thermal insulation, and are fitted
with a thermometer. By weighing the bottle filled first with water and then
the given solution at constant tempeiature the weights of equal volumes of
the two fluids may be determined, and hence the specific gravity of the test
solution.
The pycnometer is mainly used in the sugar mill laboratory for the
determination of the Brix of dilute sugar solutions extracted in the analysis
of cane or bagasse.
To Determine the Volume of the Pycnometer at a Standard
Temperature.—This determination has little practical use, but serves to
describe the technique and develop the theory. The bottle is thoroughly
cleansed, using in turn glass cleaning solution, water and alcohol. It is then
dried in a stream of dry air and weighed. It is next filled with distilled water
which has recently been boiled to expel dissolved air and cooled to 2 to 3 °C
above ambient temperature. The stopper is inserted*, care being taken to
prevent the introduction of air bubbles, and the excess water is carefully
removed by means of a filter paper (from the stopper and also from the
capillary in the side-arm type).
*The temperature of the water must be determined at the instant the stopper is
fully inserted. Where a thermometer is incorporated in the stopper, the stopper is
lightly set in place and the thermometer allowed to come to reading; where a stopper
only is provided, a thermometer is inserted first, read and withdrawn. The stopper
is inserted immediately.
DENSIMETRIC METHODS OF ANALYSIS 61
The pycnometer is then placed in a water bath at a temperature lower

than that of the water employed to fill the bottle (ambient or preferably a
lower temperature). The liquid meniscus is thus drawn down the ground
glass joint or the capillary depending on the type of pycnometer used. The
pycnometer is then wiped perfectly dry.
In drying the surface considerable care must be taken and the following
technique is recommended. The outside is first wiped thoroughly with a
piece of clean, damp flannel, then the damp surface is dried with a clean
chamois, after which a final rub is given with a second chamois. During these
manipulations and the subsequent weighing the pycnometer must not come
in contact with the fingers.
Several determinations are made with distilled water, the temperature
being noted to 0 • 1 °C for each weighing. The total weight minus the weight
of the empty vessel is the weight, in air, of the water contained, at the
observed temperature.
This weight in air has to be converted to weight in vacuo by applying
corrections for the buoyancy of the water and the weights.*
This volume VT is fixed for any pycnometer. It will be noted that the
measured weight of water W1 is related to the standard volume VT by a
complex factor which involves the density of water, the correction for
buoyancy and the thermal expansion of glass. The value of this factor for
water in a glass vessel is fixed for any temperature t1 referred to a standard
temperature T. Values for various temperatures are available from tables.
For added convenience, tables have been prepared in which the correction
is made additive or subtractive (see Tables X X I I I and XXIV). Hence, in
practice the measured weight of water contained at t1 (in grammes) is con-
verted, either by a factor or a correction, directly to the standard volume of
the pycnometer at T (in millilitres). This procedure is adopted as the basis
in the testing of standard volumetric glassware.
|The accepted values for y are (B.S.S. 1797: 1952) soda glass + 0.00003, borosili-
cate glass + 0.00001 per 1 °C rise in temperature.
*It being assumed that the weighings have been made in air of average density
0.0012 g/ml using weights of density 8.0 g/ml.
To Determine the Specific Gravity of a Test Solution.

The pycnometer is filled with the solution at a temperature 2 to 3 °C
above ainbient and the weight of the contents determined as before. Let
the weight of the contents be W2 at t2.
The density of the solution at the temperature of the determination t2
may be determined by dividing the true weight of the contents at t 2 by the
volume of the pycnometer at t2, the latter being determined either by direct
measurement using pure water at t 2 or by correction of the volume at the
standard temperature to the volume at t 2 in accordance with the coefficient
of expansion of the glass of which the vessel is made. This procedure has the
disadvantage that the observed weight of the solution must first be converted
to weight in vacuo. If it were convenient to conduct tests on the solution and
on pure water at temperature t2, the buoyancy corrections on the two weights
would be practically equal and could be neglected. Hence,
Without special precautions, it is very difficult to conduct two deter-

minations at the same temperature. Hence, in general, the test with water
will be conducted at t 1 and that with the solution at t2. Then, if the density
of the solution at t2 be designated D,
Determination of Brix.
In using the pycnometer for the determination of the Brix of sugar
solutions a modified procedure is adopted for simplicity. If the true weight
of the contents of a pycnometer at t2 be divided by the standard volume of
the pycnometer at T, the result derived is known as the apparent density
at t2. It is assumed that, as before, the weight of pure water contained at
t1 is W1.
The apparent density at t 2 is the value which would be observed by

taking a glass hydrometer calibrated to read correctly at the standard
temperature T and immersing it in the test solution at t2. A Brix hydrometer
is calibrated to read correctly at a standard temperature T, and, if used at
another temperature t2 will give a reading which differs from the actual Brix.
If the apparent density at t2, referred to above, be converted to Brix by using
the standard tables for conversion at temperature T the value derived will
coincide with the actual reading of the Brix hydrometer at t2.
Thus, in the determination of Brix, the apparent density is first derived.
This apparent density is converted to "observed" Brix, using the standard
table, and the observed Brix is then corrected for temperature according to
the normal method for the Brix hydrometer.
It will be noted that, to derive the apparent density, the observed
weight W 2 must be divided by the term
culated for various values of t1 and a table of factors could be compiled.

However, it is simpler, and sufficiently accurate, to make use of Table X X I I I ,
subtracting 1.05 from the values listed therein and then reducing the correction
as usual in proportion to the approximate volume of the pycnometer. The proce-
dure is most easily followed by reference to the examples.
In the compilation of Table X X I I I it has been assumed that the co-
efficient of expansion of glass is 0.00003. Such a coefficient is not likely to be
associated with any borosilicate glass, and even some glasses nominally of
the soda type display coefficients of expansion significantly different from
the figure stated. The existence of a coefficient different from 0.00003 will be
manifested in systematic variation of the determined pycnometer constant
with the temperature at which it is determined.
*ln the second edition of the Laboratory Manual this characteristic constant of
the pycnometer was referred to incorrectly as the Volume. It might leniently be re-
garded as an "apparent volume" but the word "apparent" is overworked, and the term
pycnometer constant is preferred.
For general scientific work it is possible and would be desirable to

analyse the results of tests over a range of temperatures to determine the
actual coefficient of expansion of the glass, and hence the true constant.
However, in the sugar laboratory the pycnometer is used almost exclusively
for the determination of Brix, in the course of which reference is made to
Table I. This table incorporates an allowance of 0.000025 for the coefficient
of expansion of glass.
Hence in practice, whatever be the material of construction of the
pycnometer, the coefficient of expansion of the material should be taken as
0.000025 for the calculation of the constant. If the coefficient of expansion of
the material is, in fact, 0.000025 the constant will be independent of tempera-
ture. For all other cases the so-called constant will vary with temperature.
For any vessel displaying this characteristic it is necessary, from the results
of tests over a range of temperatures, to draw up a temperature scale of
constants and, in practice, to adopt the value of constant corresponding to
the temperature of a determination. The apparent density thus derived
may be converted to observed Brix with the aid of Table XIV and the Brix
may then be adjusted by reference to Table I.
Examples:
For the purposes of the following examples the pycnometer is constructed
of glass having a coefficient of expansion of 0.00003 per 1 °C rise in temper-
ature.
Determination of Volume of Pycnometer.--
This specific gravity may be converted to or any other reference

temperature for the water, but, without tables applying specifically to the
solution, the reference temperature of 25 °C for the solution may not be
converted to any other temperature. If a value for density at a selected
temperature t is required, a density determination must be conducted at
that temperature. This does not apply to sugar solutions for which temper-
ature correction tables are available.
Hydrometers.
A second method of determining the specific gravity of solutions, and
the one most commonly employed in sugar laboratories, is by means of the
hydrometer. It provides by far the easiest and most direct method of deter-
mination of this factor.
In its usual form this instrument consists of a hollow glass body,
cylindrical in shape, and terminating at its lower extremity in a bulb, which
can be weighted with mercury or lead shot and at its upper extremity in
a slender, hollow stem within which a paper scale is sealed. If this instrument
be allowed to float in a solution, the weight of liquid displaced is equal to
the weight of the hydrometer. If placed in solutions of different specific
gravity the instrument will sink to varying depths; and the scale is so
graduated that the point on the stem which corresponds with the liquid sur-
face indicates the density or percentage of dissolved substance for the given
temperature.
In practice the hydrometer scale is standardized at a few points only,
and the intermediate divisions are determined by interpolation. The density
of a solution is equal to the weight W of the hydrometer divided by the
volume V of the portion submerged.
Then-
The difference between the volume submerged for any two divisions v is—
v =nr2d
where d = distance between divisions
and r = the radius of the stem.
The following table shows the relationship between the stem divisions
of a hydrometer weighing 75 g and with a cross sectional area of stem (nr2)
equal to 0-2 cm2.
It is clear that as the density increases the distance between scale

divisions decreases. To effect this progressive reduction it is customary, in
practice, to employ a dividing engine.
In the graduation of a hydrometer scale for indicating direct percentages
of sugar (Brix) the distance between scale divisions is more uniform, due to
the partial compensating effect of the non-linear relationship between Brix
and density. At 20 °C the change in density from 0 to 10 °Brix is 0-03901 g
per ml, whilst the corresponding change from 50 to 60 °Brix is 0-05089 g
per ml. This effect is illustrated in the following table, where the dimensions
of the hydrometer are the same as before:—
It is, therefore, customaryingraduating hydrometers which

read direct percentages of sugar, to calibrate at, say, three
points, and then divide the intervals between these points into
equal subdivisions. Though not absolutely accurate, the error
introduced is probably less than the errors of observation.
Brix Hydrometer
The construction of the hydrometer which reads direct
percentages of cane sugar is due to Balling. The scale as later
recalculated by Brix constitutes the form at present in general
use. The divisions of the scale are called degrees Brix, and
express weight per cent of sugar; that is, a sucrose solution of
20 °Brix is composed of 20 g of pure sucrose dissolved in 80 g
of pure water. It should be observed that there is no reference
in this definition to volume. A solution of 20 °Brix at 20 °C is
still a 20 °Brix solution at 80 °C.
The confusion which frequently arises in this connection
is due to the fact that the Brix hydrometer responds primarily
to the density of the solution tested, which varies with temper-
ature. As the glass of which the hydrometer is made has a
much lower temperature coefficient of volume than sugar
solutions, it follows that, with increasing temperature, the
hydrometer will sink deeper and yield lower readings. The
Brix scale marked on the hydrometer is related to the
density of the solution at the standard temperature (20 °C).
Hence, at any other temperature, whilst the equilibrium posi-
tion of the hydrometer is closely related to the actual density
of the solution, the reading cannot be interpreted directly as
Brix. A correction must be applied to the observed reading to
compensate for the change in reading which would result from
bringing the temperature of the solution to 20 °C. In the deriva-
tion of temperature correction tables it is assumed that a
hydrometer of a standard type of glass is immersed in a solu-
tion of sucrose in water.
One type of hydrometer which is used in Queensland mills
is illustrated in Fig. 33. The approximate dimensions are:—
Overall length—36 cm
Length of scale—15 cm
Diameter of cylindrical bulb—3 cm
Diameter of upper tube—5 mm
Length of scale division (0.1 °Brix)—1 -5 mm
The following ranges have been specified as the most
convenient for sugar-mill laboratory use:—
0—10°, 10—20°, 15—25°, 20—30°, 30—40°,
40—50°, 50—60°, 60—70°.
Fig. 33—Illustrating
a Brix hydrometer.
CHAPTER V
VOLUMETRIC EQUIPMENT
The Units of Volume
The units of volume should be based, theoretically at least, on units of
length, and, in the metric system, the cubic metre, cubic decimetre and cubic
centimetre are recognized units purely based on length. However, for a major
part of the last century, units of volume based on mass have not only been
recognized but accepted as standard. In the metric system, the familiar ones
are the litre and millilitre.
The originators of the metric system of weights and measures attempted
to make mass units compatible with volume units by defining the kilogramme
as the mass of one cubic decimetre of water at the temperature of its maxi-
mum density (4 °C). With the best accuracy available at the time this mass
unit was determined and reproduced in a mass of metal—the standard
kilogramme.
Subsequent experience with masses based on the standard kilogramme
and volumes based on the standard metre revealed small discrepancies,
indicating that the original correlation was slightly in error. The volume of
one kilogramme of water at 4C was demonstrated to measure 1.000027
cubic decimetres. This volume, based on the kilogramme was designated the
litre, with a sub-unit, the millilitre.
Two slightly different sets of units were then available, and in 1901 the
litre was officially defined and adopted for volumetric work. This was
apparently not regarded as of much significance at the time, for, at least 20
years later, volumetric glassware was still being calibrated in cc. now written
as cm3. However the millilitre triumphed, and, for the past generation,
volume and derived quantities such as density have been expressed in terms
of the litre. In 1950 the conversion factor was amended to 1. 000028.
In 1964 the 12th General Conference of Weights and Measures resolved
to revert to the purely linear basis of volume and redefined the litre to be
exactly one cubic decimetre. This means that the term litre may now re-
present either of two volumes, and for clarity it is necessary to invoke the
officially unrecognized terms "old" litre and "new" litre.
Once again, public response is very slow and even now (1969) many
chemists are hardly aware of the change. Confusion will be avoided by the
use of the term cm 3 rather than ml, and for the most part, the difference
between the cm 3 and the old ml does not matter anyway.
The Laboratory Manual, in all editions to date, has used the old litre
and millilitre as units; that policy has been adhered to in the current edition
because it does not yet appear possible to adopt the new standards through-
out. The normal solution for the International Sugar Scale is 26.000 g in 100
old ml; is it to become 25.999 g in 100 cm3? It may be decided to let the
weight stand unchanged.
This book deals with a variety of subjects, involving a wide range of
precision of results. In the analysis of factory products the difference between
the old ml and the cm 3 matters not one bit; in pycnometry it cannot be
ignored. It must be left to the reader, conscious of the different units, to
VOLUMETRIC EQUIPMENT 69
decide when they are interchangeable, when not. The important item of
record is that the volume units are of the pre-1964 era, the old litre and the
old millilitre, based on the kilogramme.
It should be stressed that the ml is absolute, and does not alter with
change of temperature. At 4 °C the volume occupied by 100 g of pure water
is exactly 100 ml. If the temperature be raised the water will expand and
occupy a greater volume than 100 ml, but the unit itself does not alter.*
As 20 °C is the standard temperature for all sugar laboratory apparatus,
all volumetric glassware must be standardized at this temperature. For
example, the 100 ml flask used in determining the polarization of sugars
will contain, at 20 °C, 100 times the volume occupied by 1 g of water at 4 °C.
Volumetric Glassware
The volumetric glassware used in the sugar laboratory includes flasks,
burettes, pipettes and measuring cylinders.
For general purposes, volumetric equipment of class B standard is
satisfactory and it is recommended that the use of class A glassware be
restricted to those operations which necessitate the highest degree of accuracy
being attained. Various standards authorities—The National Physical
Laboratory England, National Standards Laboratory Australia, The Na-
tional Bureau of Standards USA, The British Standards Institution, the
Standards Association of Australia and others have developed and laid down
specifications for class A and class B volumetric glassware. However the
accuracy of an individual piece of equipment is not guaranteed by any more
than the reputation of the manufacturer.
The first essential in standardization is to have the glassware thoroughly
clean. Traces of grease are particularly to be avoided. The vessel should be
rinsed with water and loose contamination should be removed mechanically
as far as possible in the usual way. The vessel should then be filled with an
aqueous solution of a soapless detergent, shaken vigorously and allowed to
stand for several hours. After pouring off the solution the vessel should be
rinsed with distilled water several times until all traces of the detergent have
been removed. If the vessel is not sufficiently clean after this treatment it
should be filled with chromic acid cleansing solutionf, allowed to stand over-
night if possible and then repeatedly washed with distilled water. The vessel
is rinsed with pure alcohol, then with pure ether and finally dried by a current
of dry air free from dust. The vessel should not be heated.
The capacity of a graduated glass vessel is defined by the volume of
water (or mercury) it contains or delivers at its standard temperature, when
the meniscus i.e. the concave (or convex) liquid surface in the vessel is brought
to the graduation line in a specified manner. In the case of a water meniscus
the top edge of the graduation line is set tangentially to the lowest point of
the meniscus. The provision of a strip of black paper 1 mm below the meniscus
and viewed against a white background will be found to facilitate the setting.
It should be noted that volumetric apparatus is graduated either to
contain or to deliver the particular volume. This is usually indicated on
apparatus made to British or Australian specifications by the inscription " I n "
which has been adopted in place of "C" to indicate that the vessel is graduated
to contain, and " D " is used as the inscription to indicate to deliver. Pipettes
*It may appear superflous to labour this point, but the true significance of this
fact is so frequently overlooked that students fail to make intelligent use of it.
See p. 86 for the preparation of this solution.
70 VOLUMETRIC EQUIPMENT
and burettes are obviously used only to deliver known volumes, but gradu-
ated flasks and more especially cylinders are used either to contain or to
deliver, and when ordering these goods the method of using them should be
considered.
Since the capacity of a glass vessel varies with the change of temper-
ature, any given vessel can be correct at only one temperature. The particular
temperature at which a vessel is intended to contain or deliver its nominal
capacity is the "standard temperature" of the vessel. In Australia 20 °C has
been adopted as the standard temperature for volumetric glassware.
Flasks
The volumetric flask is a vessel designed to contain a known volume of
liquid. The usual form of flask consists of a pear shaped body with a long
narrow neck of approximately cylindrical shape on which a mark is etched
to indicate the required capacity at a given temperature. The bottom should
be flat or slightly dished to allow the flask to stand stably. The neck of the
flask is made as narrow as is consistent with convenience in order that the
error involved in filling to the mark may be as small as possible.
The method usually employed in standardizing a flask is to first weigh the
vessel empty and again when filled to the mark with a liquid of known density.
Corrections must be applied for the buoyancy of air and the temperature of
the liquid. Pure water, either distilled or demineralized, is most generally
used, although mercury gives a higher degree of accuracy, particularly with
vessels of low capacity. The flask should be weighed to a precision better
than 10 per cent of the tolerance prescribed. This can be achieved with a
good quality analytical balance having a capacity suitable to the require-
ments.
A substitution method of weighing is generally used. With modern
single pan balances of constant load it is the only method which can be
employed, whilst with a two pan balance it avoids any errors due to inequality
in the lengths of the arms. When using an ordinary two pan balance the clean
dry flask is placed on one pan together with standard weights slightly in
excess of the amount of water to be weighed. Tare weights are added to the
other pan until the balance is in equilibrium. The flask is then removed from
the pan, filled with water to a distance of a few millimetres above the gradua-
tion line and the surplus water is withdrawn by means of a fine jet so that the
lowest point of the meniscus is well formed and distinct in outline. After
filling, the flask is replaced on the pan and the weights are readjusted so that
the balance is again in equilibrium. The tare weights are left undisturbed.
The difference between the weights used in the first and second weighings is
equal to the weight of water contained in the flask. The temperature is noted
immediately after completion of the last weighing. The weight of water may
then be converted to the volume at 20 °C by adding or subtracting corrections
from Tables X X I I I and XXIV. The main correction compensates for the
expansion of water at temperatures rising above 4 °C and the buoyancy
effect of a standard atmosphere on the flask and weights. The smaller correc-
tion is for departure of the atmospheric conditions from the standard. The
latter correction is negligible for most flasks used in sugar laboratories. The
tables apply to a unit volume of 1000 ml and for other volumes the correc-
tions must be reduced or increased in the ratio of the volumes.
Example for 100 ml flask filled with water at a temperature of 23 °C
and an atmospheric pressure of 755 mm of mercury.
Empty flask + standard weights on pan = 100.000 g
Filled flask + readjusted weights on pan = 0.385 g
Weight of water contained in flask = 99.615 g

Correction for 100 ml at 23 °C (Table XXIII) = +0.340 g
Correction for 755 mm pressure (Table XXIV) = —0.002 g
Capacity of flask at 20 °C = 99.953 ml
When a single pan balance is used normal weighings are made with the
flask empty and when it is filled. To minimize errors due to changes in the
buoyancy of air the second weighing should follow the first without delay.
The tolerances permitted for class B flasks are specified in Table XXV.
Burettes
The burette is employed either to deliver a measured volume of liquid
or to measure a volume of liquid delivered. It consists of a cylindrical tube
graduated usually in tenths of a ml and with a total capacity of 25 or 50 ml.
It is provided at the lower end with a glass tap, or for use with alkaline
solutions, with a rubber tube connected to a glass outlet jet and closed with
a pinch clip. A good burette is of uniform bore, the tap is well fitting and the
graduations are accurate. The fit of the tap may be improved when necessary
by using the finest grade of carborundum paste as a grinding material.
In reading a burette, care should be exercised to avoid errors due to
parallax. Various devices are employed to ensure this; the best burettes have
the graduation marks etched completely around them, so that in reading,
the front of the etching conceals the back portion. Some burettes (Schellbach
type) are manufactured with a longitudinal strip of white glass with a blue
stripe running down the centre of it. The meniscus then presents the appear-
ance illustrated in Fig. 34. This and similar devices are, however, not recom-
mended for precise work, as they introduce the possibility of irregularity in
bore.
The accuracy of a burette is also a function of its rate
of delivery; a satisfactory rate for a 50 ml burette of B
class accuracy is between 75 and 150 seconds. The delivery
time is determined from the zero line to the lowest gradu-
ation line and is taken with the stopcock fully open with the
jet NOT in contact with the side of the receiving vessel.
A burette is first tested for leakage. It is clamped in a
vertical position with the stopcock free from grease, the
barrel and key wetted with water and the burette filled
initially to the zero line with water. The rate of leakage
with the key in the closed position shall not exceed one
half of one scale subdivision in 10 minutes for class B Fig. 34 — Illus-
trating the ap-
burettes during a test of at least 20 minutes. pearance of the
meniscus of the
The tolerances permitted for class B burettes are set Schellbach
down in Table XXV. burette.
In order to record corrections from point to point through the length of
the burette, the errors (positive or negative) may be plotted as ordinates,
against the burette scale graduations as abscissae.
For calibration, the burette is clamped in a vertical position with the jet
downwards and filled through the jet to a few millimetres above the zero
graduation line. It is usual to test at five points of the scale, starting from zero
on each occasion. Delivery is made into a tared weighing vessel, the outflow
being unrestricted until the meniscus is about 1 cm above the graduation line
of the test point. The rate of flow is then reduced to allow the final setting
to be made without any allowance for drainage time.

The drop adhering to the jet of the burette is removed
by bringing the side of the weighing vessel in contact
with the tip of the burette. The weighing vessel is then
weighed, the temperature noted and the volume delivered
at 20 C is calculated from Tables X X I I I and XXIV.
The substitution method of weighing as outlined for
flasks is recommended.
Pipettes
The function of the pipette is to deliver a particular
volume or a range of measured volumes of liquid; it may
be of the bulb type shown in Fig. 35(1) or a graduated
type illustrated in Fig. 35(11). In construction the bulb
pipette consists of a straight suction tube above the
bulb and a straight delivery tube below the bulb. The
top of the suction tube should be ground smooth and
square with the axis of the tube, the outer edge of the
top being slightly bevelled. The graduation mark should
be a fine clean line of uniform thickness completely
encircling the suction tube. The delivery tube should
terminate at its lower end in a delivery jet made with a
gradual taper. The end of the jet should be ground
smooth and square with the axis of the jet. The outer
edge of the jet should be slightly bevelled.
The delivery time of a pipette is important for the
volume of liquid delivered is less than the volume con-
tained, by an amount equal to that adhering to the walls
of the pipette. This volume of adhering liquid will vary
if the delivery time is reduced or increased. However
provided the delivery time is within the specified limits,
the change in volume of the film adhering to the walls
will not introduce any gross errors into the volume
delivered.
The delivery time is the time occupied by the des-
cent of the water meniscus from the graduation line to
the position at which it appears to come to rest in the
jet. The determination of the delivery time is made with
the pipette in a vertical position and the jet in contact
with the side of the receiving vessel.
For the determination of capacity, the pipette is
clamped in a vertical position with the jet downwards
and filled as described for a burette. The water is retained
by pressure of the finger on the tip of the suction tube
and the outside of the jet is wiped free of water with a
cloth. The pressure of the finger is reduced and the water
allowed to run out slowly until the lowest point of the
meniscus coincides with the top of the graduation line.
The drop of water adhering to the jet is removed and
the volume now contained in the pipette is delivered
into a tared vessel with the tip of the jet in contact with
Fig. 35—Illustrat-
the inside of the vessel. A waiting time of approximately
ing common types 3 seconds after movement of the water has ceased, before
of pipette. removing the pipette, is now specified in international
recommendations for one mark pipettes. The natural rate of delivery

should not be increased by force such as blowing and the small quantity of
water remaining in the jet should not be expelled. The vessel is now weighed
and the weight of water may then be converted to the volume at 20 °C by
adding or subtracting corrections from Tables X X I I I and XXIV. The toler-
ances for capacity and delivery time for pipettes are specified in Table XXV.
Graduated Pipettes
Graduated pipettes may be obtained in various types, some examples
being as follows:—
(a) Calibrated downwards from a zero graduation.
(b) Calibrated upwards with the residual volume in the jet as the zero
datum.
Standardization of these graduated pipettes is carried out in a similar
manner to burettes for delivery times and for the volume of water delivered
at 20 °C corresponding to the graduation mark tested. The tip of the jet is
held in contact with the receiving vessel and no drainage time is allowed.
The tolerances allowed for graduated pipettes are shown in Table XXV.
Measuring Cylinders
Cylinders are in common use for rapid approximate estimation of liquid
volumes but they cannot be employed for accurate work. They may be
standardized by the usual method of weighing the water which they contain
or deliver.
Thermometers
Although not a volumetric instrument, the thermometer is so often
closely associated with volumetric determinations that it may well be
considered in this connection.
A good thermometer must be made of sound glass, contain pure mercury
and be filled with inert gas at a suitable pressure. The mercury thread must
be free from breaks. The dividing and figuring of the scale should be clear
and distinct and graduation lines should be of uniform thickness. If the
thermometer is of the solid stem type the graduations are etched on the stem,
or if of the enclosed scale type the scale is permanently marked on suitable
material and rigidly supported within the glass tube carrying the capillary.
The divisions should be at equal spacing.
For routine laboratory work a general purpose thermometer as described
in British Standard 1704 is most suitable. The maximum error of 1°C is
allowed for general purpose thermometers in the range —5 to +105 °C
graduated at each degree. For more accurate work thermometers as described
in British Standard 593 are recommended where the maximum error allowed
for a thermometer in the range —5 to +105 °C graduated at each degree,
is 0.3 °C.
A thermometer is subject to changes in bulb volume caused by the
gradual recovery of the glass from the strain introduced during the treatment
it receives in manufacture. This slow alteration is most noticeable in the first
year or two after the thermometer is made but may proceed for years. Such
changes are also modified by the heat treatments to which the thermometer
is subjected in practice.
In using a thermometer which is calibrated for total immersion it should
be arranged as far as practicable for the entire mercury column to be immersed
i n t h e l i q u i d . W h e r e t h i s i s n o t possible i t b e c o m e s n e c e s s a r y t o a p p l y a
c o r r e c t i o n for t h e e m e r g e n t p o r t i o n o f t h e c o l u m n w h i c h i s n o t a t t h e s a m e
t e m p e r a t u r e a s t h e b u l b . T h e following f o r m u l a i s a p p l i c a b l e for a p p r o x i m a t e
corrections:—•
Tc = T 0 + 0.000156L (To — T m )
where Tc = corrected temperature
To — observed temperature
Tm = temperature of the mid point of the emergent thread
taken by another short thermometer
and L = l e n g t h in degrees of t h e e m e r g e n t c o l u m n .
In g e n e r a l for t e m p e r a t u r e s b e l o w 100 °C, t h e m a g n i t u d e of t h i s c o r r e c -
t i o n will n o t e x c e e d o n e or t w o t e n t h s of a d e g r e e . T h e r m o m e t e r s d e s i g n e d
for a l i m i t e d d e g r e e of i m m e r s i o n a r e a v a i l a b l e — t h e c o r r e c t d e p t h of i m m e r -
sion b e i n g i n d i c a t e d b y a line e n g r a v e d o n t h e s t e m .
CHAPTER VI
THE BUREAU'S METROLOGY LABORATORY

The Bureau maintains a testing service for certain apparatus used in
sugar mill laboratories. According to Regulation 57 of "The Regulation of
Sugar Cane Prices Act 1962-1966", "Only such measuring instruments as
are certified by the Bureau of Sugar Experiment Stations to be within the
required limits of accuracy shall be used in the determination of Brix, pol
and fibre for cane payment purposes". Such instruments include volumetric
glassware, Brix hydrometers, polarimeters or saccharimeters, polarimeter
tubes, refractometers, balances, weights and thermometers.
The metrology laboratory of the Bureau retains standard equipment
certified by the National Standards Laboratory, Sydney, and is registered
with the National Association of Testing Authorities Australia for classes of
tests for the examination of all the abovementioned apparatus.
Examination of apparatus calibrated at 20 °C is conducted in a room
in which the temperature is controlled at 20 + 1 °C and the relative humidity
at 5 5 + 5 per cent.
When the equipment being tested is made to a specified standard the
tests are conducted for compliance with that standard. In the absence of any
nominated standard, the equipment is examined for compliance with toler-
ances which apply to Class B requirements of the relevant British or Aus-
tralian standards for the particular item of apparatus, or for compliance
with the specifications for apparatus used in the analysis of cane for payment
purposes as outlined in Table XXV.
Reports are issued for all apparatus tested and when the tests are
conducted in accordance with the terms of registration with NATA, the
reports are endorsed to this effect. In addition if the apparatus is approved
for use in the analysis of cane for payment purposes the report is endorsed
accordingly.
As outlined in the introduction to Chapter V the unit of volume is based
on the kilogramme, i.e. the old litre and millilitre have been retained through-
out this edition of the manual.
Thermometers
All thermometers should be carefully tested before being put into use.
The service available at the Bureau is for thermometers in the range 0 to
110 °C. They are calibrated for use in the vertical position either partially
immersed or immersed to the reading, by comparison with mercury-in-glass
thermometers which have been standardized by the National Standards
Laboratory Australia. It is customary to test at the icepoint (0 °C) and the
highest graduation mark, as well as at three or four intermediate points.
Brix Hydrometers
The testing of Brix hydrometers covers all ranges within the limits of
0 to 70° Brix.
The method of standardization is by comparison of readings of the test
hydrometer with those of a standard hydrometer of known corrections.
This is carried out in solutions contained in glass cylinders of sufficient size
76 THE BUREAU'S METROLOGY LABORATORY
to allow both hydrometers to float freely side by side. This method is in-
dependent of temperature but a constant temperature is desirable. At the
Bureau the testing is carried out in a constant temperature room at
The reading of each hydrometer is obtained by viewing, from below the liquid
surface, the point where the level of the liquid surface intersects the stem of
the hydrometer. This point is clearly defined when a screen painted with the
top section white and the lower section black is placed behind the cylinder
fig. 36- A dual comparator used by the Bureau for checking the length of sacchari
meter tubes.
THE BUREAU'S METROLOGY LABORATORY 77
with the junction of the black and white sections slightly below the surface
of the solution when both hydrometers are immersed. This screen provides
a dark ellipse around the stem of the hydrometer. This ellipse becomes a thin
straight line as the head is raised to bring the eye to a position exactly on the
level of the surface of the liquid. With the eye at this level the reading of each
hydrometer is taken without altering the position of the head. Readings are
thus obtained on the two hydrometers under identical conditions.
The scale is checked at each end of the range and at a third point
approximately in the middle.
Polarimeter Tubes
For the calibration of length of polarimeter tubes a comparator (Fig. 30)
which incorporates two dial gauges is employed. Each tube is compared with
a standard bar of known length, the dial gauge measuring the difference
between the lengths of the tube and the bar to an accuracy better than 0.01
mm. The two dial gauges provide a check on the accuracy of measurement;
a difference between the two readings indicates that a check on the dial gauges
is necessary. This calibration is carried out in the constant temperature room
Tolerances for tubes are shown in Table XXV.
Cover Glasses
("over glasses for polarimeter tubes are checked for strain by means of a
strain viewer. They are also examined to ensure that the surfaces are plane
parallel and free from scratches or other defects.
Saccharimeters
The scales of saccharimeters are calibrated bv
by means of live standard
quartz plates.
nlates. These plates cover a range from
Saccharimeters are also examined for correct mechanical and optical
operation and anv
any defective parts are replaced where possible. The tolerance
is shown in Table XXV.
Quartz Plates
Ouartz control plates for use with quartz wedge saccharimeters are
tested in a Hates Fric saccharimeter for S rotation. The rotation in angular
degrees for subsequent conversion to S is also determined in a Schmidt and
Haensch polarimeter using the sodium yellow 5892 A or the mercury green
5461 A wavelengths of light. Ouartz plates are also tested for uniform thick-
ness and lor any strain due to incorrect mounting.
Refractometers
Abbe refractometers are tested against calibrated liquids and glass
standards covering the range 1.33 to 1.65 refractive index at 20 C.
Balances
Balances up to a maximum capacity of five kilogrammes are tested
according to the principles set out in Chapter III.
Weights
Weights of values up to 1(H) gramme are standardized on the basis of
weighings made in air of density 0.00120 g/ml against standard weights of
density S.O g/ml. The method of double weighing is used.
Volumetric Glassware
Calibration of volumetric glassware is determined according to the
method set out in Chapter V for each item of glassware.
CHAPTER VII
SAMPLING OF SUGAR MILL PRODUCTS

In the preceding chapters considerable attention has been paid to the
necessity for precision in all apparatus employed in sugar laboratory control
work. However, accurate apparatus and refined methods of analysis are
totally worthless if the material analysed is not representative of the total
substance, the composition of which it is desired to determine. Sugar-mill
products in particular present a most difficult problem in this regard, but
unless complete and accurate methods of sampling are employed the labora-
tory control must be regarded as only approximate and indefinite.
The method of sampling depends, of course, on the nature of the partic-
ular product; and further, an accurate analytical result is of little value for
control purposes if the total quantity of substance is not, in turn, accurately
determined. Thus, a true analysis of a representative sample of mixed juice
gives no measure of the quantity of sugar entering manufacture, unless the
true quantity of such juice is also known. The necessity for the highest
degree of precision in both sampling and measuring cannot be overemphasized.
Yet all too often one finds that the supervision of these operations is placed
in the hands of juniors, while the expert technician performs the analyses.
It is certainly true that greater precision in results is often obtained by
having the chief chemist carry out the sampling and by leaving the analyses
to the laboratory junior, but it must be emphasized that, whoever takes the
sample, it must be taken in a completely unbiased manner.
It must always be remembered that even the best sampling methods are
approximate, and chemists should be continually on the watch for improve-
ments in technique. The following methods are regarded by the Bureau as
being simple and practicable, and at the same time, not unscientific.
Cane
The correct sampling of a field of cane is quite a difficult matter. As the
result of studies which have been carried out, it has been found that a large
number of individual sticks must be selected at random from all parts of the
field if an accurate estimate of its c.c.s. is desired. The number of stalks
necessary depends on the degree of variation in crop growth from point to
point in the block, particularly if the crop is far removed from maturity.
From 20 to 50 sticks should be regarded as the range of sampling necessary.
The best method for determining the degree of maturity of a crop is to carry
through a series of systematic tests.
The collection of stick samples for fibre analysis was formerly a universal
practice at Queensland mills. This method of cane sampling is fully described
in Regulation 57 of the Regulation of Sugar Cane Prices Act, but it has been
largely replaced by the practice of sampling prepared cane. Prepared cane
samples can be used for the determination of cane fibre by disintegrating the
sample in a hammermill or cutter grinder, transferring the sample to a fibre
bag and determining fibre in the usual manner; or the prepared cane samples
can be used for direct analysis of cane, utilizing the wet disintegrator to
determine Brix and pol and a Spencer or similar type of air stream oven to
determine moisture. Prepared cane is usually obtained from the elevator
feeding into the number one mill hopper by means of a hydraulically or
SAMPLING OF SUGAR MILL PRODUCTS 79
pneumatically operated door in the b o t t o m of t h e elevator. In order to avoid

t h e risk of i n c o r r e c t s a m p l i n g c a u s e d by t h e p o s s i b i l i t y of s e g r e g a t i o n in t h e
carrier, i t i s i m p o r t a n t t h a t t h e d o o r c o v e r a s m u c h o f t h e w i d t h o f t h e
e l e v a t o r a s possible. T h e d o o r o p e n i n g s h o u l d also b e sufficiently w i d e t h a t
a free fall of t h e full d e p t h of t h e c a n e in t h e e l e v a t o r o c c u r s . T h e p r e p a r e d
c a n e is u s u a l l y allowed to fall o n t o a l a r g e s a m p l i n g t a b l e w h e r e it is s p r e a d
o u t a n d s u b - s a m p l e d b y h a n d for h a m m e r - m i l l i n g o r d i s i n t e g r a t i o n . V a r i o u s
a v e n u e s for a u t o m a t i c m e c h a n i c a l s u b - s a m p l i n g a r e a t p r e s e n t b e i n g i n -
vestigated.
Juice
Various devices are employed for obtaining continuous samples of juice
from the mills and juice gutters. The simplest form is probably a metal
container provided with a conical lid in which a small hole has been drilled.
This hole is covered with fine gauze to exclude bagasse particles. The con-
tainer is usually suspended in the stream of juice from the first roller of the
train. Tests have shown that if three such vessels are suspended beneath the
same roller the samples collected may vary in composition within relatively
wide limits, and, therefore, it is essential to collect a sample from the full
length of the roller.
This may be done by fitting a trough beneath the roller in such a way
that the entire quantity of juice expressed by the roller is collected. At the
centre of the trough a cup is provided to which is attached a large downpipe
several inches long. The sampler is placed directly below the centre of the
outlet.
This method suffers from a serious disability. The sample is collected
at a uniform rate, irrespective of the rate of juice flow. With normal crushing
the variation will not be great, and the sample obtained should be fairly
representative of the entire juice; but this limitation should be borne in
mind in those areas where the cane supply is frequently highly variable.
The size of the hole in the container determines the capacity of the
sampler. If the hole is too large frequent changes are necessary, while if too
small the sample is insufficient. For normal sampling the hole is made of such
dimensions as to provide a gallon of sample juice every four hours.
For first expressed juice sampling this method has now been superseded
by automatic continuous devices. Several types are in use in Queensland,
but in all the collection of the sample involves the use of a trough to catch the
juice, this trough being constructed to conform with Regulation 57 of the
Regulation of Sugar Cane Prices Act. All of the juice flow from this trough
is collected and fed into the suction of a juice sampling pump. By means of a
proportioning device, part of the juice flow from the pump is diverted to a
sample can system located adjacent to the first mill or in the laboratory, and
the remainder returned to the mill bed. Normally the sample cans are held
in an automatic sampling device which changes the sample flow from one
can to the next as each successive rake of cane comes through the first mill.
The samples are identified by means of pins or balls in sample wheels which
have their speeds geared to the speed of the carrier or elevators, or, in the
most recent type of automatic sampler, the samples are tracked through the
conveying system electronically. This electronic sampler also has the facility
of being able to alter the proportioning device so that a more or less constant
quantity of juice is collected for each rake of cane, irrespective of the length
of the rake.
Sampling from juice gutters also presents difficulties. The best device
for this purpose is a small under-shot water wheel. One of the spokes is made
SO SAMPLING OF SUGAR MILL PRODUCTS
hollow and terminates in a spoon-shaped blade. This spoon takes up a little

of the juice, which flows down the spoke to the hollow axle which is provided,
and thence into the container. The main objection to this type is that the
small pipes are liable to become choked, after which sampling will cease.
In order to ensure a true average sample, small baffles should be fitted in the
trough upstream from the wheel to effect a thorough mixing of the juice.
Sampling of mixed juice, particularly where suspended matter deter
minations are to be carried out on the juice, is best accomplished by means
of a pitot-tube type sampler placed in the delivery pipe from the mixed juice
pump. In this way, a sample of the juice is taken before the suspended solids
have had a chance to settle, and a reasonably accurate sample can be obtain-
ed. A moving receiving tube which passes at regular intervals through the
juice flowing from the sampling tube comprises an efficient method of sub-
sampling the main sample flow.
Syrup
With the replacement of reciprocating syrup pumps by centrifugal
pumps, samplers such as the Calumet described in earlier editions of this
Manual are no longer applicable for the purpose of syrup sampling. Continu-
ous sampling of syrup may be effectively carried out by piping a small sample
of syrup from the pump delivery line and sub-sampling this smaller flow by
means of a sample splitter. Syrup samplers must be checked and cleaned
at regular intervals to ensure that crystallization does not occur, thus blocking
the sampler. If continuous sampling is not used, syrup may be snap sampled
at regular intervals and the snap samples composited over a period. Preserv-
ative is not required for syrup, molasses, or massecuite samples.
Massecuites and Molasses
The composition of massecuite varies from point to point within the pan,
due to imperfect circulation, and therefore the sample should be taken
continuously as the massecuite is discharging. For control purposes a "snap"
sample is usually sufficient, though for preference three such samples should
be taken and composited for each strike. These should be drawn at regular
intervals as the massecuite is discharged, but the first should not be taken
from the first flow of massecuite. In compositing samples of massecuite, care
must be taken that the respective portions are proportional to the quantity
of massecuite which each represents.
Molasses may be sampled similarly to syrup (q.v.) and similar precautions
as with syrups should be taken in preparing a representative composite
sample. It is preferable to obtain a continuous sample of final molasses. A
convenient sampler for those mills using molasses scales is to fit a small pipe
leading from the receiving tank to a sample container. Each time the weighing
tank discharges, the inlet to this pipe is submerged to a similar depth, and
the quantity of molasses transferred to the container is uniform.
Raw Sugar
Raw sugar is now handled in bulk in Queensland, and sugar sampling
at the bulk terminals is carried out by removing a portion of the sugar from
the bulk containers as they are being discharged. At the mill various devices
are being used for sugar sampling. Theoretically, it is best to sample from a
stream in free fall, and, if the practical difficulties could be overcome, this
could be achieved on a sugar belt if the belt were fitted with a sampling gap,
almost the full width of the belt, and a sample can placed under the belt at the
feed point. This is however, a rather difficult and expensive method of
SAMPLING OF SUGAR MILL PRODUCTS 81
sampling and samples are usually obtained by means of motor-driven samp-
ling spoons or other devices. The disadvantages of these devices are that,
unless very sophisticated control equipment is used, they are not strictly
proportional to sugar rate and are easily fouled by wet sugar.
Bagasse
The accurate sampling of bagasse is a very difficult problem. Here,
again, no satisfactory continuous sampler has been devised and hand
sampling is necessary. In general the analyses of final bagasse samples are
not considered individually, but only with reference to their average value,
hence advantage may be taken of the fact that bagasse can be preserved for
reasonable periods. In this way samples may be taken at frequent intervals
without increasing the number of analyses to be made by the chemist.
For final bagasse the compositing of samples taken at short intervals,
and the subsequent analysis of the well mixed sample, is strongly recom-
mended in preference to the taking of "snap" samples once or twice per shift.
The former method is far more representative of the bagasse in process, and
the sampling procedure described below does not inflict any extra work on
the analyst.
For sampling bagasse a small chute the width of the bagasse blanket is
provided. This chute is held across and below the falling bagasse, and when
it is full the contents are transferred to a closed container containing pre-
servative. A suitable type is shown in Fig. 37. The chute should hold 2 or 3 lb
of final bagasse so that the resulting
total sample is about 30-50 lb.
When the composite is completed
the large sample is spread out,
rapidly but effectively mixed, and
then sub-sampled for analysis.
The mixing must be carried out
thoroughly, otherwise the whole
sampling process will have been
wasted; but it must be done
quickly to avoid moisture loss by
evaporation. This loss is to a
certain extent minimized by the
fact that, by the time mixing is
carried out, the temperature of
the sample will have dropped to
approximately that of its sur-
roundings.
In mills where sudden
changes in varieties and condi-
tions occur, half an hour should
be the maximum interval, whilst
in others where conditions are
comparatively uniform a one-hour
period is permissible. The time
schedule for sampling should be
adhered to, irrespective of milling
conditions, as long as the mill is
crushing. The composite sample Fig. 37—Illustrating container recommended
is preserved by means of a pad for compositing samples of bagasse.
82 SAMPLING OF SUGAR MILL PRODUCTS
s a t u r a t e d w i t h s t r o n g a m m o n i a a n d c h l o r o f o r m ( p r o p o r t i o n s 6 : 1) or
t o l u e n e . W h i l e , a s m e n t i o n e d p r e v i o u s l y , final b a g a s s e c a n b e p r e s e r v e d
for a r e a s o n a b l e l e n g t h of t i m e , four h o u r l y a n a l y s i s p e r i o d s a r e c o n s i d e r e d
p r e f e r a b l e to a o n c e p e r shift a n a l y s i s of t h e c o m p o s i t e .
S a m p l e s f r o m earlier mills i n t h e t r a i n a r e u s u a l l y i n t e n d e d t o s u p p l y
t h e e n g i n e e r w i t h specific i n f o r m a t i o n a n d m a y n o t b e i n t e n d e d for c o n t r o l
p u r p o s e s . H o w e v e r , s o t h a t t h e s e s a m p l e s c a n b e reliable, t h e y s h o u l d b e
t a k e n o v e r a p e r i o d o f t i m e w i t h a shovel. I t i s i m p o r t a n t t h a t t h e full d e p t h
o f b a g a s s e b e s a m p l e d since t h e t o p s u r f a c e m a t e r i a l h a s a h i g h e r j u i c e c o n t e n t
t h a n t h e r e m a i n d e r . Also s a m p l i n g s h o u l d b e c a r r i e d o u t a c r o s s t h e full
w i d t h of t h e roller.
Filter Cake
With the rotary filter, next to weighing at regular intervals the complete
out-turn of cake in a given time, the following procedure is recommended.
The length of the filter is divided into a suitable number of equal portions.
At half hourly intervals the mud from one or more screen segments (depend-
ing on the size of the screens and the length of the portion) is caught on a
suitable tray. This quantity of mud from the known area of screen is then
weighed, and a small area removed by means of a sampler resembling a scone
cutter. The weight of mud in each trayful is recorded and the small samples
composited in a closed container for subsequent analysis. At the end of a
period the total weight of cake produced by the filter can be calculated from
the following expression:—
where W = total weight of cake for the period, in tons

w = average weight contained on mud sample tray in pounds
n — revolutions of filter during period (preferably obtained
from revolution counters)
a = area of cake removed by the mud sample tray
A = area of screen surface on the filter.
The weight of pol in mud can then be calculated from the cake weight
and the pol per cent cake determined on the composited sample. Composite
mud samples cannot be effectively held for pol determination for periods
much longer than four hours, and analysis of mud samples for pol twice per
shift is recommended.
Care of Samplers and Containers

All sugar-mill products are susceptible to rapid deterioration due to
bacterial activity; it is therefore imperative that all sample containers be
maintained in a thoroughly clean condition and be subjected to frequent
sterilization. Sample jars should be washed with hot water after each usage
and thoroughly dried. Metal containers (preferably of stainless steel) should
be frequently washed and steamed.
Preservation of Samples
Preservation of certain specific samples has been discussed in this
chapter, but details of common preservatives and recommendations for their
use will be found in the chapter on laboratory reagents.
CHAPTER VIII
LABORATORY R E A G E N T S
This chapter has been re-arranged by listing, wherever possible, the

various reagents under each specific analysis. Celite and Triethanolamine,
for example, are included under the heading of "Filterability Determination".
It is anticipated t h a t this method of presentation will expedite analytical
procedure.
Poisons: A good analyst is familiar with the reagents being used and
their individual properties. The repeated use of common reagents, however,
C o m m o n Toxic Materials
General Toxicity
Highly toxic. Avoid inhalation of the vapour.

Poisonous, combustible, volatile with steam.
A narcotic agent with insidious chronic
effects.
Prolonged exposure to low concentrations
can result in chronic irritation of the
nervous system—an acute narcotic agent
in high concentrations.
Highly toxic gas. Not readily detected by
the senses at a concentration of one p.p.m.
Highly corrosive. Explosive when mixed
with certain organic solvents.
Toxic. Included in this table for compara-
tive purposes.
A very poisonous gas. A chemical commonly
taken too lightly. Higher concentrations
are very dangerous as the sense of smell
becomes paralysed.
Cumulative poisons. Refer to the special
precautions listed in this chapter.
Highly toxic. Can be absorbed via the re-
spiratory tract or by contact with the
skin.
Corrosive to all tissues. Permanent damage
to the respiratory tract can result from
prolonged contact.
Highly corrosive. Severe lung damage can
result from inhalation of the vapour.
Prolonged exposure to low concentrations
can cause inflammation of nasal and
throat tissues.
Narcotic agent. Its toxicity is considered
to be associated with the benzene concen-
tration present as an impurity.
Highly toxic. Do not inhale or allow this
chemical to come in contact Avith the skin.
Parts of gas or vapour per million parts of air by volume.

No specific level adopted at this stage by the National Health and Medical Re-
search Council of Australia.
84 LABORATORY REAGENTS
can t e n d to allow a "familiarity b r e e d s c o n t e m p t " a t t i t u d e to arise. T h e

m a j o r i t y of c h e m i c a l s u s e d in s u g a r l a b o r a t o r i e s a r e highly toxic substances,
a n d for t h e s a f e t y o f all c o n c e r n e d , t h i s p o i n t c a n n o t b e e m p h a s i z e d t o o
strongly. Some general information on t h e toxic properties of some of t h e
more commonly used chemicals in sugar laboratories is listed above in t a b u l a r
f o r m . T h e m a x i m u m p e r m i s s i b l e levels i n t h i s t a b l e a r e t h e t h r e s h o l d l i m i t
values which h a v e been proposed by t h e American Conference of Govern-
m e n t a l I n d u s t r i a l H y g i e n i s t s , a n d w h i c h h a v e also b e e n r e c o m m e n d e d b y t h e
N a t i o n a l H e a l t h a n d Medical Research Council of Australia. However, t h e
fact t h a t a chemical is n o t listed in this table does n o t necessarily m e a n t h a t
i t i s n o t t o x i c , a n d all l a b o r a t o r y c h e m i c a l s a n d r e a g e n t s s h o u l d b e h a n d l e d
as if t h e y were poisonous. W h e n k n o w n toxic or corrosive chemicals are
being used the wearing of the appropriate protective equipment, such as
goggles, g l o v e s , a n d r e s p i r a t o r s , i s s t r o n g l y r e c o m m e n d e d .
Boiler Water Analysis

Alkalinity
Barium Chloride Solution—Dissolve 10 g of b a r i u m c h l o r i d e B a C l 2 . 2 H 2 0
i n d i s t i l l e d w a t e r a n d d i l u t e t o 100 m l .
Methyl Orange Indicator—Dissolve 0.10 g of m e t h y l o r a n g e in 100 ml of
h o t w a t e r , cool, f i l t e r i f n e c e s s a r y a n d a d j u s t t o v o l u m e .
Phenolphthalein Indicator—Dissolve 1.0 g of p h e n o l p h t h a l e i n in 60 ml
of industrial m e t h y l a t e d spirits. W h e n dissolved, a d d 40 ml of water, m i x
well, filter i f n e c e s s a r y a n d a d j u s t t o v o l u m e .
Sodium Sulphate Crystals—Reagent grade Na2S04.10H2O.
Sulphuric Acid 0 . 0 2 N — D i l u t e 10.0 ml of 1 . 0 0 N s t a n d a r d s u l p h u r i c a c i d
to 500 ml w i t h distilled water. T h e p r e p a r a t i o n of 1 . 0 0 N s t a n d a r d acid is
described elsewhere in this chapter.
Phosphate
Acid Molybdate Solution—Dissolve w i t h o u t h e a t i n g , 8.8 g of a m m o n i u m
m o l y b d a t e i n 100 m l o f w a t e r . I n a s e p a r a t e c o n t a i n e r , c a r e f u l l y a d d 3 8 m l
of concentrated sulphuric acid to a p p r o x i m a t e l y 300 ml of water. Allow t h e
d i l u t e d a c i d t o cool t o r o o m t e m p e r a t u r e a n d t h e n t r a n s f e r t h i s s o l u t i o n a n d
t h e a m m o n i u m m o l y b d a t e t o a 5 0 0 m l v o l u m e t r i c flask. D i l u t e t o v o l u m e
w i t h distilled w a t e r .
Hydroquinone—Dissolve 0.5 g of h y d r o q u i n o n e in 50 ml of 0.02N sul-
p h u r i c acid. S t o r e i n a d a r k o r a m b e r c o l o u r e d b o t t l e .
Carbonate—Sulphite Solution—Dissolve 130 g of a n h y d r o u s p o t a s s i u m
c a r b o n a t e a n d 24 g of s o d i u m sulphite ( N a 2 S 0 3 . 7 H 2 0 ) in 500 ml of w a t e r .
Hardness
Wanklyns Soap Solution—This is u s u a l l y p u r c h a s e d as a p r e p a r e d r e a g e n t
from a chemical supplier.
Sodium Sulphite
Potassium Iodate—Iodide Solution—Dissolve 0 . 7 1 3 g of p o t a s s i u m i o d a t e
in 2 0 0 ml of w a t e r a n d t h e n a d d 7 g of p o t a s s i u m i o d i d e a n d 0.5 g of s o d i u m
b i c a r b o n a t e . W h e n d i s s o l v e d , t r a n s f e r t o a o n e l i t r e v o l u m e t r i c flask a n d
dilute to volume.
Starch Indicator Solution—Mix 0.5 g of s o l u b l e s t a r c h w i t h 5 ml of c o l d
w a t e r , a n d t h e n a d d 100 m l o f b o i l i n g w a t e r . H e a t o n a b o i l i n g w a t e r b a t h
LABORATORY REAGENTS 85
for 5 m i n u t e s , cool a n d s t o r e in a r e f r i g e r a t o r . (A c o m m e r c i a l solid i n d i c a t o r

p r e p a r a t i o n c a n also b e u s e d ) .
Sulphuric Acid, 6.5 per cent v/v.—Carefully a d d 65 ml of c o n c e n t r a t e d
s u l p h u r i c a c i d t o a p p r o x i m a t e l y 9 0 0 m l o f distilled w a t e r . Cool t o r o o m
t e m p e r a t u r e a n d dilute to a volume of one litre.
Sulphate
Barium Chloride, 0 . 0 4 N — D i s s o l v e 4 . 8 8 6 g of b a r i u m c h l o r i d e ( B a C l 2 .
2 H 2 0 ) in distilled w a t e r a n d dilute to a volume of one litre.
EDTA—(Diaminoethanetetra—acetic acid, disodium salt), 0.02N.—Dis-
solve 3.72 g of E D T A in d i s t i l l e d w a t e r a n d d i l u t e to a v o l u m e of o n e l i t r e .
Hydrochloric Acid, 0 . 5 N approximately—Measure o u t 45 ml of c o n c e n -
t r a t e d h y d r o c h l o r i c a c i d ( d 1.18) a n d p o u r i n t o a p p r o x i m a t e l y 5 0 0 m l o f
water. Mix a n d t h e n dilute to a volume of one litre.
Solochrome Black Indicator—Weigh o u t 0.5 g of s o l o c h r o m e b l a c k
W . D . F . A . a n d d i s s o l v e in a b o u t 2 ml of h o t w a t e r . A d d 10 g of s o d i u m chlor-
i d e , m i x t h o r o u g h l y a n d d r y a t 105 °C. W h e n d r y , a d d 9 0 g o f s o d i u m c h l o r i d e
a n d g r i n d t h o r o u g h l y . T h i s i n d i c a t o r c a n also b e p u r c h a s e d i n t a b l e t f o r m .
Sulphate Buffer Solution—To 56.5 ml of a m m o n i a (d = 0.880) a d d 4.125
g o f a m m o n i u m c h l o r i d e a n d m a k e u p t o 5 0 0 m l w i t h w a t e r . A d d 3.72 g o f
E D T A , m i x a n d t h e n a d d 2.03 g o f m a g n e s i u m c h l o r i d e ( M g C l 2 - 6 H 2 0 ) .
Buffer S o l u t i o n s
pH 4 . 0 0 Potassium Hydrogen Phthalate Buffer—Dissolve 10.21 g of d r y
p o t a s s i u m h y d r o g e n p h t h a l a t e A . R . i n freshly distilled w a t e r . D i l u t e t o o n e
l i t r e . T h e p H o f t h i s s o l u t i o n i s defined a s b e i n g 4.00 a t 1 5 ° C a n d 4 . 0 1 a t 3 0 °C.
pH 6.85 Mixed Phosphate Buffer—Dissolve 3.402 g of p o t a s s i u m d i -
h y d r o g e n p h o s p h a t e K H 2 P 0 4 a n d 4.45 g of disodium h y d r o g e n p h o s p h a t e
N a 2 H P 0 4 . 2 H 2 0 i n freshly distilled w a t e r a n d d i l u t e t o o n e l i t r e . T h e p H o f
t h i s buffer i s 6.85 a t 2 5 ° C a n d i t h a s a negligible p H c h a n g e o v e r t h e r a n g e
of ordinary room t e m p e r a t u r e .
pH 9.18 Borax Buffer—Dissolve 19.071 g of s o d i u m b o r a t e N a 2 B 4 0 7 .
1 0 H 2 O i n f r e s h l y distilled w a t e r a n d d i l u t e t o o n e l i t r e . T h e s o l u t i o n h a s a
p H of 9.18 a t 2 5 °C a n d 9.07 a t 38 °C.
Clarifiability T e s t
Lime-Sucrose Reagent
T w o solutions are initially required:
S o l u t i o n A: D i s s o l v e 150 g of refined s u g a r in a p p r o x i m a t e l y 60 ml of
hot water.
Solution B: Slowly add, with stirring, 15 g of A . R . calcium oxide to
100 ml of a l m o s t b o i l i n g w a t e r .
Carefully m i x s o l u t i o n B i n t o s o l u t i o n A . F i l t e r t h e h o t s o l u t i o n t h r o u g h
a 6 3 3 A o r s i m i l a r t y p e o f filter p a p e r u n d e r v a c u u m , u s i n g S u p e r c e l f i l t e r a i d .
T h e filtered s o l u t i o n m u s t b e s t o r e d i n a r e f r i g e r a t o r , w h e r e i t will k e e p for
a p p r o x i m a t e l y three weeks.
Filterability Determination
Triethanolamine Buffer Solution—Two solutions are prepared separately
in 50 per cent w/w glycerol solution.
Solution A: Dissolve 15.0 g of A.R. calcium acetate in approximately

300 ml of 50 per cent glycerol solution in a beaker. Mild heating may be used.
Solution B: In a second beaker, dissolve 400 g of triethanolamine with
approximately 200 ml of 50 per cent glycerol.
N.B.—Triethanolamine can cause severe skin irritation. Avoid direct contact.
Transfer solutions A and B to a one litre volumetric flask and use
50 per cent glycerol to rinse both beakers and to dilute to volume. Mix well
and allow to stand overnight.
Add a small quantity of filter aid and filter. Store in a stoppered clear
glass bottle.
Celite—This is a standard filter aid No. 505, wrhich has been standardized
by the C.S.R. Company. No other type of filter aid is directly applicable to
this test.
Glass Cleaning Solution
Dissolve 80 g of potassium bichromate (K 2 Cr 2 0 7 ) in 300 ml of water in a
litre pyrex beaker and cool to room temperature. Carefully add 460 ml of
concentrated sulphuric acid with stirring. The addition of the acid precipitates
chromic acid, and the solution will act as an effective cleaning agent while
red crystals of this compound are present.
Glass cleaning solution is extremely toxic and highly corrosive. All
necessary precautions should be observed and it is advisable to stand the
bottle in a lead tray so that damage to bench surfaces can be minimized.
Indicators
The preparation and characteristics of indicators for selected pH ranges
are listed below:
Indicator Preparation pH Range Colour Change
Methyl Violet 0.25 g per 100 ml of water 0.1—1.5 Yellow to blue
Ouinaldine Red 0.10 gin 100 ml of ethyl alcohol 1.4—3.2 Colourless to red
Methyl Orange 0.10 g per 100 ml of water 3.1—4.4 Red to orange
Bromphenol Blue 0.10 g in 8.6 ml of 0.02 x. 3.0—4.6 Red to orange
NaOH. Dilute to 250 ml with
water.
Bromcresol Green 0.10 g in 7.15 ml of 0.02 N. 3.8—5.4 Yellow to blue
water.
Methyl Red 0.10 g in 18.6 ml of 0.02 x. 4.2—6.2 Red to yellow
water.
Bromphenol Red 0.10 g in 9.75 ml of 0.02 x. 5.2—7.0 Yellow to red
water.
Bromthymol Blue 0.10 g in 8.0 ml of 0.02 x. 6.0—7.6 Yellow to blue
water.
Phenol Red 0.10 g in 14.2 ml of 0.02 N. 6.8—8.4 Yellow to red
water.
Cresol Red 0.10 g in 13.1 ml of 0.02 x. 7.2—8.8 Yellow to red
water.
Phenolphthalein 1.0 g in 60 ml of ethyl alcohol. 8.2—10.0 Colourless to red
Dilute to 100 ml with distilled
water.
Thymolphthalein 0.10 g in 100 ml of ethyl 9.3—10.5 Colourless to blue
alcohol.
Alizarin Yellow 0.10 g in 100 ml of 50% ethyl 10.0—12.0 Yellow to lilac
alcohol.
Phosphate Analysis
Acid Molybdate Solution—Dissolve 16.6 g of ammonium molybdate in
600 ml of distilled water. Gentle heating may be used, but the temperature
must not rise above 60 °C.
Carefully add 96 ml of concentrated sulphuric acid and cool. Dilute to
one litre with distilled water. Store in a dark bottle in a cool place.
Acid Reagent—Carefully add 96 ml of concentrated sulphuric acid to 600
ml of distilled water. Cool and dilute to one litre.
Acid Washed Supercel—Add 50 g of supercel to one litre of distilled
water. Add 50 ml of concentrated hydrochloric acid and stir for 5 minutes.
Vacuum filter the slurry and wash with distilled water until no trace of acid
remains (silver nitrate test). Dry the supercel at 100 °C for 6 hours and
store in a screw top jar.
Amidol Reagent—Dissolve 1.0 g of amidol and 20 g of sodium metabi-
sulphite in distilled water. Dilute to a volume of 100 ml. Add a level teaspoon
of acid washed supercel and filter under vacuum through two Whatman No. 5
filter papers. Store in a dark bottle and hold under refrigeration. Prepare
freshly each week.
Standard Phosphate Stock Reagent—Dry approximately 2 g of A.R. potas-
sium dihydrogen phosphate (KH 2 P0 4 ) for 1 hour at 110 °C. Weigh out
1.0984 g of the dried salt, dissolve in distilled water and dilute to 250 ml in
a volumetric flask. This reagent contains 1.00 mg/ml of P and should keep
for about two years if a few ml of chloroform are added and it is stored in a
refrigerator.
Standard Phosphate Solution—Pipette 10.0 ml of the stock reagent into
a one litre volumetric flask and dilute to volume. This solution contains
0.01 mg/ml of P and is used for the preparation of the standard phosphate
graph as described in Chapter IX.
Pol Determination
Acetic Acid 1 + 4—This solution is usually prepared in relatively large
quantities. Apart from its use in pol determinations, the solution is effective
for removing precipitated lead salts from volumetric glassware.
To prepare a litre of 1 + 4 solution, add 200 ml of glacial acetic acid
to distilled water in a litre measuring cylinder and dilute to volume.
Herles' Reagents—Two separate stock solutions are prepared in the
following manner :
Solution A—Dissolve 50 g of A.R. sodium hydroxide pellets with
distilled water in a litre volumetric flask. Dilute to volume after cooling.
Solution B—Dissolve 500 g of lead nitrate with distilled water in a litre
volumetric flask. Dilute to volume.
Reagent Check—Dispense an equal volume of solution A and solution B
into a beaker. Determine the pH of the resultant mixture. If the value
obtained is not below 7 pH, solution A must be diluted until the resultant
mixture gives an acid reading.
N.B.—Sodium hydroxide and lead nitrate are dangerous solutions when
prepared to the above concentrations. They should not be dispensed with
mouth aspirated pipettes.
Lead Acetate
Safety Precautions with Lead Compounds:—Lead s a l t s a r e c u m u l a t i v e
p o i s o n s a n d t h e following r u l e s s h o u l d b e o b s e r v e d w h e n a n y l e a d c o m p o u n d s
or solutions containing lead are being used.
1 . Vessels c o n t a i n i n g l e a d s o l u t i o n s m u s t b e l a b e l l e d " P o i s o n " .
2. Do not open containers of d r y lead a c e t a t e in an enclosed room.
A v o i d b r e a t h i n g t h e fine d u s t o f t h i s s u b s t a n c e , e s p e c i a l l y w h e n
transferring it from one container to another.
3. Always wash the h a n d s thoroughly after handling d r y lead a n d
polarizing solutions.
4 . A v o i d w i p i n g t h e face o r e y e s w i t h a l a b o r a t o r y glass t o w e l a n d d o
n o t u s e t h e s e t o w e l s for w i p i n g e a t i n g u t e n s i l s .
5. K e e p t h e reagents a n d polarizing solutions a w a y from cuts or a b r a -
sions.
6 . D o n o t u s e p o l a r i z a t i o n filter-glasses for d r i n k i n g p u r p o s e s .
7 . T h e a p p a r a t u s a n d p r o c e d u r e s u s e d for p r e p a r i n g o r t r a n s f e r r i n g w e t
or d r y lead should be such t h a t there is no risk t h a t an analyst m a y
ingest or absorb a n y of t h e reagent.
8. A s u p p l y of a n t i d o t e s s h o u l d be p r o v i d e d in a c e n t r a l p l a c e in a
laboratory, together with instructions as to how they should be used,
viz. 1 0 p e r c e n t a q u e o u s m a g n e s i u m s u l p h a t e , followed b y m i l k o r
a l b u m e n i n cold w a t e r .
9. A n o t i c e c o n t a i n i n g t h e a b o v e p r e c a u t i o n s s h a l l be p o s t e d in a p r o m i -
n e n t place in t h e laboratory.
Basic Lead Acetate Powder—The m o r e i m p o r t a n t specifications p e r t a i n -
ing to t h e quality of basic lead a c e t a t e powder are shown below:
T o t a l L e a d (as P b O ) * * : N o t less t h a n 7 5 . 0 p e r c e n t
B a s i c L e a d (as P b O ) * * : N o t less t h a n 3 3 . 0 p e r c e n t
Moisture*: N o t m o r e t h a n 1.5 p e r c e n t
Insoluble in water: N o t m o r e t h a n 2.0 p e r c e n t
Insoluble in acetic acid: N o t m o r e t h a n 0.05 p e r c e n t
A n a d d i t i o n a l specification t o m e e t A u s t r a l i a n r e q u i r e m e n t s i s t h a t
7 5 p e r c e n t m u s t p a s s t h r o u g h a 115 m e s h T y l e r sieve a n d 100 p e r c e n t m u s t
p a s s t h r o u g h a 3 5 m e s h T y l e r sieve.
* M o i s t u r e is d e t e r m i n e d by d r y i n g 1 g of s a m p l e at 100 °C for 2 h o u r s .
**Total a n d Basic Lead are determined by the National B u r e a u of S t a n d a r d s
M e t h o d ( b a s e d o n C i r c u l a r C . 4 4 0 p . p . 120-122).
Basic Lead Acetate Solution (Wet Lead)— D i s s o l v e 5 6 0 g of b a s i c l e a d
a c e t a t e p o w d e r ( c o n f o r m i n g t o t h e a b o v e r e q u i r e m e n t s ) i n o n e l i t r e o f freshly
boiled distilled w a t e r , w h i c h h a s p r e v i o u s l y b e e n cooled, i n a s e a l e d c o n t a i n e r .
Boil for 3 0 m i n u t e s a n d a l l o w t o s e t t l e o v e r n i g h t i n a sealed c o n t a i n e r .
S t a n d a r d i z a t i o n : D e c a n t t h e s u p e r n a t a n t l i q u i d . D i l u t e w i t h freshly b o i l e d
distilled w a t e r to 1.25 specific g r a v i t y (54 B r i x ) .
T h e m e t h o d s o f a n a l y s e s p r e v i o u s l y specified for b a s i c l e a d a c e t a t e
powder are again employed, with t h e variation t h a t 25 ml of wet lead solution
a r e s u b s t i t u t e d for t h e o r i g i n a l 5 g s a m p l e w e i g h t . I C U M S A specifies t h a t w e t
l e a d m u s t c o n t a i n b e t w e e n 9.6 a n d 10.5 g of b a s i c l e a d ( e x p r e s s e d as P b O )
p e r 100 m l o f s o l u t i o n . I f t h e q u a n t i t y d e t e r m i n e d i s a b o v e t h i s r a n g e , t h e
calculated volume of glacial acetic acid should be a d d e d a n d t h e analysis
repeated.
N.B.—The basic lead acetate solution should be stored in a stoppered con-

tainer and labelled "Poison".
Neutral Lead Acetate Solution—A 10 per cent solution is used i.e. dissolve
100 g of lead acetate Pb(C 2 H 3 0 2 ) 2 in distilled water and dilute to one litre.
The pH of the solution is then determined and adjusted to 7.0 with either
acetic acid or sodium hydroxide.
Preservatives
Mercuric Chloride—Highly toxic. Prepare a saturated solution of the salt
in alcohol. Store in a suitable automatic dispenser and use at the rate of
0.5 ml per litre of juice.
N.B.—Mercuric chloride cannot be used in samples taken for reducing sugar
analysis.
Phenyl Mercuric Acetate {P.M.A.)—Prepare a solution containing 1 g of
the salt per litre. Label "Poison" and store in a suitable automatic dispenser.
The following table is presented as a rough guide for the preservation
and storage of samples for routine mill analysis. The recommendations are of
a general nature but should provide effective preservation of normal samples
under average factory conditions.
Preservation of Samples
*The calculated amount of lead acetate should be added with each aliquot in order
to avoid overleading of initial portions of the sample.
Reducing Sugar Analysis

Methylene Blue Solution—Dissolve 1 g of methylene blue powder in 100
ml of distilled water. This reagent must be freshly prepared at least every six
months.
Phosphate-Oxalate, Deleading Solution—Dissolve 30 g of C.P. potassium
oxalate (K 2 C 0 0 4 ) in 400 ml of distilled water, and 70 g of disodium phosphate
(Na 2 HP0 4 .12H 2 0) in another 400 ml portion of distilled water. Pour the
two solutions into a one litre volumetric flask, mix and dilute to volume.
Fehling's Solution—Two reagents are separately prepared and mixed in
equal volumes just prior to use:
Fehling's A—Dissolve 34.639 g of C.P. copper sulphate (CuS0 4 .5H,0)
in a 500 ml flask and dilute to volume. Filter through prepared asbestos.
Fehling's B—Dissolve 173 g of Rochelle salt (sodium-potassium tartrate)
in about 250 ml of water, mix with 100 ml of solution containing 50 g of
sodium hydroxide, in a 500 ml volumetric flask. Allow to stand for two days.
Dilute to volume and filter through prepared asbestos.
Standard Invert Sugar Solution—Weigh out 9.500 g of A.R. sucrose and
wash with approximately 100 ml of distilled water into a one litre volumetric
flask. Dissolve by gently swirling the flask.
Transfer 5.0 ml of concentrated hydrochloric acid into the volumetric
flask. Stopper with a cotton wool plug. Allow the flask and contents to stand
at room temperature from three to seven days, according to the prevailing
temperature.
In a separate operation, determine the volume of a prepared sodium
hydroxide solution required to adjust 5.0 ml of concentrated hydrochloric-
acid to 3.0 pH. Use methyl orange as an indicator. Add the determined
quantity of sodium hydroxide to the semi-prepared invert solution.
Dissolve 2.0 g of benzoic acid in a beaker. Gentle heating may be used.
Add the benzoic acid to the invert solution, cool and carefully dilute to a
volume of one litre. The prepared invert solution now contains 1 gramme
of invert sugar per 100 ml of solution.
Standardization of Fehling' s Solution—Pipette 50.0 ml of standard invert sugar
solution into a 250 ml volumetric flask. Add one drop of phenolphthalein
indicator and carefully neutralize with 5 N sodium hydroxide solution.
Dilute to volume with distilled water. Rinse and fill an offset burette with
this solution.
Pipette 5.0 ml of each of the Fehling's A and B solutions into a 200 ml
conical boiling flask. Add approximately 24.5 ml of the neutralized standard
invert. Heat to boiling and titrate in the manner described in Analytical
Methods, Chapter IX. Repeat the determination until two successive titres
agree to within 0.1 ml.
The calculated titration value is 25.64 ml. If the actual result varies by
more than 0.5 ml from this value, the strength of the Fehling's A must be
adjusted. If the actual value is within the 0.5 ml range, but different from the
calculated value of 25.64 ml, a correction factor must be calculated and
applied to all determinations involving that batch of Fehling's solution.
Standard Acids and Alkalis

Sulphuric Acid 1.00 Normal (0.5 M)—Cautiously add 28 ml of concen-
trated sulphuric acid (Sp.Gr. 1.84) via a measuring cylinder to approximately
900 ml of distilled water. Cool, transfer to a one litre volumetric flask and
dilute to volume.
Standardize as follows: Transfer 1.0599 g of predried A.R. sodium
carbonate to a 300 ml Erlenmeyer flask. Add 100 ml of distilled water, dis-
solve and add 2 drops of methyl orange indicator. Titrate against the un-
standardized acid. The titration should require exactly 20.0 ml of 1.00 N
sulphuric acid. Adjust the strength of the solution until this is obtained.
Hydrochloric Acid 0.20 Normal (0.2 M)—Measure out 18 ml of concen-
trated hydrochloric acid (Sp.Gr. 1.18). Pour this into approximately 500 ml of
water and then dilute to a volume of one litre in a measuring cylinder. Agitate
to obtain thorough mixing.
Standardize as follows: Weigh accurately two portions, each between
0.240 and 0.280 g, of pre-dried A.R. sodium carbonate. Carefully transfer
each to wide necked 250 ml conical flasks containing about 50 ml of distilled
water. Swirl gently until dissolved. Add 3 drops of methyl orange indicator
and titrate against the unstandardized acid until the colour changes from
yellow to orange.
If V ml of acid are used for titrating W g of sodium carbonate, then
W
Strength of acid (factor) F =
° 0.010b x V
From the two portions of sodium carbonate originally weighed out, two
independent factors will be obtained. These should be in close agreement
before the mean value of F is accepted.
Adjustment—Note the volume of 0.2 N acid left in the one litre measuring
cylinder (V ml). Add Y(F — 1) ml of water to it, mix well and repeat the
standardization. The final factor (F) should be 1.00+0.005.
Sodium Hydroxide, 0.20 Normal (0.2 M).—The water used for the prepa-
ration of this reagent must be free from dissolved carbon dioxide. If in doubt,
boil the water just before use and cool to room temperature in a sealed vessel.
Prepare a stock solution of sodium hydroxide by dissolving 53 g of the
chemical in 50 ml of distilled water. Store in a polythene bottle for three days.
Decant off 12 ml of the stock solution and transfer to a one litre meas-
uring cylinder. Dilute to volume and thoroughly mix. The solution is then
standardized as follows: Pipette 25.0 ml of the diluted solution into a 250 ml
conical flask and add 3 drops of methyl orange indicator. Titrate with 0.2 N
hydrochloric acid until the colour changes from yellow to orange. Repeat the
standardization. If V ml of acid (mean of the two determinations) are re-
quired, then
Adjustment—Note the volume of 0.2 N sodium hydroxide left in the litre

measuring cylinder (V ml). Add V(F — 1) ml of water to it, mix well and
repeat the standardization. The final factor (F) should be 1.00^0.005.
Sodium Carbonate 1.00 Normal (0.5 M)—The water for the preparation
of this reagent must be free from dissolved carbon dioxide. If in doubt, boil
the water just before use and cool to room temperature in a sealed vessel.
W e i g h o u t 2.650 g o f a n h y d r o u s s o d i u m c a r b o n a t e a n d d i s s o l v e i n
a p p r o x i m a t e l y 50 ml of w a t e r . Transfer t h e solution to a 500 ml v o l u m e t r i c
f l a s k a n d d i l u t e t o v o l u m e . M i x well a n d s t o r e i n a g r o u n d glass s t o p p e r e d
bottle.
Starch Analysis—Sugar
Calcium Chloride Dihydrate Solution—To 5 3 0 g of U n i v a r c a l c i u m c h l o r -
i d e d i h y d r a t e , a d d 4 7 0 g o f d i s t i l l e d w a t e r . A d j u s t t o 8.2 p H w i t h 1 N s o d i u m
h y d r o x i d e . S t o r e in a s e a l e d c o n t a i n e r .
Acetic Acid 1 N . — D i l u t e 57 ml of g l a c i a l a c e t i c a c i d to a v o l u m e of
one litre.
Calcium Chloride—Acetic Acid Reagent—Add 11 ml of 1 N a c e t i c a c i d
to one litre of calcium chloride d i h y d r a t e solution.
Potassium Iodate Solution 0.01 N . — W e i g h a c c u r a t e l y 0.3566 g of A . R .
p o t a s s i u m i o d a t e a n d d i s s o l v e i n a l i t r e v o l u m e t r i c flask. D i l u t e t o v o l u m e
a n d p o u r into a b r o w n glass s t o p p e r e d bottle. Store in a d a r k c u p b o a r d .
Concentrated Potassium Iodide—10% W/V—Dissolve 10 g of A . R . p o t a s -
s i u m i o d i d e in a 100 ml v o l u m e t r i c flask. S t o r e in a p l a c e a w a y f r o m l i g h t in a
b r o w n glass s t o p p e r e d b o t t l e . T h i s r e a g e n t m u s t b e d i s c a r d e d w h e n t h e s o l u -
tion becomes yellow.
Potassium Iodide—Iodate Reagent—This r e a g e n t m u s t be p r e p a r e d on
t h e d a y it is to be used. To one p a r t of concentrated potassium iodide 10 per
cent solution a d d 9 p a r t s of distilled w a t e r a n d m i x . To this solution a d d an
e q u a l v o l u m e o f 0.01 N p o t a s s i u m i o d a t e r e a g e n t . M i x a n d s t o r e i n a b r o w n
s t o p p e r e d b o t t l e for n o l o n g e r t h a n o n e d a y .
Standard Starch Solution—Determine t h e m o i s t u r e c o n t e n t of t h e s t a r c h
b y d r y i n g 2 g a t 105 ° C for t w o h o u r s ; d i s c a r d t h i s p o r t i o n . W e i g h i n t o a 3 0
ml b e a k e r t h e q u a n t i t y of u n d r i e d s t a r c h equivalent to a d r y weight of 0.400
g. A d d 500 ml of distilled w a t e r i n t o a conical flask a n d boil gently. A d d 5 ml
o f cold d i s t i l l e d w a t e r t o t h e w e i g h e d q u a n t i t y o f s t a r c h a n d m i x t o a t h i n
slurry consistency. Transfer to t h e boiling w a t e r as r a p i d l y as possible.
R e m o v e a n y residual s t a r c h from t h e beaker w i t h additional 5 ml aliquots of
c o l d w a t e r . B o i l t h e s o l u t i o n for t h r e e m i n u t e s . T i m i n g s h o u l d c o m m e n c e
f r o m t h e first a d d i t i o n o f s t a r c h t o t h e b o i l i n g f l a s k . T r a n s f e r t h e h o t s o l u t i o n
q u a n t i t a t i v e l y , via a funnel, to a one litre volumetric flask, which h a s pre-
viously been rinsed with h o t water. By w a y of t h e original 30 ml beaker,
wash t h e boiling flask w i t h h o t distilled w a t e r a n d transfer to t h e volumetric
flask. Continue this operation until the total volume in the flask is approxi-
m a t e l y 9 0 0 m l . M i x , cool i n r u n n i n g w a t e r a n d d i l u t e t o v o l u m e . S t o r e u n d e r
r e f r i g e r a t i o n . T h i s s o l u t i o n s h o u l d k e e p for o n e w e e k .
Sucrose Analysis
Jackson and Gillis Hydrochloric Acid Solution—Dilute c h e m i c a l l y p u r e
h y d r o c h l o r i c a c i d to a specific g r a v i t y of 1.1029. T h i s is e q u i v a l e n t to 2 4 . 8 5
B r i x a t 2 0 °C.
Jackson and Gillis Sodium Chloride Solution—Dissolve 2 3 1 . 5 g of c h e m i c -
a l l y p u r e s o d i u m c h l o i i d e i n distilled w a t e r . D i l u t e t o o n e l i t r e i n a v o l u m e t r i c
flask.
Sugar Detection
Alpha Naphthol—This s o l u t i o n d a r k e n s r a p i d l y o n e x p o s u r e t o l i g h t a n d
s h o u l d b e p r e p a r e d freshly e a c h w e e k . T h e s o l u t i o n i s u s e d a t a r a t e o f 5 d r o p s
per sample. On this basis the quantity required can be estimated before
alcohol and dilute to volume with ethyl alcohol.

Phenol Reagent—Dissolve 50 g of A.R. phenol in distilled water and
dilute to one litre.
N.B.—A.R. grade phenol is stipulated. If this is not available, redistillation
of other grades of phenol should be carried out before it is used.
This reagent is also used for the determination of alcohol precipitated
gums.
Water Analysis—Chlorides
Potassium Chromate Indicator—Dissolve 5.0 g of potassium chromate
(K 2 Cr0 4 ), in approximately 75 ml of distilled water. Add silver nitrate solu-
tion by drops, until a permanent brick-red precipitate is established. Cover
the container and allow to stand overnight. Filter into a 100 ml volumetric
flask and dilute to volume with distilled water.
the preparation of this reagent. It is also advisable to visually check that no

haze forms when a crystal of silver nitrate is added to a sample of this water.
Dry approximately 5 g of silver nitrate on a watch glass at 100 °C for
15 minutes. Transfer to a desiccator and cool to room temperature.
Weigh out 4.786 g of the dried chemical and transfer to a 1000 ml
volumetric flask. Dissolve and dilute to volume. Store in a dark bottle away
from light.
CHAPTER IX
ANALYTICAL METHODS
The various methods of analysis have been grouped under headings,
for ease of reference and are located as follows: —
Subject Contents Page
Brix Mill Products 95
Pol Dry Lead Method 97
Normal Weight Method 98
Herles' Method 99
Notes on Pol Determination 99
Pan Products 100
Dry Substance Sand Method 100
Josse Filter Paper Method 101
Bagasse Analysis Moisture 102
Pol 103
Cane Analysis Pol by Disintegrator Method 105
Brix by Disintegrator Method 105
Pol in Open Cells 100
Fibre 107
Sucrose-High Purity Optical Invertase Method 108
Materials Jackson and Gillis Modification No. IV 110
Sucrose-Low Purity Chemical Method 112
Materials
ReducingJSugars Dane and Eynon Method 113
Ash Gravimetric Method 115
Conductometric Method 115
Sugar Analysis Polarization 110
Moisture 119
Filtcrability 119
Grain Size 121
Starch 123
Total Colour Attenuation 124
Mud Analysis Insoluble Solids—Vacuum Filtration Method 124
Insoluble Solids—Aluminium Dish Method 125
Moisture 126
Pol 126
Fibre 126
Gums Determination of Gums in Juice 127
Phosphates Total Phosphate in Raw Sugar 128
Total Phosphate in Syrups and Clarified Juice 129
Total Phosphates in Juices 129
Soluble and Insoluble Phosphate 129
Sugar in Effluents Phenol-Sulphuric Acid Method 130
Bartholomae Method 131
Alpha-Naphthol Test 131
Quality of Mill Lime Neutralizing Value 132
Available CaO 132
Caustic Cleaning Solution Determination of Concentration 133
Laboratory SettlinglTest C.S.R. Procedure 133
Cyclone S a m p l i n g and Pressure Filtering Device 135
Supersaturation Theory of Supersaturation 136
Saturation Cell 137
Boiler Water Analysis Alkalinity 139
Phosphate 140
Sulphite 141
Hardness 141
Total Dissolved Solids 142
Sulphate 142
Water Analysis Chlorides 143
ANALYTICAL METHODS 95
T h e p r e v i o u s E d i t i o n listed t h e v a r i o u s a n a l y s e s w h i c h w o u l d b e r e q u i r e d
for e a c h p r o d u c t "if a c o m p l e t e c h e m i c a l c o n t r o l on all f a c t o r y o p e r a t i o n s
were to be obtained . . . " The advances of the last decade in m a t t e r s pertain-
ing t o f a c t o r y efficiency a n d s u g a r q u a l i t y h a v e h o w e v e r , r e s u l t e d i n t h e
i n t r o d u c t i o n o f m a n y n e w m e t h o d s o f a n a l y s i s t o o u r I n d u s t r y . A s far a s
possible t h e l a t e s t m e t h o d s o f a n a l y s i s h a v e b e e n i n c l u d e d i n t h i s c h a p t e r .
I t i s r e a l i z e d t h a t local c o n d i t i o n s m a y n e c e s s i t a t e s m a l l d e v i a t i o n s f r o m
r e c o m m e n d e d m e t h o d s , a n d t h a t t h e f r e q u e n c y w i t h w h i c h a n a l y s e s for
r o u t i n e c o n t r o l p u r p o s e s a r e c a r r i e d o u t i s a q u e s t i o n w h i c h s h o u l d b e left
to t h e d i s c r e t i o n of t h e c h e m i s t in c h a r g e of e a c h f a c t o r y . A f a c t o r for c o n -
sideration in this regard however, is t h a t while t h e frequent analysis of certain
p r o d u c t s i s e s s e n t i a l for b o t h r o u t i n e c o n t r o l a n d r e c o r d k e e p i n g p u r p o s e s ,
the practical value of each analysis should be considered and the general
l a b o r a t o r y routine reviewed from t i m e to time. If procedures are not reviewed,
t h e s i t u a t i o n c a n arise w h e r e a l a r g e n u m b e r o f a n a l y t i c a l d a t a i s c o m p i l e d
on samples which m a y b e a r little or no relationship to t h e actual material in
p r o c e s s . T h e m o r e p r a c t i c a l s y s t e m i s o n e w h i c h p e r m i t s sufficient a n a l y s e s
for b a s i c c o n t r o l , a n d w h i c h still l e a v e s s o m e t i m e for t h e a n a l y s t s t o s t u d y
various aspects of the process which m a y w a r r a n t investigation.
T h e f o r m o f p r e s e n t a t i o n h a s b e e n r e v i e w e d w h e r e v e r possible i n t h i s
C h a p t e r i n a n e n d e a v o u r t o assist b o t h t h e a n a l y s t a n d t h e s t u d e n t t o o b t a i n
a brief r e s u m e of t h e g e n e r a l p r i n c i p l e s of e a c h m e t h o d , m e r e l y by reference
t o t h e a p p r o p r i a t e s u b - h e a d i n g s . S o m e m e t h o d s h a v e b e e n c o n d e n s e d for
sake of brevity, a n d although t h e essential details and procedures h a v e been
r e t a i n e d , a n a l y s t s e n t i r e l y u n f a m i l i a r w i t h a specific a n a l y s i s a r e a d v i s e d t o
resort to original publications to obtain a m o r e comprehensive b a c k g r o u n d
of t h e fundamentals of t h e particular m e t h o d .
A d d i t i o n s t o t h i s C h a p t e r since t h e F o u r t h E d i t i o n h a v e b e e n o b t a i n e d
f r o m t h e Colonial S u g a r R e f i n i n g C o m p a n y L i m i t e d , t h e S u g a r R e s e a r c h
I n s t i t u t e and various other sources. Their permission to publish these
m e t h o d s is g r a t e f u l l y a c k n o w l e d g e d . T h e l i b e r a l u s e of t h e 1964 E d i t i o n of
the ICUMSA Methods of Sugar Analysis, and the R e p o r t of the Proceedings
of t h e F o u r t e e n t h Session of I C U M S A 1966, as reference s t a n d a r d s is also
acknowledged.
Brix
T h e m e t h o d of Brix determination is dependent u p o n the t y p e of analysis
to be performed. T h e majority of Brix determinations are usually carried out
b y m e a n s o f a B r i x h y d r o m e t e r , b u t i n d i r e c t c a n e a n a l y s i s , for e x a m p l e ,
B r i x i s d e t e r m i n e d b y precision r e f r a c t o m e t e r , o r b y p y c n o m e t e r .
Brix by Hydrometer
M a n y s a m p l e s s u c h a s juice, m a c e r a t i o n f l u i d a n d s y r u p a r e sufficiently
l o w in v i s c o s i t y for a d i r e c t h y d r o m e t e r d e t e r m i n a t i o n to be c a r r i e d o u t .
Samples of relatively high viscosity, such as massecuites a n d molasses, re-
q u i r e p r i o r d i l u t i o n w i t h w a t e r i n a k n o w n w r eight t o w e i g h t r a t i o . F o r
p u r p o s e s of u n i f o r m i t y t h e s t a n d a r d d e g r e e of d i l u t i o n in Q u e e n s l a n d is o n e
p a r t of w a t e r to o n e p a r t of s a m p l e i.e. a 1:1 d i l u t i o n , a n d t h i s is a c c o m p l i s h e d
as follows:—
T a r e a c o n t a i n e r of a c a p a c i t y in excess of o n e l i t r e on a s u i t a b l e b a l a n c e .
Mix t h e s a m p l e a n d a d d 5 0 0 . 0 g t o t h e t a r e d c o n t a i n e r . A d d a p p r o x i m a t e l y
300 m l o f h o t w a t e r a n d s t i r u n t i l d i s s o l u t i o n i s c o m p l e t e . Cool a n d f u r t h e r
d i l u t e t h e c o n t e n t s w i t h cold w a t e r t o a t o t a l w e i g h t o f 1000.0 g . T h o r o u g h l y
96 ANALYTICAL METHODS
m i x t h e solution. W h e n t h e Brix reading is finally taken, t h e reading of t h e

d i l u t e d s a m p l e m u s t b e c o r r e c t e d for t e m p e r a t u r e . T h i s t e m p e r a t u r e -
corrected Brix is then multiplied by a factor of t w o to o b t a i n t h e Brix of
t h e original sample.
Preparation—The p r o c e d u r e defined in R e g u l a t i o n 57 of t h e S u g a r C a n e
P r i c e s A c t for t h e d e t e r m i n a t i o n o f B r i x for c a n e p a y m e n t p u r p o s e s a p p l i e s
i n p r i n c i p l e t o all B r i x d e t e r m i n a t i o n s b y h y d r o m e t e r , n a m e l y : —
"A brixing cylinder, d r y or well-drained, is set up and, w i t h o u t stirring,
sufficient o f t h e s a m p l e j u i c e i s p o u r e d i n t o f i l l t h e c y l i n d e r . I f a n y a p p r e c i a b l e
q u a n t i t y o f b a g a s s e , t r a s h , o r o t h e r foreign m a t t e r i s s u s p e n d e d i n t h e j u i c e ,
the juice should be d e c a n t e d t h r o u g h a strainer into the cylinder.
T h e c y l i n d e r a n d c o n t e n t s a r e a l l o w e d t o r e m a i n u n d i s t u r b e d for 2 0
m i n u t e s o r t h e c o n t e n t s m a y b e p l a c e d u n d e r a p r e s s u r e n o t e x c e e d i n g 1 0 in.
H g a b s . for a p e r i o d o f 5 m i n u t e s . I n t h e l a t t e r case t h e j u i c e m u s t b e a l l o w e d
t o s t a n d u n t i l a t least 2 0 m i n u t e s h a v e e l a p s e d since t h e j u i c e w a s l a s t
stirred . . . "
Three i m p o r t a n t facets of t h e d e t e r m i n a t i o n are as follows:—
Temperature—The t e m p e r a t u r e of t h e s o l u t i o n m u s t be a p p r o x i m a t e l y
t h a t o f t h e s u r r o u n d i n g s . I f i t i s t o o h i g h , t h e s o l u t i o n m u s t b e cooled, a n d
c a r e s h o u l d b e t a k e n t o e n s u r e t h a t t h e e n t i r e s a m p l e i s cooled u n i f o r m l y .
Preferably t h e c o n t e n t s of t h e cylinder should be t h o r o u g h l y m i x e d after
cooling.
Suspended Matter—Coarse p a r t i c l e s in t h e s a m p l e a r e r e m o v e d by s t r a i n -
ing through a fine mesh gauze as the sample is being poured into t h e cylinder.
T h e h e a v y p a r t i c l e s o f s m a l l e r size t h a t p a s s t h r o u g h t h e s t r a i n e r will u s u a l l y
settle in the b o t t o m of the cylinder during the obligatory 20 m i n u t e s standing
p e r i o d . S o m e p a r t i c l e s h o w e v e r will still r e m a i n i n s u s p e n s i o n . T h e s e c a n
h a v e a significant effect o n t h e h y d r o m e t e r r e a d i n g a n d s h o u l d b e r e m o v e d
b y e i t h e r f i l t r a t i o n o r c e n t r i f u g i n g i f precise r e s u l t s a r e r e q u i r e d .
Air Bubbles—Samples of b o t h low a n d h i g h B r i x fluids f r e q u e n t l y c o n t a i n
a c o n s i d e r a b l e q u a n t i t y of air b u b b l e s at t h e t i m e of s a m p l i n g . F u r t h e r air
c a n also b e e n t r a p p e d i n t h e p r o c e s s o f p o u r i n g t h e l i q u i d i n t o t h e c y l i n d e r .
R e m o v a l of t h i s air is a c c o m p l i s h e d e i t h e r by t h e a p p l i c a t i o n of v a c u u m or
b y a l l o w i n g t h e s a m p l e t o s t a n d for 2 0 m i n u t e s a s s e t o u t i n t h e R e g u l a t i o n .
Procedure—The c l e a n e d , d r i e d h y d r o m e t e r s h o u l d b e l o w e r e d i n t o t h e c y l i n -
der, c a u s i n g t h e l i q u i d t o overflow a n d c a r r y a w a y w i t h i t a n y f r o t h floating
o n t h e surface. T h e h y d r o m e t e r i s l o w e r e d u n t i l i t f l o a t s freely, a n d c a r e
s h o u l d be t a k e n to see t h a t t h e s t e m is w e t t e d for o n l y a few t e n t h s of a u n i t
above the point at which the h y d r o m e t e r comes to rest. If in the above
o p e r a t i o n t h e h y d r o m e t e r s t e m is w e t t e d m o r e t h a n a few t e n t h s of a u n i t
a b o v e t h e m e n i s c u s , t h e r e a d i n g s h o u l d b e n o t e d , t h e h y d r o m e t e r lifted, a n d
t h e emergent portion of t h e s t e m wiped dry. T h e h y d r o m e t e r is t h e n carefully
lowered to the reading first observed.
I f t h e r e i s a n y a p p r e c i a b l e difference i n t e m p e r a t u r e b e t w e e n t h e s o l u t i o n
a n d t h e h y d r o m e t e r , t h e l a t t e r s h o u l d b e a l l o w e d t o f l o a t freely u n t i l t e m p e r -
ature equilibrium is established.
I f t h e s o l u t i o n i s clear a n d l i g h t c o l o u r e d t h e p o i n t a t w h i c h t h e p l a n e
o f t h e l i q u i d s u r f a c e w o u l d i n t e r s e c t t h e scale i s r e a d i l y o b s e r v e d . F r e q u e n t l y
t h e r e a d i n g o f t h e u p p e r edge o f t h e m e n i s c u s m u s t b e t a k e n a n d a c o r r e c t i o n
a p p l i e d . F o r t h e class o f h y d r o m e t e r g e n e r a l l y u s e d i n Q u e e n s l a n d t h e m e n i s -
c u s c o r r e c t i o n i s close t o + 0 . 1 5 ° B r i x , s o t h a t i f r e a d i n g s a r e t o b e m a d e t o
t h e n e a r e s t 0.1° i t i s justifiable t o a d d e i t h e r 0.1° o r 0.2° a c c o r d i n g t o t h e
r e a d i n g a t t h e t o p o f t h e m e n i s c u s . W h e n e v e r possible a n effort s h o u l d b e
m a d e to estimate the t r u e point at which t h e surface plane would intersect
t h e scale. T h i s e l i m i n a t e s a n y d o u b t s a s t o w h e t h e r t h e m e n i s c u s c o r r e c t i o n
s h o u l d b e 0.1 o r 0.2. I n a n y case, t h e r e a d i n g a t t h e t o p o f t h e m e n i s c u s s h o u l d
n e v e r b e s e t d o w n a s a r e s u l t , b u t s h o u l d b e c o r r e c t e d m e n t a l l y before b e i n g
entered on the records as observed Brix.
The t e m p e r a t u r e of the solution should be determined immediately t h e
hydrometer reading has been m a d e a n d t h e necessary correction applied to
give t h e t r u e B r i x v a l u e . E x a m p l e : —
Significance of the Brix Determination—The d e t e r m i n a t i o n of B r i x as a s e p a -

r a t e entity can be of i m p o r t a n c e in measuring such factors as Brix of masse-
c u i t e , B r i x o f m a c e r a t i o n fluid e t c . B r i x m e a s u r e m e n t h o w e v e r , i s n o r m a l l y
associated with t h e determination of pol in order to obtain a measure of t h e
q u a n t i t y of i m p u r i t i e s p r e s e n t in a s o l u t i o n . In t h i s r e g a r d , t h e a s s o c i a t i o n of
a Brix test with the determination of pol by the d r y lead m e t h o d has a dual
purpose. The Brix of the solution is obtained, and, in addition, the Brix
r e a d i n g is u s e d to give a m e a s u r e of t h e d e n s i t y of t h e s o l u t i o n , a n d h e n c e t h e
w e i g h t of 100 ml of t h e s o l u t i o n in air.
A B r i x h y d r o m e t e r is, of c o u r s e , c a l i b r a t e d in d e g r e e s B r i x , b u t e v e r y
graduation corresponds to a particular density. W h e n a h y d r o m e t e r calibrated
at 20 °C i m m e r s e d in a l i q u i d at 20 °C r e a d s , for e x a m p l e , 25.0 ° B r i x , it is
e s t a b l i s h e d t h a t t h e d e n s i t y of t h e s o l u t i o n is 1.103557 g p e r m l . If t h e
h y d r o m e t e r itself w e r e n o t affected b y t e m p e r a t u r e , t h e n i r r e s p e c t i v e o f t h e
t e m p e r a t u r e of t h e s o l u t i o n , a r e a d i n g of 25.0° w o u l d i n d i c a t e a d e n s i t y of
1.103557 g p e r m l . In a c t u a l fact, t h e h y d r o m e t e r itself is affected v e r y l i t t l e
by t e m p e r a t u r e ; the substantial t e m p e r a t u r e corrections which are applied
t o o b s e r v e d B r i x r e a d i n g s (for t e m p e r a t u r e s o t h e r t h a n 2 0 °C), a r e d u e a l m o s t
e n t i r e l y t o t h e effect o f t e m p e r a t u r e o n t h e s u g a r s o l u t i o n a n d , for p r a c t i c a l
p u r p o s e s , t h e t e m p e r a t u r e coefficient of v o l u m e of t h e h y d r o m e t e r is i g n o r e d ,
a n d a r e a d i n g at t °C is t a k e n as an i n d e x of t h e d e n s i t y of t h e s o l u t i o n
a t t °C.
Pol
T h r e e m e t h o d s for t h e d e t e r m i n a t i o n o f p o l i n j u i c e s a n d s i m i l a r l i q u i d s
c o n t a i n i n g u p t o 2 5 p e r c e n t s u c r o s e a r e listed i n t h i s E d i t i o n . I n t h e first
m e t h o d a n d o n e version o f t h e t h i r d m e t h o d , t h e B r i x o f t h e s a m p l e m u s t
also b e d e t e r m i n e d .
The u s e o f t h e d r y l e a d m e t h o d i s o b l i g a t o r y for f i r s t e x p r e s s e d j u i c e
analyses for c a n e p a y m e n t p u r p o s e s . O n l y i f u n s a t i s f a c t o r y clarification i s
obtained b y the d r y lead m e t h o d m a y the other m e t h o d s b e used.
The specification o f l e a d a c e t a t e p u r i t y a n d t h e p r e p a r a t i o n o f H e r l e s '
reagents are listed in C h a p t e r V I I I .
Dry Lead Method

In order to obtain t h e pol per cent of a solution, a s e p a r a t e Brix deter-
m i n a t i o n is required with this m e t h o d . In t h e procedure outlined below,
attention is d r a w n to t w o aspects, the addition of lead acetate powder a n d
t h e choice o f c o n t a i n e r . T h e q u a n t i t y o f l e a d a c e t a t e a d d e d s h o u l d b e j u s t
sufficient to achieve satisfactory clarification, and overleading must be

avoided.
The most suitable container for this determination is a flat-bottom
conical flask of approximately 150 ml capacity, with a neck opening just wide
enough to permit easy addition of the lead powder, but narrow enough to be
easily stoppered for the purpose of shaking the contents.
Procedure—Transfer approximately 100 ml of juice to a flask. Add 1 g
of dry lead acetate, stopper and shake vigorously. Allow a reaction time of
several minutes. A further mixing of the contents at this stage is re-
commended.
Filter. Add the juice to a maximum safe level and cover the top of the
filter to minimize evaporation. Discard the first 10 ml of filtrate, and read the
optical rotation of the solution in a 200 mm tube.
Calculation—This is simplified by the use of Schmitz's Table for undiluted
solutions (Table II), which has been derived from the formula—
The table is used in the following manner:—

Suppose the uncorrected Brix = 18.1 (without temperature correction)
and the polariscope reading = 60.5 CS. Under the column headed 18 (the
closest approximation provided) and opposite 60 (the whole number of the
polariscope reading), the value of 14.57 is found. Add to this the amount of
0.12 (equivalent to 0.5 pol reading found in the inset table for tenths of a
degree pol reading). The pol of juice then = 14.57 + 0.12 = 14.69.
If it is desired to work out results for cases not shown in Schmitz's
Tables, the pol may be derived from the formula—
Values of apparent density at 20 °C for corresponding Brix values are avail-

able from Table XV.
Normal Weight Method
This method is not recommended for general use, but it occasionally has
some application where, for example, the pol per cent of a juice is required
without an accompanying Brix determination.
Unlike the previous method, the normal weight method is affected by
the presence of insoluble matter in the juice, and also by the volume of
precipitate formed when wet lead clarification is used.
Procedure—Transfer three normal weights of juice (78.00 g) to a 100 ml
volumetric flask. Wash in any residual juice with a small quantity of distilled
water.
Addition of Lead Acetate—Two alternatives are available:
A. Dry Lead—Dilute the flask contents to 100 ml with distilled water
and then add approximately 0.8 g of dry lead acetate.
Shake thoroughly, allow to stand and filter as in the previous method.
Read in a 200 mm tube.
B. Wet Lead—Add 2 ml of wet lead solution and then dilute to the
100 ml mark. Shake, allow to stand and filter. Read in a 200 mm tube.
Herles' Method
This method has been found to be of considerable benefit for clarifying
juices that will not respond satisfactorily to lead acetate addition.
Two variations of the method are presented:
A. Gravimetric Method—
Procedure—Weigh out 2 normal weights of juice into a 100 ml volumetric
flask.
Add 5 ml of reagent B, followed by 5 ml of reagent A. (Chapter V I I I :
Herles' reagents). Add distilled water short of the mark and mix well by
swirling. Dilute to 100 ml.
Mix, filter and polarize in a 200 mm tube.
B. Volumetric Method—A separate Brix measurement is required in

this case.
Procedure—Add 50 ml of juice into a 100 ml volumetric flask. Proceed as
above to the stage where a polariscope reading is obtained.
Calculation—Multiply polariscope reading by 2.
Refer to Schmitz's table (Table II) and derive pol per cent juice from
the undiluted polariscope reading and the uncorrected Brix of the sample.
Notes on Pol Determination
Of the three methods described, the dry lead method is preferred and
is used almost exclusively throughout the Industry. The notable exception
to this is when juices from canes in an advanced stage of deterioration are
encountered. In this instance, Herles' method will generally prove to be the
most effective.
The formula on which Schmitz's Table is based, namely—
should theoretically be applied only when solutions are analysed at 20 °C.

At temperatures other than 20 °C however, the influences of polariscope and
tube coefficients are very minor items in practice, and the formula is used as
if it were independent of temperature, with the one qualification that the
polariscope reading and Brix determination are carried out at the same
temperature.
However, while the use of the observed Brix compensates adequately for
the changes in density of undiluted juice at different temperatures, the effects
of temperature on the optical rotation of sucrose, reducing sugars, etc., must
also be considered. Sucrose solutions display a rotation which decreases with
temperature. Invert sugar solutions display a much higher change of rotation
in the reverse direction. When the reducing sugars (considered as invert sugar)
constitute 6f per cent of the sucrose, the temperature coefficient of the
mixture vanishes.
An empirical formula suggested for the correction of the observed polar-
ization of juices as read in a quartz wedge compensated saccharimeter is
N o t e t h a t w h e n t h e p o l a r i s c o p e r e a d i n g i s 80, t h e c o r r e c t i o n i s z e r o . T h e
polariscope readings of undiluted juices a p p r o x i m a t e to 80 so t h a t , according
t o t h i s f o r m u l a , t h e o m i s s i o n o f a t e m p e r a t u r e c o r r e c t i o n i s justified. H o w e v e r ,
i n d i v i d u a l s a m p l e s o f j u i c e s h a v e b e e n f o u n d t o d i s p l a y significant t e m p e r -
a t u r e coefficients a n d t h e p r a c t i c e o f c o n d u c t i n g j u i c e a n a l y s e s a t o r n e a r
20 °C is r e c o m m e n d e d .
T h e d e t e r m i n a t i o n of t h e pol of o t h e r m a t e r i a l s is best discussed in
r e l a t i o n t o specific p r o d u c t s a s follows:—•
Pan Products *
For the determination of pol in p a n products, b o t h t h e concentration of
s o l u t i o n a n d t h e a m o u n t o f clarifying a g e n t m u s t b e v a r i e d t o s u i t t h e n a t u r e
o f t h e p r o d u c t . F o r p u r p o s e s o f u n i f o r m i t y , t h e following d i l u t i o n s a n d
a m o u n t s o f d r y l e a d a r e s u g g e s t e d . T h e s e s h o u l d b e a d e q u a t e for t h e m a j o r i t y
of s a m p l e s e n c o u n t e r e d in e a c h c a t e g o r y .
Product Aliquot Weight of

Dry Lead
Syrup 1 normal weight of straight syrup/100 ml

A and B Massecuite 1 normal weight of 1:1 dilution/100 nil 1 g
A and B Molasses 1 normal weight of 1:1 dilution/100 ml 3 g
Magma 1 normal weight of 1:1 dilution/100 ml 2 g
C Massecuite 2 normal weights of 1:1 dilution/300 ml 5 g
Final Molasses 2 normal weights of 1:1 dilution/300 ml 8 g
T h e effects of o v e r l e a d i n g a r e m o r e p r o n o u n c e d in C m a s s e c u i t e a n d
final m o l a s s e s a n a l y s e s a n d a c o n s i d e r a b l e inflation of t h e p o l r e a d i n g s c a n
r e s u l t . F o r C m a s s e c u i t e a n d final m o l a s s e s a n a d d i t i o n a l s t e p s h o u l d b e
e m p l o y e d in t h e d e t e r m i n a t i o n as follows: —
After n o r m a l l e a d i n g a n d f i l t r a t i o n , a d d 5 0 m l o f t h e f i l t r a t e t o a 50-55 m l
v o l u m e t r i c flask. T h e n a d d 2 ml of 1 + 4 a c e t i c a c i d r e a g e n t a n d d i l u t e to
5 5 m l w i t h distilled w a t e r . Mix t h o r o u g h l y a n d p o l a r i z e i n a 200 m m t u b e .
T h e c a l c u l a t i o n for t w o n o r m a l w e i g h t s i n 300 m l o f 1:1 d i l u t e d s a m p l e
a n d filtrate d i l u t i o n f r o m 5 0 t o 5 5 m l t h e n b e c o m e s
P o l p e r c e n t = p o l r e a d i n g X 3.3
This additional step is necessary due to the relatively high concentration
of laevulose in these products. Lead in solution combines with laevulose to
give a s o l u b l e c o m p o u n d o f l o w o p t i c a l r o t a t i o n . A c e t i c a c i d s p l i t s u p t h i s
compound, thereby restoring t h e rotation of t h e laevulose.
Dry Substance
T h r e e m e t h o d s a r e a v a i l a b l e for t h e d e t e r m i n a t i o n o f d r y s u b s t a n c e b y
drying under controlled conditions, t h e Sand m e t h o d , t h e T a t e and Lyle
V a c u u m O v e n M e t h o d , (De W h a l l e y 1964), a n d t h e J o s s e F i l t e r P a p e r m e t h o d .
Of the three, t h e Josse Filter Paper m e t h o d w i t h v a c u u m drying is considered
t o b e t h e m o s t s u i t a b l e for Q u e e n s l a n d c o n d i t i o n s . T h e S a n d m e t h o d i s still
used b y some factories, b u t its replacement b y t h e Josse Filter P a p e r m e t h o d
is recommended.
Sand Method
Sand Preparation—A s u p p l y of fine p r e p a r e d s a n d is r e q u i r e d . T h e r e -
c o m m e n d e d m e t h o d of preparation is as follows:—
Use only sand that will pass through a 40 mesh and be retained on a 60
mesh screen. Digest the sand in hot hydrochloric acid, and then wash in
running water until the tailings will not give a positive reaction with silver
nitrate. Oven dry and then ignite in a muffle furnace at a temperature in
excess of 600 °C.
Special Apparatus—Flat bottomed aluminium dishes, approximately
three inches in diameter with 3/4 inch vertical walls and close fitting lids, are
used for the determination. A glass stirring rod of such a length that it will
just fit inside the dish on a slope is also required.
Procedure—Pre-dry approximately 50 g of sand in the aluminium dish.
Allow to cool in a desiccator just prior to use. Weigh dish plus sand and stirrer.
Add a known weight of sample. This varies from 10 g for juices to 6 to 10 g
of 1:1 dilution for massecuites and molasses. Mix sand and sample thoroughly
with the glass stirring rod. Great care must be taken during this operation
to avoid any loss of sand.
Dry, either in a hot air oven at 103-105 °C for four hours, or preferably,
under a vacuum of 28 inches Hg at 70 °C until successive weighings at two
hourly intervals do not differ by more than 0.5 mg. This usually takes about
16 hours. The air bleed into the oven should be fitted with a double calcium
chloride drying tower. After completion of drying, replace the lid and allow
to cool to room temperature in a desiccator. Complete the final weighing with
a minimum of delay. Calculate the weight of dry solids and express as a
percentage of the weight of the original undiluted sample.
Josse Filter Paper Method

The determination of dry substance by this or any other drying method
can be subject to errors from various sources, unless analytical procedure,
drying conditions and timing between operations are rigidly controlled.
Two of the main sources of error in this regard are evaporation effects be-
tween addition and weighing of sample, and re-absorption after drying.
Special Apparatus—Glass weighing bottles approximately 3 cm diameter
and 7 cm in height with ground glass stoppers are required. Strips of filter
paper 60 x 4.5 cm are rolled in loose coils and placed inside the bottles.
Procedure—Pre-dry the bottle and paper in a vacuum oven at 63 °C for
a minimum of 6 hours. Stopper immediately after removal from the oven and
cool in a desiccator for 20 minutes. Weigh the sealed bottle plus paper. The
sample, undiluted in the case of juices, or diluted 1:1 in the case of massecuites
or molasses, is then added in the following manner.
Remove the paper, introduce approximately 2 g of sample and weigh.
Then add 1 ml of distilled water, mix by swirling, insert the paper coil and
allow to stand for 30 minutes before commencement of drying.
The sample is then dried at 63 °C for 16 hours under a vacuum of from
26 to 29 inches Hg. A slight bleed of air, which is dried in double calcium
chloride towers, is allowed to pass into the oven during the drying period.
At the end of the drying period the vacuum is released slowly, the air entering
through the drying towers. The bottles are then closed and cooled in a
desiccator for 20 minutes before weighing. The weight of dry solids is calcu-
lated and expressed as a percentage of the weight of the original undiluted
material.
Bagasse Analysis
Preparation of Sample
The method of collecting and compositing bagasse has been described
in Chapter VII. The sub-sampling of a large quantity of bagasse is facilitated
by hammer-milling, which comminutes and mixes the bagasse. This is
particularly useful for first mill bagasse where large pieces are usually present.
Drying of the sample will also be facilitated by the finer subdivision. When
hammer milling is carried out, care must be taken to avoid contamination
of the samples, and care should be exercised during any bagasse sampling to
minimize loss of moisture.
Moisture
Large capacity drying ovens based on the principle of the old Spencer
type oven are now standard equipment in most mill laboratories. Bagasse is
placed in a cylindrical container measuring approximately 11 inches by 7
inches in diameter, the base of which is covered by a layer of 22 mesh gauze

supporting a layer of 100 mesh gauze. Hot air is then passed through the
sample. When a number of drying containers are to be used continuously,
it is convenient to adjust all the containers to the same tare weight.
Procedure—Add 1000 g of bagasse sample to the container and dry at a

temperature of from 105 to 115 °C until the weight loss is less than 2 g in
30 minutes. This usually takes from three to four hours. Weighings are made
while the container is still hot.
Pol
The wet disintegrator method of pol determination has now almost
completely replaced the old hot digestion method. Several minor changes
have been made to the machine described by Foster (1955), but the same
Fig. 39—Wet-Disintegrator.
basic principle is still employed. The procedures described in this Manua are,
however, designed for use with the modified type of wet disintegrator i.e. a
machine fitted with three six inch blades at half inch intervals up the shaft,
shaft end one eighth inch from the bottom of the can, and a water-cooled
baffled can. The blades on these machines must be kept sharp.
Procedure—Weigh out 1200 g of first mill bagasse or 1000 g of bagasse
from subsequent mills. Transfer to the disintegrator can and add 10 kg of
water. Disintegrate for 30 minutes at approximately 5600 rev/min and ensure

that an adequate flow of cooling water is applied to the waterjacketed dis-
integrator can. Remove approximately 200 ml of extract for pol analysis,
strain through a 40 mesh gauze into a 250 ml conical flask, stopper and cool
to room temperature.
Clarify with a minimum amount of dry lead acetate, shake, and allow
to stand for at least five minutes. Filter, discard the first 10 to 15 ml of
filtrate and polarize in a 400 mm tube.
Calculation—It is assumed in the following formula that the specific
gravity of the extract is 1.000 and that the fibre contains 25 per cent hygro-
scopic water.
where R = pol reading of extract

W = weight of water added
B = weight of bagasse
M = moisture in total bagasse (B)
Q — purity of residual juice
neglected.
For the routine analysis of final bagasse, where a 10:1 ratio of water to
bagasse is used, a simplified formula, which neglects the influence of hygro-
scopic water, is frequently employed, and the formula reads as follows:—
where w = moisture per cent bagasse

Q = purity of residual juice.
The purity of residual juice is frequently assumed to be 70, and a table, based
on this assumption, and on the simplified formula given above, mav be found
in Table III.
Cane Analysis
The present Queensland cane payment system evaluates cane for pay-
ment purposes in terms of c.c.s. or commercial cane sugar. The c.c.s. is
calculated from the pol and Brix of cane, which are determined by means of
an empirical formula involving the pol and Brix of first expressed juice and
the fibre per cent cane.
The need for a more exact method of cane analysis has resulted in the
development of a system for direct cane analysis. In direct analysis, pol and
Brix of cane are determined by use of the wet disintegrator on a sample of
prepared cane. Moisture is also determined on the prepared cane sample and
fibre calculated using the formula: Fibre per cent cane = 100 — Brix per cent
cane — water per cent cane.
The method of sampling cane for direct analysis is described in Chapter
VII.
Sample Preparation
Thoroughly mix the sample of prepared cane. If cane preparation is
considered inadequate, the sample may be given additional preparation by
passing the cane through a hammer mill or cutter-grinder. Care must be taken
to minimize loss of moisture if comminution of the sample is carried out
and if a cutter-grinder is used, the blades must be kept sharp. Transfer the
sample to a sealed container and commence the following analyses with a
minimum of time delay.
Moisture
This is determined in the manner described for moisture per cent bagasse.
Brix and Pol
Procedure—Weigh out accurately 2000 g of prepared cane and transfer
to the water jacketed disintegrator can. Add 6000 g of water from a suitable
dispenser.
Disintegrate the material as described in the procedure for pol per cent
bagasse.
Brix of Extract—To a separate portion of extract, add approximately
2 g of filter aid per 100 ml and filter. Discard the first runnings. Take all
necessary precautions to minimize evaporation.
Determine the Brix of extract by a precision refractometer after having
previously checked the zero point of the instrument with distilled water, or
by means of a pycnometer.
Calculations (Deicke 1959)—
and y = weight of cane

x = weight of water
z = per cent hygroscopic water
w = moisture per cent cane
For 2000 g of cane, 6000 g of water and an assumed hygroscopic water
content of 25 per cent, the formula is simplified to
Pol of Extract—For dry lead clarification and polarization of the extract

in a 400 mm tube.
Pol per cent cane =
Pol in Open Cells

An estimate of the percentage of broken and unbroken cells in cane
can be obtained from the determination of pol in open cells as opposed to pol
of the total sample; The determination is seldom used for routine control
purposes, but it is of value in establishing the degree of cane preparation
obtained prior to crushing.
The basis of the method is that sugar can be rapidly leached from broken
cells under conditions which do not induce diffusion of sugar from unbroken
cells. It must also be assumed that the pol content of broken cells is the same
as the pol content of unbroken cells. The forementioned must be viewed with
some reservation and results should be considered more on a comparative
than an absolute basis.
A version of the method of Aldrich and Rayner (1962) as modified by
the Sugar Research Institute, is listed below.
Special Apparatus—A 3 gallon
bottle neck container of the type and
dimensions shown in Fig. 40 is re-
quired.
Procedure—The prepared cane
should be thoroughly mixed before
subsampling.
Pol in open cells—Weigh out
1000 g of prepared cane and transfer
into the special container. Add
10,000 g of water, seal and rotate on
a jar mill for 10 minutes at 70 rev/
min.
Determine the pol reading of
the extract in a 400 mm tube.
Pol in total sample—Transfer
2000 g of prepared cane and 6000 g
of water to a wet disintegrator and
disintegrate for 30 minutes. Deter-
mine the pol reading of the extract
in a 400 mm tube.
Pol in total sample—Transfer 2000 g of prepared cane and 6000 g of water
to a wet disintegrator and disintegrate for 30 minutes. Determine the pol
reading of the extract in a 400 mm tube.
ratio of the pols of the extracts, and if this ratio is designated r, the formula
for percentage of pol in open cells reduces to
Fibre
The direct determination of fibre for cane payment purposes is carried
out by either of the two methods described below. It should be emphasized
however that the form of presentation of these methods does not constitute
an official interpretation of the Cane Prices Regulations.
Whole Stalk Method -The use of this method has been superseded in most
factories by the prepared cane method, but whole stalk selection and analysis
is still required for certain milling and agricultural experiments.
Procedure—Sticks should be selected in a manner which will ensure that
they are a representative selection of the original parcel of cane. A group of
12 sticks constitutes a suitable unit for fibre analysis, and if the amount of
cane to be sampled cannot be adequately represented by this number, it is
preferable to take as many groups of 12 as required and to analyse each group
separately.
Sub Sampling—Lay the 12 sticks on the ground in descending order of
length and with all tops in the same direction. Cut each stalk into three equal
sections, top, middle and butt. Sections are then selected and laid out as
follows:—
Stalk Section Direction
1 Top Unchanged
2 Middle Unchanged
3 Butt Unchanged
4 Top Reversed
5 Middle Reversed
6 Butt Reversed
This sequence is repeated for the second group of six sticks.
Preparation—When the old Queensland type fibrator is employed the
12 sections are fibrated, without reversal, to the extent of half the length of
each section. The resultant fibrated material should represent two complete
stalks of cane. It is important that the fibrator should be sharp and in good
order. The fibrated material should be mixed thoroughly and quickly on a
shallow tray and a representative portion selected and placed in an airtight
container. The actual analysis is then carried out in a similar manner to that
described for the prepared cane method.
An alternative and more efficient preparatory device is the Jeffco type
cutter-grinder. When this is employed however, the full sections are fibrated.
Prepared Cane Method—The method previously described has several
limitations, the more important being that it is extremely difficult to obtain
a representative sample of cane. The lengthy procedure of stick selection and
preparation also limit the number of determinations that may be carried out
in any one period.
The need for an improved method of fibre determination resulted in the
development of a technique which permits the sampling and analysis of
prepared cane just prior to milling. A more detailed discussion of this subject
may be found in a paper by Anderson and Petersen, (1959).
Sample Preparation—A sample of prepared cane is removed from the
carrier to a table by the method as described in Chapter VII. After rapid but
thorough mixing, a sub-sample is transferred to a Waddell type hammer mill
which has previously been conditioned with a discarded portion of the sample.
Procedure—Hammer m i l l t h e c a n e for a p p r o x i m a t e l y 15 s e c o n d s a n d
again rapidly b u t thoroughly mix the prepared sample. Transfer a represent-
a t i v e s u b - s a m p l e t o a closed c o n t a i n e r . W e i g h a p r e d r i e d f i b r e b a g i n a n air-
t i g h t c o n t a i n e r a n d r e c o r d t h e w e i g h t of b a g + c o n t a i n e r (Wl). R a p i d l y
t r a n s f e r a p p r o x i m a t e l y 150 g o f t h e h a m m e r m i l l e d s a m p l e t o t h e b a g . F a s t e n
the top of the bag and transfer to the airtight container. Weigh the bag +
c o n t a i n e r a n d r e c o r d as (W2).
Washing—Immerse t h e b a g i n c o l d r u n n i n g w a t e r a n d s q u e e z e a t t h e
c o m m e n c e m e n t of w a s h i n g a n d at 15 m i n u t e i n t e r v a l s for a p e r i o d of o n e
hour. R e m o v e the bag, squeeze or spin d r y to remove surplus w a t e r a n d
t r a n s f e r t o b o i l i n g w a t e r , r e p e a t i n g t h e p r o c e d u r e for a f u r t h e r h o u r .
Drying—Remove s u r p l u s w a t e r b y s q u e e z i n g o r s p i n d r y i n g a n d t r a n s f e r
t o a n air o v e n . D r y t o c o n s t a n t w e i g h t a t 100 t o 105 °C. W h e n r e m o v e d f r o m
t h e o v e n for w e i g h i n g t h e b a g s a r e p l a c e d i n t h e a i r t i g h t c o n t a i n e r . R e c o r d
t h e w e i g h t o f c o n t a i n e r + b a g + f i b r e (W3). E m p t y t h e b a g s a n d r e m o v e all
a d h e r i n g fibre. R e - d r y in t h e o v e n for o n e h o u r at 100 to 105 o C. Cool in t h e
a i r t i g h t c o n t a i n e r a n d r e - w e i g h (W4).
N.B.—The determination should be carried out in duplicate whenever

practicable.
Sucrose in High Purity Materials

The present methods for the determination of sucrose in relatively high
purity materials e.g. first expressed juice, clarified juice and syrup, are based
on the original Clerget method whereby the polarization of the sucrose solu-
tion is determined both before and after inversion. The method is based on
the assumption that optically active materials other than sucrose are not
affected by the inversion.
The inverting agents employed are either the enzyme invertase or hydro-
chloric acid. The former is considered to yield more correct results, due to the
fact that it is an enzyme specific to sucrose, but because of the necessity of
maintaining and storing a supply of suitable invertase, this method has in the
past received only partial acceptance for factory control analysis.
Attempts to eliminate the defects of hydrochloric acid as an inverting
agent have led to the development of numerous modifications of Clerget's
method. The method most widely accepted is the Jackson and Gillis Modifica-
tion No. IV, in which sodium chloride is added to the solution used for the
direct polarization, to offset the effect of the chloride ions in the acid added
to the inverted solution.
Two methods of analysis are presented. Both require a high degree of
analytical precision to obtain reproducibility, and it is recommended that for
reliable results the determination of sucrose on any one sample be carried out
at least in duplicate.
Optical Invertase Method

Preparation—Dissolve t w o a n d a half t i m e s t h e n o r m a l w e i g h t of t h e
s u b s t a n c e i n w a t e r i n a 2 5 0 m l v o l u m e t r i c f l a s k . ( D e p e n d i n g o n t h e colour,
multiples or fractions of this weight m a y be used a n d t h e weights calculated
to a b a s i s of 26 g p e r 100 ml.)
Add sufficient dry lead to just clarify the solution, mix by swirling and
dilute to volume. Mix by shaking and filter, keeping the funnel covered with
a watch glass. Reject the first 25 ml of nitrate. If the filtration rate is slow,
it is advisable to use two filters in parallel.
Delead the filtrate by adding ammonium dihydrogen phosphate in as
small an excess as possible. Mix well, filter and again reject the first 25 ml of
filtrate.
Direct Reading—Pipette 50.0 ml of lead-free filtrate into a 100 ml
volumetric flask. Dilute to volume, mix well and transfer to a 200 mm water
jacketed tube. Allow to stand for approximately 10 minutes, record the
temperature and polarize.
The polariscope reading multiplied by 2 is taken as the direct reading,
designated P.
Invert Reading—Two alternatives are available, either a 24 hour inver-
sion using 5 ml of invertase for the actual inversion, or a rapid inversion at
elevated temperatures using 10 ml of invertase.
24 Hour Inversion—In a separate operation accurately determine the
quantity of acetic acid required to reduce 50 ml of the filtrate to a pH of 4.4.
To another 50.0 ml portion in a 100 ml volumetric flask add the requisite
quantity of acid and 5 ml of invertase solution. Dilute almost to volume
and allow to stand overnight, preferably at a temperature of not less than
20 °C.
Dilute to volume, mix well and polarize in a water jacketed tube at 20 °C.
Determine the optical activity of a similar portion of the invertase previously
used by diluting this portion to 100 ml and polarizing. Correct the invert
polarization for the effect of the optical activity of the invertase solution, and
multiply by 2 to obtain the corrected invert reading for a normal solution,
designated P 1 .
Determine the total solids of the original sample by refractometer, mul-
tiply this figure by the density at 20 °C and use the result to calculate total
solids from the original solution in 100 ml of the invert solution, designated g.
Rapid Inversion—If this procedure is used, add 10 ml of invertase solu-
tion to 50.0 ml of nitrate in a 100 ml volumetric flask. Transfer to a water
bath and hold at 55-60 °C for 15 minutes with occasional swirling. Cool the
flask and contents, add soduim carbonate until distinctly alkaline to litmus
paper, adjust to volume and polarize in a water jacketed 200 mm tube.
Record the temperature to the nearest 0.1 °C. Allow the solution to remain
in the tube for approximately 15 minutes and again determine the polariza-
tion. If there is no change from the previous reading, mutarotation is com-
plete.
If it is necessary to work at a temperature other than 20 °C, both the
direct and invert polarizations should be made at the same temperature,
which should be as near as possible to 20 °C.
Calculation—The percentage sucrose, S, in the original sample is derived
from the formula
N.B.—The strength of each batch of invertase should be periodically

checked to ensure that it complies with the A.O.A.C. specification. This is
defined as invertase which under the specified conditions of the test will
produce a drop in polarization of 3.96 in a solution of 10 g of sucrose in 110 ml.
The test is carried out as follows:—
Dilute 1 ml of invertase concentrate to 200 ml with distilled water.
Dissolve 10.00 g of pure sucrose in a 100-110 ml volumetric flask, using
approximately 60 ml of distilled water. Add two drops of glacial acetic acid
and make up to a volume of 100 ml.
Add 10 ml of the diluted invertase to the sugar solution, mix thoroughly
and allow to stand for exactly 60 minutes at 20 CC.
Render alkaline to litmus by the addition of solid sodium carbonate.
Polarize in a 200 mm tube to obtain a reading P.
If the activity is unity or greater, the invertase complies with the

A.O.A.C. specification.
Jackson and Gillis Modification No. IV

This method is applicable in the presence of invert sugar, as the effect
of hydrochloric acid inversion on this substance is balanced by the addition
of sodium chloride ions to the solution used for the direct polarization. As
previously mentioned, the method is not recommended for low purity
materials or materials containing appreciable quantities of optically
active non sugars, the specific rotations of which can be subject to significant
changes during acid inversion.
Preparation—Juices are taken undiluted, while sugar, syrup and high
grade pan products are prepared at a concentration of 2 normal weights in
200 ml.
Clarify the appropriate preparation with dry lead (as for pol determina-
tion) and filter. Delead the filtrate with anhydrous potassium oxalate. The
quantity required is determined by a potassium iodide test on small portions
of the filtrate.
Direct Polarization—Pipette 50.0 ml of filtrate into a 100 ml volumetric
flask. Add 10.0 ml of Jackson and Gillis sodium chloride solution. Dilute to
volume with distilled water and filter only if necessary. Stopper and retain
so that this solution and the one from the next stage are read at approximately
the same time and at the same temperature.
Polarize in a water jacketed 200 mm tube and multiply the result by 2.
Designate as P.
Invert Polarization—Pipette 50.0 ml of filtrate into a 100 ml volumetric
flask. Either of the following procedures may be adopted for inversion but the
U.S. Customs method is considered to be more precise and is preferred.
A. Walker Method—Insert a thermometer in the flask and heat in a
water bath until a temperature of 65 °C is attained. Remove the flask and
add 10.0 ml of Jackson and Gillis hydrochloric acid solution. Mix by swirling
and set aside for 30 minutes.
Cool to room temperature, wash any adhering liquid from the thermo-
meter and dilute to volume. Polarize in a water jacketed 200 mm tube at the
same temperature at which the direct reading is determined and multiply
the reading by 2. Designate as P1. Record the temperature of the polarization
to the nearest 0.1 °C.
Or B. U.S. Customs Method—Transfer 10 ml of Jackson and Gillis

hydrochloric acid solution to the cold 50 ml of nitrate. Insert a thermometer
and transfer to a water bath. Heat to 60 °C and hold for 10 minutes. Agitate
the flask during the first 3 minutes. Rapidly cool to room temperature, wash
adhering liquid from the thermometer and dilute to volume. Polarize as
described in the previous alternative.
Calculation—
The concentration of sucrose is calculated from P and P1 using the
formula
In the case of an undiluted solution this formula gives an apparent sucrose

reading which is used in conjunction with Schmitz's Table as if it were a pol
reading.
A separate Clerget divisor is required for each method.
Walker Method Divisor = 132.63 + 0.0794 (m —13) —0.53 (t — 20)
U.S. Customs Method. Divisor = 132.56 + 0.0794 (m —13) —0.53 (t — 20)
where t = temperature of polarization °C
and m = total solids, g per 100 ml, in the actual
invert solution
N.B.—The divisors for the Walker Method for solutions ranging from
8 to 26 Brix are shown in Table IX, while the temperature corrections are
shown in Table X.
The divisors for the U.S. Customs Method may be obtained by deducting
0.07 from those listed in this table.
Brix = 18.1°
P at 25.7 °C = 60.2
P1 at 25.7 °C = —18.3
P—P1 = 78.5
Divisor for 18 Brix = 132.31
Temperature correction = —3.02
Corrected divisor = 129.29
In the case of solutions of normal strength, or related thereto by a simple

ratio, the values of P and P 1 must be expressed as for a normal solution.
Hence, if the original solution were of half normal strength the direct and
invert readings would be made at quarter normal strength and the readings
must be multiplied by four to give P and P1.
The Clerget divisors may be calculated from the formulae given above.
For sugars (1 N.W. in 100 ml) the value 132.63 at 20 °C may be taken, and
for final molasses (1 N.W. in 300 ml) 131.88 at 20 °C. These apply to the
Walker method of inversion, and must, of course, be corrected to the temper-
ature of the operation. The formula shown above
S = (P — Pl) X 100
Clerget divisor
then gives the percentage of sucrose S directly, when P and P 1 are expressed
in terms of a normal solution.
Sucrose in Low Purity Materials

Optical methods are not recommended for the determination of sucrose
in low purity materials. A more suitable technique is that known as the Chemi-
cal Method. Basically the chemical method involves the determination of the
original reducing sugar content of the sample, followed by another reducing
sugar determination after the sucrose present has been inverted to reducing
sugar. Two methods for carrying out the inversion are given.
Chemical Method
The weights and suggested dilutions shown below are normally suitable
for final molasses samples. They may have to be varied to suit local condi-
tions. (If B molasses is to be analysed, a concentration 10 g of sample in 250
ml, and titration of the undiluted filtrate should suffice).
Procedure—Accurately weigh out approximately 4 g of final molasses.
Transfer to a 250 ml volumetric flask. Dissolve and dilute to volume. Warm
the flask and contents to 40 °C. Add 1 g of powdered potassium oxalate.
(This precipitates the calcium from the solution.) Shake well and cool. Filter
through a No. 1 Whatman paper after having added a small amount of
kieselguhr to assist filtration.
Direct Reducing Sugar Determination—Pipette 50.0 ml of filtrate into a
100 ml flask. Dilute to volume and shake.
Prepare Fehling's solution by adding 5.0 ml of No. 1 and 5.0 ml of No. 2.
Fehling's into a 250 ml boiling flask. Add four drops of methylene blue
indicator and titrate as described in the section on reducing sugars determina-
tion.
Estimation of Total Sugars
A. Invertase Method—Pipette 50.0 ml of filtrate into a 250 ml volumetric
flask. Add two drops of glacial acetic acid followed by 10 ml of invertase.
Heat in a water bath to 57.5 °C for 25 minutes. Agitate continuously
for the first three minutes and then intermittently for the remainder. Cool
to 20 °C and make to volume with distilled water. Titrate against 10.0 ml
of mixed Fehling's solution using methylene blue as an indicator.
B. Acid Inversion Method—Pipette 50.0 ml of filtrate into a 200 ml
volumetric flask. Add 10.0 ml of Jackson and Gillis hydrochloric acid solution.
Insert a thermometer and heat the flask and contents to 60 °C in a water
bath. Agitate the flask during the initial three minutes of heating. After a
total heating time of ten minutes, remove the flask, cool in water and dilute
to volume.
Add one drop of phenolphthalein indicator and neutralize with 4 N
sodium hydroxide to the first darkening of the solution. Dilute to
volume. Titrate against 10.0 ml of mixed Fehling's solution using methylene

blue as an indicator.
Calculation—(Example for the Acid Inversion method using the weights
and dilutions as stipulated).
Per cent sucrose = (total sugars — reducing sugars) X 0.95

Note 1. In this calculation the 0.5 g sucrose column in Table V is used.
Note 2. In this calculation the 0.0 g sucrose column in Table V is used.
Reducing Sugars
Of the numerous methods available for the determination of reducing
sugars, only one is listed in this Edition, namely the Lane and Eynon method,
as this has now received almost universal acceptance by the Queensland
Sugar Industry. Briefly, this method consists of the titration of a sugar
solution of unknown reducing capacity against standard strength Fehling's
solution.
For accurate results the level of reducing sugars in the test sample should
be approximately 0.2 g per 100 ml of solution. If the test solution has a
concentration greater than this it must be diluted. If the test solution has a
reducing sugar concentration less than 0.1 g per 100 ml, a known quantity
of standard invert solution should be added to the test solution to laise the
reducing sugar concentration to a level of approximately 0.2 g per 100 ml.
The amount of added invert is later subtracted from the final result. In the
case of high polarization sugars, this can normally be obtained by adding
20 ml of standard invert solution to a 200 ml flask. One drop of phenolphtha-
lein indicator is added, and the excess acidity is then neutralized with caustic
soda solution. The weighed quantity of sugar (usually 50 g) is then added to
the flask, dissolved and diluted to volume.
For other sugar mill products the dilution required must be ascertained
by a process of trial and error. Clarification of samples is not usually carried
out, but when any appreciable quantity of calcium is present this is precipi-
tated by adding 0.1 g of potassium oxalate per 100 ml, and filtering off the
precipitate.
Method of Lane and Eynon
Incremental Method of Titration—Prepare the Fehling's solution just
prior to the titration, by pipetting 5 ml of Fehling's A solution and 5 ml of
Fehling's B solution into a 250 ml boiling flask.
N.B.—If water is added at this point to obtain a more workable volume,
the quantity added must be standardized. This same volume must also be
used in the initial standardization of the Fehling's solution.
Exploratory Titration—Add approximately 15 ml of the test solution
from an offset burette to the prepared Fehling's. Heat to boiling. The colour
of the boiling solution will give an indication of the additional quantity of test
liquid required to reduce the remaining copper. If the end point appears to
be reasonably close, continue boiling for two minutes and add four drops of
methylene blue indicator. Continue the titration in aliquots of 1 ml or less
until the colour is completely discharged.
N.B.—The liquid must be kept boiling during all stages of the titration.
Final Titration—Repeat the above in a modified form i.e. To 10 ml of
mixed Fehling's solution, add the volume determined from the rough titration
less approximately 0.5 ml.
Heat to boiling, and boil for exactly two minutes. Add four drops of
methylene blue indicator, and recommence the titration 15 seconds after the
commencement of indicator addition.
Complete the titration within a total boiling time of three minutes.
Calculation of Results—The reducing power of an invert sugar solution
is affected by both the volume of the final solution and the concentration of
sucrose present in the solution. Allowances for these factors have been
calculated in Table IV and the expanded version in Table V.
Example {A) Undiluted Juice
Uncorrected Brix of juice = 19.7
Pol of juice = 17.8
Approximate density of juice (Table XIV) = 1.08 grammes per ml
Grammes sucrose per 100 ml (pol x density) = 19.0 approx.
Titration (ml) = 20.0
mg R.S. per 100 ml (Table IV) = 222
Per cent R.S. in sample 222 x 100
= 1000 x 108
= 0.21 per cent
Example (B) Sugar with Added Invert
Added invert = 100 mg per 100 ml
Sucrose concentration = 25 g per 100 ml
Titration (ml) = 27.5
mg R.S. per 100 ml (Table IV) = 155
After deduction for added invert = 55
55 x 100
Per cent R.S. in sample
= 1000 x 25
= 0.22 per cent
Ash
Theoretically, ash is defined as the residue remaining after burning off
all organic matter. In practice however, the position is more complicated,
as the total removal of "ash" from all sugar products is not always possible.
A further complication arises from the fact that the chemical form in which
the ash is determined is normally not the form in which the ash is present in
a sugar product.
Furthermore, a diversity of opinion still exists on such points as whether
single or double sulphation should be used and whether or not a ten per cent
deduction should be applied. The overall quantity of sulphuric acid to be
used for the determination is also a matter of debate. Apart from the varia-
tions in registered quantities that result from changes in technique, the in-
fluence of these changes on working formulae such as R.S./Ash ratio, and the
effect on the difference between actual and expected purity when considering
final molasses exhaustion criteria, should also be borne in mind.
In an endeavour to remedy this situation and to obtain some uniformity
in reporting results for Mutual Control purposes, we strongly recommend that
the following be adopted for control analysis—double sulphation, no deduc-
tion, concentrated acid addition of 0.5 ml before the first incineration followed
by five drops before the second incineration. For the analysis of sugar for
payment purposes, the practice of single sulphation, using 2 ml of concentrated
acid and the application of 10 per cent deduction to the result, is still followed
in Queensland.
Gravimetric Ash Determination
Three items of importance that are associated with the ash determination
are listed below:—
Quality of Sulphuric Acid—Check each bottle of sulphuric acid to be
used for ash determination as follows:—
Transfer 25 ml of the acid from a measuring cylinder to a prepared
platinum crucible. Evaporate cautiously in a fume cupboard. Transfer to a
muffle oven and ignite at 500 °C. Cool in a desiccator. The weight of residual
ash from the 25 ml aliquot should not exceed 0.001 g. Acids with a residue in
excess of this figure should not be used for this work.
Preparation of the Platinum Crucible—Wash the crucible and polish both
inside and out with moistened keiselguhr. Rinse with distilled water and
remove excess droplets with filter paper. Heat to 800 °C for approximately
30 minutes and allow to cool in a desiccator.
Health Hazard—It is important that the preparatory stages of heating
should be carried out in a fume cupboard effectively vented to the atmosphere.
Sulphuric acid vapour can cause severe damage to the respiratory tract.
The vapour also has a highly corrosive action on metallic laboratory fittings.
Procedure—The following sample weights for the various sugar products
are recommended.
Sugar 5g
First Expressed and Clarified Juices 20 g
Syrup and A Massecuite 3g
Products of lower purity 2g
Weigh out the recommended weight of sample into a prepared platinum
crucible. Add 0.5 ml of concentrated sulphuric acid by drops over the surface
of the sample. Heat the crucible gently on a hot plate to carbonise the sample.
(Dilute solutions should be evaporated to syrup consistency in a water bath
to avoid loss of solids.) Continue heating on a hot plate until frothing has
ceased. Incinerate in a muffle oven at 550 °C until no trace of unburnt carbon
is visible.
Remove the crucible, cool and add five drops of concentrated sulphuric
acid to wet the residue. Transfer to a muffle oven and again incinerate until
a temperature of 800 °C is attained. Remove after 15 minutes at 800 °C and
transfer to a desiccator. Weigh when cool and express the weight of residue
as a percentage of the original sample.
Conductometric Ash
An approximation of the ash content of raw sugar products can be
obtained rapidly by the conductometric method. When sugar is dissolved in
water, the soluble impurities disperse into electrically charged particles called
ions. As the passage of an electric current through a solution is dependent
upon the concentration of ions present, a measure of the concentration of
soluble impurities can be obtained from a simple conductivity measurement.
One shortcoming of the conductometric method is that the relationship
between gravimetric and conductometric ash must be known for each grade
of sugar product. This relationship is then assumed to be valid for all samples
tested in each category. Significant departures from these standards can occur
in actual practice however, but the method is a useful adjunct to routine
factory control purposes.
Apparatus—A special elec-
trolytic conductivity meter
known as an "ash bridge" is
used. A suitable conductivity
meter is illustrated in Fig. 41.
Procedure—Weigh out 10 g
of sample (if below one per
cent ash) and transfer to a
200 ml volumetric flask. Dis-
solve and dilute to volume.
N.B.—If the sample has
an ash content above one per
cent, a mixture of sample and
pure sucrose should be substi-
tuted to give a 10 g sample
with an ash content equal to
approximately 0.5 per cent.
Determine the conductivity of the solution, making corrections for the
temperature at which the determination is carried out.
Calculation—
where C = the predetermined relationship between gravi-

metric and conductometric ash for the particular
grade of product.
Sugar Analysis
The majority of methods for the routine analysis of raw sugar are
presented under this sub-heading. The procedures for reducing sugars, ash
and phosphates however, may be located under their specific sub-headings
as their procedures have a general application to other types of sugar products.
Polarization
The procedure for raw sugar polarization has been the subject of much
debate for a number of years. Investigations into this analysis are still being
carried out, and, no doubt, the pending introduction of automatic polari-
meters into the industry will result in considerable changes in this section.
The polarization of a sugar is one of the most exacting analyses carried out
by a sugar chemist, and rigorous adherence to a standard procedure is
essential if reproducible results are to be obtained.
At the 14th Session of ICUMSA in 1966, a recommendation was duly
adopted for a method to be referred to as ICUMSA polarization Method 1.
This method is based on the use of the International Sugar Scale, clarification
by the standard wet lead solution, a standard specification for apparatus,
and for the procedures to be followed during preparation of the solution,
filtration, polarization of the filtrate and the corrections to be applied to the
observed polarization. The following procedure is based in principle on
ICUMSA polarization Method 1.
Apparatus
This should conform to the standards laid down by ICUMSA (1966).
Included in the apparatus are saccharimeters or sugar polarimeters, quartz
plates, balances, flasks, polarimeter tubes or cells, cover glasses, funnels,
filter paper and basic lead acetate.
Although the specification for flasks includes various types, it is re-
commended that the flask made to the British Standard 675 Type 2, be the
only flask used for the polarization of raw sugar. This flask has been specific-
ally designed for this purpose not only in its dimensions, but also for ease of
mixing after completion to volume.
All sugar polarizations should be conducted in a room maintained at a
constant temperature and relative humidity (20° ± 0.5 °C and 65-70 R.H.).
If this temperature is not attainable the range 15 to 25 °C should not be
exceeded, if possible.
Preparation of Solution
Thoroughly mix the sugar samples received for analysis prior to weighing
capsule, on a balance with a sensitivity reciprocal of 0.1 milligrammes per

scale division. Transfer by washing with about 60 ml of distilled water into
a 100 ml flask conforming to B.S. 675 Type 2 specification.
Dissolve the sugar, without any loss from the flask, and add 1.0 ml of
basic lead acetate solution, (made to the specification as detailed in Chapter
VIII) from a reservoir protected from atmospheric carbon dioxide. Mix in the
added lead solution by swirling gently, then add further distilled water until
the bulb of the flask is filled. Allow to stand at least 10 minutes making sure
that no air bubbles are entrapped in the flask.
Dilution to Volume
Add distilled water to bring the meniscus level to about five mm below
the graduation line. If necessary, ether or alcohol vapour from a blower may
be used to clear the meniscus before finally making to volume with distilled
water. For setting of the meniscus to the graduation line it is recommended
that a strip of black paper be secured around the neck of the flask with a
clip, at about 1 mm below the graduation mark. Place the flask on a stand at
eye level and add the distilled water from a fine jet until the lowest point of
the meniscus is at the top edge of the graduation line.
Remove any drops of water adhering to the neck of the flask by means
of a rolled strip of filter paper. Stopper and thoroughly mix the solution.
Allow it to stand for at least five minutes to permit settling of the precipitate.
Filtration
Filter the solution through a single paper (the moisture content of which
is in the range 6-8 per cent when dried for 3 hours at 100 °C), fitted neatly
without any overlap in a stemless funnel made of non-corrosive material.
Cover the filter with a suitable cover of non-corrosive material to minimize
evaporation during filtration. Discard the first 5 to 10 ml of filtrate and do
not return any of the filtrate to the filter.
N.B.—The nitration should be carried out as rapidly as possible and the
funnel must be seated firmly in the mouth of the filter glass and not in a
filter stand.
Rinse a clean dry glass pol tube of 200 i 0.03 mm length (previously
tested so that no detectable change in reading is observed on rotating the tube
in the trough of the saccharimeter), at least twice with filtrate. This rinsing
assists in wetting the walls of the tube and washes out any unobserved foreign
matter. When the tube is finally filled with the filtrate, close off with a cover
glass made of good optical glass with plane parallel faces free from defects.
The cover glasses are held in position with the threaded cap ends complete
with good quality rubber washers of the correct size. Do not overtighten the
caps as this could cause strain to the cover glasses, resulting in their becoming
optically active. With enlarged end tubes any air bubbles in the tube are
collected in the enlarged end by inverting the tube a few times, so that on
placing the tube in the trough of the saccharimeter a continuous path of solu-
tion is presented to the polarized light. To avoid undue temperature rise in
the filtrate, the tube must be handled as little as possible before being placed
in the trough of the saccharimeter.
The saccharimeter used shall be fitted with the International Sugar Scale
in compliance with the ICUMSA (1966) standards.
Reading of the Filtrate

The saccharimeter shall be standardized at the time of reading, by means
of a standard quartz plate of the value close to the observed polarization.
The value of the quartz plate shall have been checked by an authorized
authority.
Determine the reading of the filtrate, making at least five settings of the
instrument and averaging the result. Each setting should be read to the
accuracy of the instrument.
A scale correction based on the reading of the standard quartz plate is
then applied to the observed reading.
Determine the temperature of the filtrate as soon as practicable after the
saccharimeter readings, by immersing a thermometer graduated in tenths of
a degree in the tube after a little of the solution has been removed. To mini-
mize handling, it is recommended that the tube be placed upright in a clean
dry container whilst the temperature is being determined.
After the temperature of reading has been measured, the correction to be
applied to adjust the observed polarization to 20 °C is made as follows: —
When the reading is obtained in a quartz wedge saccharimeter
P20 = pt +. 0.00033 S (ty — 20) — 0.0047R (tv — 20)
where P20 = polarization at 20 °C
Pt = polarization at t °C
S = per cent sucrose in sample
R = per cent reducing sugars in sample
tr = temperature of solution as read °C.
When a sugar polarimeter is used the coefficient 0.00033 S is smaller and
may be taken as 0.00019 5.
The temperature used in the above formulae for correcting polarizations
to 20 °C is the actual temperature of reading, and the assumption is made
that this temperature is the same as that at which the solution was made to
the mark. Even if all operations are carried out in a constant temperature
room, this assumption will not necessarily be correct. Any change in concen-
tration of the solution caused by a change in temperature between making
to the mark and polarizing should be allowed for. For this reason if it is not
possible to carry out the preparation of solutions, the nitrations, and the
readings in a constant temperature room, it is important that the temperature

should vary as little as possible from the start to finish of the operations i.e.,
by not more than 0.5 degree C. If however, there is reason to suspect that the
temperature of reading the filtrate differs from the temperature of making
to the mark by more than 0.5 degree C, the temperature of making to the
mark shall be determined. This shall be done by placing a clean dry thermo-
meter, graduated in tenths of a degree C, in the flask immediately after
shaking and before the solution is poured on the filter. This temperature
should be noted and recorded to the nearest tenth of a degree, and if necessary
the quantity 0.027 (tr —• tm) should be added to the observed polarization,
where tr is the temperature of reading the filtrate in the saccharimeter, and
t m is the temperature of making the solution to the mark.
The pol of the sugar reported will be the observed reading, corrected
for scale error, corrected if necessary for errors in flask and tube, and corrected
for temperature when observations are made at temperatures other than 20°C.
Moisture
For routine control purposes, the moisture content of raw sugar is taken
as the loss of weight resulting from the air drying of a 5 g sample at 103 to
105 °C for a period of three hours. The value recorded should be regarded as
relative rather than absolute, as some thermal degradation of the sample
occurs under these test conditions.
Although a simple procedure, the moisture determination can give vary-
ing results unless both technique and test conditions are adequately stan-
dardized. Determinations should be carried out in duplicate and repeat deter-
minations carried out if the duplicates differ by more than 0.05 per cent.
Drying Dishes- -These are approximately two inches in diameter, half
an inch deep and should be fitted with close fitting lids.
Procedure—Prepare the requisite number of dishes by drying overnight
in an air oven. Transfer the covered dishes to a desiccator and allow to cool
to room temperature. Weigh the dish plus lid to ^O.OOOl g.
Rapidly add approximately 5 g of sample evenly over the dish surface
and replace the lid. Determine the weight accurately. The sample addition
and weighings should be carried out as rapidly as possible. Transfer the dish
and contents to an air oven and dry for three hours at 103 to 105 °C.
At the completion of drying, replace the lid and allow to cool to room
temperature in a desiccator. Weigh the dish plus dried sample again to
±0.0001 g. Express the loss of weight as a percentage of the original sample
weight.
Filterability
The test involves the constant pressure filtration of a raw sugar solution
under standard conditions. The filtration rate of the test solution is compared
with the filtration rate of a pure sugar solution which has been filtered under
identical conditions.
Strictly speaking, the per cent filterability is defined at 20 ±1 °C, and
the procedure and calculation tables are designated for temperature controlled
laboratories. Temperature control of ±1 °C is difficult to maintain however,
and if the test is performed at a temperature outside this range, the result
can only be validly expressed as "filterability at t°C".
Table XXXVII will permit the calculation of "filterability at t °C"
between the ranges of 12 and 32 °C. As temperature changes are likely to
ANALYTICAL METHODS
occur during the test, the average of the temperatures taken before and after
the test should be used.
Special Apparatus—Pressure Filter. The C.S.R. type filter shown in
Fig. 42 is assembled in the following order:— rubber gasket, filter disc,
Whatman No. 54 filter paper, retaining ring and second rubber gasket.
Air Pressure. A supply of compressed air or nitrogen at 50 pounds per
square inch is required.
Stirrer. This should have a running
speed between 1000 and 1200 rev/min.
Excessive and prolonged stirring should
be avoided so that damage to filter aid
particles is minimized.
Procedure—Mix the sample thor-
oughly and weigh out the appropriate
amount of sugar (listed in the following
table) into a 400 ml beaker.
Add 99.4 ml (equivalent to 99.1 g
in air) of distilled water. Then add
0.720 g (equivalent to 0.48 per cent on
solids) of standard filter aid, and dis-
solve the sugar using the stirrer. This
usually requires 25 to 35 minutes of
stirring. Minimize evaporation by keep-
ing the solution away from draughts
and covering it when not being stirred.
Add 2.0 ml of standard buffer
solution (Chapter VIII), and stir for
two minutes ±lO seconds. Cover the
solution and allow to stand for 15 min-
utes ±0.5 minutes.
Assemble the filter, stir for a fur-
ther 60 seconds and pour the liquid into
the filter body. Read the temperature
of the solution to ±0.1 °C.
Per cent Moisture of Sugar Sample Weight g ±0.05
0.0 — 0.2 149.0

0.2 — 0.5 150.0
0.5 — 0.8 151.6
0.8 — 1.0 152.6
Close filter, apply air pressure of 50 lb/in 2 gauge and commence timing
of filtration immediately the pressure is applied. Discard the filtrate for the
first two minutes and collect the filtrate for the next five minutes in a tared
100 ml beaker. Release the air pressure and determine the temperature of
the residual solution.
Calculation—Average the initial and final temperatures to 0.1 °C. Re-
weigh the beaker to determine the amount of filtrate collected between two
and seven minutes of filtering. Refer to Table X X X V I I and find the corre-
sponding weight of pure sugar syrup equivalent to the weight obtained at the
temperature of the determination. Calculate per cent filterability as
Notes on the Determination

(i) Keep the filter and gaskets thoroughly clean.
(ii) Keep the filter disc, when not in use, in the lightly assembled filter.
(iii) Make sure that the gaskets are not perished or damaged in any way.
(iv) Check the pressure gauge at regular intervals.
(v) The filter disc should be calibrated once every two months to check
its performance.
(vi) For affined or good filtering sugars, twice the amount of solution
may be required. In these cases, twice the amount of buffer solution
and filter aid will have to be added.
Calibration of Pressure Filter Discs—The performance of a filter disc
must be checked at regular intervals against the standard flow rates in
Table XXXVII, before any routine filterability determinations are carried
out. If the discrepancy is greater than four per cent, a replacement filter is
required.
The calibration is carried out as follows:—
Prepare about 500 g of 60° Brix syrup using A.R. sucrose and distilled
water. Add a weight of standard filter aid equal to 2 1/2 per cent of the weight
of the solids in the syrup. Mix and pressure filter in two separate portions
through Whatman No. 54 filter papers. Discard the first 20 ml of filtrate
from each filtration. Mix both portions of clear filtrate, weigh, and adjust
the Brix to 60.0 ± 0 . 1 ° Brix.
Determine the amount of filter aid equal to 0.48 per cent of the solids in
the syrup. Add about 50 ml of syrup to the weighed amount of filter aid in a
separate beaker and mix to a smooth slurry consistency by means of a rubber
tipped stirring rod. Avoid grinding of the filter aid. Transfer the slurry to the
bulk of the syrup and recover any residual slurry with original syrup.
Add 1.4 ml of standard buffer solution. Mix for two minutes using the
electric stirrer, cover and allow to stand for 15 minutes as before. Filter the
syrup as previously described.
N.B.—(i) The quantity of syrup collected should be within 4 per cent of
the corresponding quantity shown in the table.
(ii) If a check reveals faults, and the pressure gauge is correct, renew the
filter disc. Calibrate the new disc before use.
Grain Size Distribution: Grist Analysis

The results obtained from previous routine methods for grist determina-
tion were often influenced by the amount of syrup film surrounding the
crystals, and by the conditions of humidity and temperature prevailing at the
time of the determination. The C.S.R. method presented below, however,
minimizes the tendency of crystals to adhere to each other, by removal of
most of the syrup film with successive washings of methyl and isopropyl
alcohol.
Special Apparatus—
Drying Oven—This should have an explosion proof rating and should be
so situated that any emerging alcohol vapours can be directly removed to
outside atmosphere.
Sieves—Three British Standard screens or their equivalents in the Tyler
rating are employed. The recommended screens are as shown:—
! British Standard Screen Tyler Screen

Mesh Size of Opening Mesh Size of Opening
mm mm
i
18 0.853 20 0.833
25 0.599 28 0.589
0.422 35 0.417 !
36
Jar Mill—A jar mill with a speed of approximately 75rev/min is required

for the mixing process. Several commercial units are available, but some
items of laboratory machinery can be modified for this purpose.
A two pint Agee jar with the normal sealer cap is required for mixing.
The outer surface of the jar should be covered wdth one thickness of bandage
impregnated with Araldite. Also required are an Agee lid ring covered with
100 mesh gauze, and an outer rubber sealing ring, which will form a seal when
the jar is inverted over a Buchner funnel.
Sample Preparation—Thoroughly mix the sugar sample and transfer
approximately 11.0 g to the Agee jar. Add 250 ml of 99 per cent methyl
alcohol, seal and rotate for three minutes at 75 rev/min on the jar mill.
Substitute the gauze covered cap, invert the jar over a Buchner funnel and
draw off the alcohol under vacuum. Add 250 ml of 99 per cent isopropyl
alcohol, rotate for three minutes and again remove the alcohol under vacuum.
N.B.—The preceding alcohol washings should be repeated at this stage,
if the sugar sample is below 98 polarization.
Oven dry the sugar on a flat tray at 80 to 90 °C. Occasionally disturb the
sugar with a spatula to prevent caking. Allow the sugar to cool in a desiccator.
Sieve Separation—Weigh out 100.00 g of prepared sample and sieve for
10 minutes on a Ro-tap shaker or Pascall sieve vibrator. Empty the sugar
crystals caught on each sieve onto sheets of glazed paper, brushing out the
sieve with a firm tapping brush, taking care not to damage the screens.
Transfer the sugar from each section to a tared container and weigh the
fractions to 0.01 g.
Round off weights so that the weights of the four fractions add up to
100.0 g. Report the results as a percentage. The percentage of fines is defined
as the percentage passing through the B.S.25 mesh screen, and by plotting
cumulative weight fraction against sieve aperture (linear axis) on arithmetic
probability paper, mean aperture and coefficient of variation can be obtained
in the following manner.
Mean aperture == sieve aperture corresponding to 50 per cent weight fraction.
Starch
The C.S.R. method for the determination of starch in raw sugar is
presented below in a slightly abbreviated form. The method involves hot,
mild digestion of an aqueous solution of raw sugar in calcium chloride/acetic
acid to ensure that any starch present is in a form suitable for subsequent
reaction with iodine. The starch/iodide complex is then determined colori-
metrically at 700 nm. This complex is essentially a colloidal suspension which
is stable for at least five minutes.
Standardization—A standard graph is prepared using B.D.H. Laboratory
Reagent Potato Starch Batch No. 2499440. Refer to Chapter VIII for
preparation of the standard starch and other starch reagents.
Prepare aliquots of the standard starch solution, increasing in concentra-
tion from 0 to 500 p.p.m. starch on solids. These are obtained by adding 40 g
of standard starch-free sugar to each of eight 100 ml volumetric flasks and
then adding 0, 5, 10, 15, 20, 25, 30 and 50 ml aliquots of standard starch solu-
tion. Add distilled water to each flask to make a total volume of approximate-
ly 75 ml, and dissolve. Dilute to volume, stopper and mix. Pipette 15 ml of
each solution into separate 50 ml volumetric flasks and then add 25 ml of
calcium chloride/acetic acid reagent from an automatic burette or graduated
cylinder. Mix thoroughly.
Hold each flask in boiling water for 15 minutes and swirl at five minute
intervals to facilitate the escape of gaseous materials. After exactly 15 minutes
of heating, cool the flasks in running water, dilute to volume, stopper and mix.
From each 50 ml flask, pipette 15 ml aliquots into each of two 25 ml
volumetric flasks designated (a) blank sample and (b) test sample. Then add
2.5 ml of 1 N acetic acid reagent to each 25 ml flask. Flask (a) from each set
is then diluted to volume, stoppered, mixed and later used as a separate blank
for each test sample.
Prepare and analyse each of the flask (b) test samples as a separate entity
in the following manner:— Add 5 ml of freshly prepared potassium iodide-
iodate solution (Chapter VIII). Swirl during the addition of this reagent and
then make to the mark, stopper and mix. Transfer to a 1 cm cuvette. Deter-
mine the optical density at 700 nm against the corresponding blank. The
determination should be completed as rapidly as practicable after the iodide-
iodate solution has been added.
Plot p.p.m. starch on solids against optical density.
Procedure—-The procedure used for raw sugar is basically the same as
that used to obtain the standardization curve.
Dissolve 40.0 g of sugar in 50 ml of distilled water in a 100 ml volumetric
flask. Make up to the mark and mix. Pipette 15 ml of this solution into a 50
ml volumetric flask, add calcium chloride/acetic acid reagent, mix, digest in
a boiling water bath, cool and make up to the mark as previously described.
Pipette 15 ml aliquots into each of two 25 ml volumetric flasks. Add
2.5 ml of 1 N acetic acid to each flask, mix well and make one flask up to the
mark, stopper and mix. This is the sample blank solution.
Fill a 1 cm cuvette with this solution and use it to adjust the spectro-
photometer for infinity and zero optical densities at a wavelength setting of
700 nm.
Add 5 ml of potassium iodide-iodate reagent to the other flask, make up
to the mark, stopper and mix. Transfer this solution to a 1 cm cuvette and
read the optical density at a wavelength of 700 nm, within five minutes.
Read the concentration of starch as p.p.m. on raw sugar solids from the
standard graph.
Total Colour Attenuation
Two methods of colour attenuation have been issued by the C.S.R.
Company. The more precise of these is not included in this Edition as it
requires the use of a precision spectrophotometer of a type which is not
generally available in mill laboratories.
The procedure for the routine method for colour measurement of raw
sugar is given below. The method is also applicable to low polarization sugars,
but in this case, the initial sample weight should be reduced to maintain
maximum sensitivity on the spectrophotometer scale.
Special Apparatus—A millipore vacuum filtering apparatus or a C.S.R.
type pressure filter may be used. Filtration is affected through Millipore type
A.P.30 prefilter discs and type PH (0.3 micron) filter membranes.
Sample Preparation—Weigh out 12.50 g of raw sugar and transfer to a
100 ml volumetric flask. Dissolve in approximately 40 ml of distilled water
and dilute to volume. Mix thoroughly.
pH Adjustment—By means of a graduated measuring cylinder, transfer
50 ml of the solution to a beaker and determine the pH. Adjust the pH of the
solution to 7.00 ± 0.05 pH by drops of either 0.1 N NaOH or 0.1 N HC1,
stirring vigorously during the addition.
Filtration—Filter the solution through a Millipore prefilter disc and 0.3
micron filter membrane. If insufficient sample is collected before the filtration
rate slows appreciably, the filter and prefilter should be renewed.
Reading—Determine the optical density at 420 nm in a 1 cm cuvette
against a distilled water blank.
Calculation—
Total colour attenuation @ 420 nm =
1000 x optical density
(concentration of solution g/ml) x (cell size in cm)
N.B.—If less than ten drops of alkali or acid are used for neutralization,
the calculation, for an original sample weight of 12.50 g per 100 ml, may be
abbreviated to—
Total colour attenuation = 8000 x optical density
If more than ten drops are used for neutralization, the refractometer
Brix should be accurately determined and converted to g/ml concentration,
using Table VII of the Manual.
Mud Analysis
Insoluble Solids
The measurement of insoluble solids in clarifier feed and primary mud
is usually carried out in conjunction with the laboratory settling test for the
assessment of clarifier performance, while the determinations on filter feed and
filter cake are carried out to assess rotary filter performance. Two methods
are given below.
Vacuum Filtration Method—Weigh out 200 g of well mixed sample
and filter through a Buchner funnel. Do not wash the cake with water.
Peel off the cake from the filter paper and weigh the wet cake. Dry to
constant weight at 96 to 100 °C.
Determine the soluble solids content of a separate quantity of gravity
filtered filtrate. This is required to correct for the weight of soluble solids
contained in the cake.
Calculation—
Per cent insoluble solids =
Aluminium Dish Method—This method has been used extensively by

the Bureau in clarifier investigations and is useful where a large number of
samples have to be analysed. Its accuracy is mainly dependent upon accurate
subsampling of a relatively small quantity of material, and the minimizing
of evaporation effects. When samples with a relatively low insoluble solids
content are encountered, the accuracy of the determination may be improved
by prethickening before subsampling. If this is carried out the formula must
be modified accordingly.
Equipment—Flat bottomed aluminium dishes with close-fitting lids.
A deep welled measuring spoon to contain approximately 3 g of sample.
Procedure—Prepare the aluminium dishes by pre-drying and cooling in
a desiccator. Weigh . . .. .. .. .. .. .. .. W1
Thoroughly but rapidly mix the sample and transfer approximately 3 g
to the aluminium dish. Immediately seal the dish and weigh dish plus
contents .. .. .. .. .. .. . .. .. W2
Remove the lid and rotate the capsule to spread the sample in an even film
over the bottom of the container.
Oven dry for 16 hours at a temperature of 70 °C. Seal the container and
allow to cool in a desiccator for 30 minutes. Weigh and record as ..W3
Soluble Solids Correction—Filter a separate portion of the original sample,
taking care to minimize evaporation effects. Determine the Brix to an
accuracy of ±0.03 units by means of a precision refractometer.
Calculation—
N.B.—In the case of materials containing an appreciable amount of

fibre, the fibre content must be determined as described below, and sub-
tracted from the insoluble solids content to obtain the actual percentage of
mud solids.
In the case of filter cake, it may be necessary to apply some compression
to the sample in order to obtain a juice sample for the determination of
refractometer Brix.
Moisture
Low temperature drying of mud is recommended for experimental pur-
poses. For comparative routine determinations on filter cake however, drying
at 100 °C will not introduce serious errors.
Procedure—Weigh out 5.0 g of well mixed sample into a tared aluminium
container.
Dry at 70 °C for 16 hours or for four hours at 100 °C. Cool in a desiccator
and reweigh.
Calculate moisture per cent original sample.
Pol
In the determination of per cent pol in mud by wet lead clarification an
arbitrary adjustment is made to the weight of sample taken, to correct for the
error introduced by the presence of insoluble solids.
Procedure—Thoroughly mix the sample and weigh out 50 g into a nickel
weighing dish. Add a small quantity of water to promote mobility and trans-
fer into a wide mouthed (Kohlrausch type) 200 ml volumetric flask. Add
sufficient wet lead to clarify. This usually requires from 2 to 5 ml. Dilute to
volume with distilled water, shake and allow to stand for at least 5 minutes.
Filter and then polarize in a 400 mm tube.
Calculate pol per cent mud by halving the polariscope reading.
Fibre
For the determination of fibre in mud, a 3 inch diameter 3 inch high cylin-
drical container fitted with a 100 mesh gauze base is employed. An old style
Spencer over drying capsule is ideal for this purpose.
Procedure—Transfer 50 g of the premixed mud sample into the drying
capsule. Hold over a sink and wash with a steady stream of water until the
runnings are clear. Allow surplus water to drain off and then dry to constant
weight in a Spencer-type oven.
The fibre per cent mud will equal double the dry weight of the fibre
(in g), weighing to an accuracy of ± 0.C1 g.
Gum Analysis
The following is a revised version of the U.S.D.A. method for the deter-
mination of gums in cane juices by alcohol precipitation. The method has
been used extensively in cane deterioration studies as it provides a quantita-
tive index of changes that occur in gum content during cane storage. Other
methods of gum determination are available, and although the results of the
method described below may not agree precisely with these, the alcohol
precipitation method is considered to be the most suitable for routine analyses.
Preparation of Standard Graph—Prepare aqueous solutions of A.R. dex-
trose (C 6 H 12 0 6 ) to the following concentrations:—0.001 per cent, 0.05 per
cent and 0.01 per cent.
To a separate test tube for each concentration, add 2.0 ml of dextrose
solution and 1 ml of phenol reagent. (See Chapter VIII under Sugar Detec-
tion). Rapidly add 10 ml of concentrated sulphuric acid to each test tube,
holding the tip of the safety pipette about two inches above the liquid
surface. Take care in case the mixture boils and ejects from the tube. Swirl
to mix and allow to stand for ten minutes.
After t h e r e a c t i o n t i m e h a s e l a p s e d , cool i n w a t e r for t e n m i n u t e s a n d

determine optical density at 485 nm against a blank prepared as above using
distilled w a t e r in place of t h e dextrose solution.
N.B.—The p h e n o l - s u l p h u r i c acid m e t h o d r e q u i r e s a n e l e v a t e d r e a c t i o n
temperature to convert the polysaccharides present to dextrose and other
monosaccharides.
F r o m the optical density results a s t a n d a r d graph of polysaccharide
concentration (expressed as anhydroglucose) versus optical density is ob-
tained.
The concentration of anhydroglucose is calculated by deducting ten
per cent from t h e concentration of t h e dextrose solutions originally used.
T h e r e a s o n for t h i s d e d u c t i o n c a n b e seen f r o m t h e following f o r m u l a e : —
D e x t r o s e C 6 H 1 2 0 6 , M o l e c u l a r W e i g h t 180.156
P o l y - D e x t r o s e ( C 6 H 1 0 O 5 ) n , M o l e c u l a r W e i g h t 162.141
A difference of 18.015 or 9.9997 p e r c e n t .
Determination of G u m s in Juice
Sample Preparation—Sieve a p o r t i o n of t h e j u i c e s a m p l e t h r o u g h a 3 2 5
m e s h s c r e e n . C e n t r i f u g e for six m i n u t e s a t n o less t h a n 2000 g . P r o v i d e d t h e
j u i c e i s u n h e a t e d , t h e a b o v e p r o c e d u r e will r e m o v e s t a r c h i n t e r f e r e n c e . I f t h e
juice or p r o d u c t has been heated, t h e starch c a n n o t be isolated, a n d " t o t a l
g u m s " will b e d e t e r m i n e d .
Alcohol Precipitation—Pipette 10 ml of t h e s u p e r n a t a n t l i q u i d i n t o a
s e p a r a t e c e n t r i f u g e t u b e c o n t a i n i n g 3 0 m l o f a b s o l u t e alcohol, m i x a n d allow
t h e p r e c i p i t a t e t o f o r m b y s t a n d i n g for a t l e a s t five m i n u t e s .
R e c e n t r i f u g e for six m i n u t e s t o c o n c e n t r a t e t h e g u m s i n t h e b o t t o m
o f t h e c e n t r i f u g e t u b e . D e c a n t t h e s u p e r n a t a n t l i q u i d a s q u i c k l y a s possible
t o a v o i d loss o f g u m s . I n v e r t t h e t u b e s o v e r a t o w e l a n d allow excess alcohol
to d r a i n off.
Purification of Gums—Add a few d r o p s of 80 p e r c e n t alcohol i n i t i a l l y
t o assist i n r e s u s p e n d i n g t h e g u m s , a n d s t i r w i t h a glass r o d . W a s h t h e t u b e
w i t h m o r e alcohol u s i n g a t o t a l of 30 ml of 80 p e r c e n t alcohol. Allow to s t a n d
for five m i n u t e s .
C e n t r i f u g e for six m i n u t e s a t n o less t h a n 2000 g . D e c a n t t h e s u p e r n a t a n t
l i q u i d a n d a g a i n allow t o d r a i n o v e r a t o w e l . D i s s o l v e t h e g u m s i n distilled
w a t e r a n d d i l u t e to a v o l u m e of 100 ml in a v o l u m e t r i c flask.
Blank and Test Solution—Pipette 2.0 ml of g u m s o l u t i o n i n t o a t e s t t u b e
a n d p r o c e e d w i t h t h e a d d i t i o n of 1 ml of p h e n o l r e a g e n t a n d 10 ml of s u l p h u r i c
acid as described in t h e section on p r e p a r a t i o n of t h e s t a n d a r d graph.
T h e b l a n k solution is p r e p a r e d in a similar m a n n e r , w i t h the exception
t h a t 2.0 m l o f d i s t i l l e d w a t e r i s s u b s t i t u t e d for t h e g u m s o l u t i o n .
Determine the optical density of t h e test against t h e blank solution at
485 n m .
Calculation—Read off t h e p e r c e n t g u m s in j u i c e for t h e corresponding
o p t i c a l d e n s i t y o n t h e s t a n d a r d g r a p h . (If t h e o p t i c a l d e n s i t y is outside the
limits of t h e graph, t h e g u m solution m u s t be rediluted). A Brix determination
i s c a r r i e d out o n t h e o r i g i n a l j u i c e a n d t h e r e s u l t s e x p r e s s e d a s gums per cent
solids.
Phosphate Analysis
T h e C . S . R . a m i d o l m e t h o d i s r e c o m m e n d e d for t h e d e t e r m i n a t i o n o f
p h o s p h a t e in r a w sugars, syrups a n d juices. P h o s p h a t e is d e t e r m i n e d by
measuring t h e intensity of t h e blue coloration developed in t h e presence of
acid m o l y b d a t e a n d amidol at a wavelength of 660 n m . F o r purposes of
u n i f o r m i t y , i t i s s u g g e s t e d t h a t all p h o s p h a t e r e s u l t s b e e x p r e s s e d a s p a r t s
p e r million p h o s p h o r u s i.e. p . p . m . P .
W h e n u s i n g t h i s m e t h o d o f a n a l y s i s t h e following p o i n t s s h o u l d b e b o r n e
in mind:
(a) I n h a l a t i o n o f t h e v a p o u r f r o m a m i d o l s o l u t i o n s s h o u l d b e carefully
a v o i d e d a t all t i m e s . T h i s s u b s t a n c e i s v e r y t o x i c .
(b) T h e m e t h o d specifies a c i d w a s h e d s u p e r c e l a s s o m e b a t c h e s o f s u p e r -
cel, a s r e c e i v e d , h a v e b e e n f o u n d t o c o n t a i n a p p r e c i a b l e q u a n t i t i e s o f p h o s -
p h o r u s . E a c h b a t c h o f filter p a p e r s s h o u l d also b e c h e c k e d t o e n s u r e t h a t
phosphorus cannot be e x t r a c t e d from t h e paper into t h e sample.
(c) It is a d v i s a b l e to h a v e a s e t of flasks a n d c u v e t t e s w h i c h a r e k e p t
solely for p h o s p h a t e a n a l y s i s a s m i n u t e t r a c e s o f t h e r e d u c i n g a g e n t u s e d i n
t h i s d e t e r m i n a t i o n c a n affect t h e r e s u l t s o f o t h e r a n a l y s e s .
Preparation of Standard Graph—The p r e p a r a t i o n of t h e s t a n d a r d p h o s -
p h a t e s o l u t i o n ( c o n t a i n i n g 0.01 m g P p e r m l ) a n d t h e a s s o c i a t e d r e a g e n t s a r e
d e s c r i b e d i n C h a p t e r V I I I . T h e following a l i q u o t s o f t h e s t a n d a r d p h o s p h a t e
s o l u t i o n a r e t r a n s f e r r e d i n t o 5 0 m l v o l u m e t r i c flasks: 0 , 1 , 2 , 3 , 4 , 7.5 a n d
10 m l .
Colour Development—To e a c h flask a d d t w o d r o p s of c o n c e n t r a t e d h y d r o -
chloric a c i d followed b y distilled w a t e r t o m a k e t o a t o t a l v o l u m e o f 3 0 m l .
T h e n a d d 1 0 m l o f a c i d m o l y b d a t e followed b y 4 m l o f a m i d o l r e a g e n t b y
m e a n s of a u t o m a t i c dispensers. Dilute to v o l u m e with distilled water, s h a k e
a n d let s t a n d for a t l e a s t 1 0 m i n u t e s t o a l l o w a s t a b l e c o l o u r t o d e v e l o p .
Blank Preparation—Prepare a b l a n k s o l u t i o n in a 50 ml flask u s i n g t w o
d r o p s o f c o n c e n t r a t e d h y d r o c h l o r i c acid, 1 0 m l o f a c i d r e a g e n t a n d d i s t i l l e d
water. Adjust t h e s p e c t r o p h o t o m e t e r w i t h t h e b l a n k solution to r e a d zero
o p t i c a l d e n s i t y i n a 1 c m cell a t 660 n m w a v e l e n g t h .
Colour Measurement—Determine t h e o p t i c a l d e n s i t y of t h e c o l o u r e d
solution after t h e s p e c t r o p h o t o m e t e r h a s been s t a n d a r d i z e d w i t h t h e b l a n k
solution. This operation should be carried out between 10 a n d 30 m i n u t e s
after t h e addition of amidol reagent.
Prepare a s t a n d a r d g r a p h by plotting optical density against mg of P
used from t h e s t a n d a r d solution.
Total Phosphate in R a w Sugars

Preparation—Weigh o u t 4 0 . 0 g of s a m p l e a n d t r a n s f e r to a 2 0 0 ml
v o l u m e t r i c flask. A d d sufficient w a t e r t o d i s s o l v e t h e c r y s t a l s .
p H Adjustment—Reduce t h e p H o f t h e s o l u t i o n t o a p p r o x i m a t e l y 4 . 0 .
This usually requires only t w o drops of concentrated hydrochloric acid.
Dilute t o volume w i t h distilled w a t e r a n d m i x .
Filtration—Prepare a s l u r r y by m i x i n g a p p r o x i m a t e l y 20 ml of t h e solu-
tion w i t h a level teaspoon of acid w a s h e d supercel. Use this slurry to precoat
t w o W h a t m a n N o . 5 p a p e r s i n a B u c h n e r f u n n e l . R i n s e t h e B u c h n e r flask
with this filtrate and discard. Filter approximately 50 ml of the test solution
through the pre-coated papers.
Colour Development—Pipette 20 ml of the filtered solution into a 50 ml
flask. Add 10 ml of acid molybdate and 4 ml of amidol by means of automatic
dispensers. Dilute to volume, shake and allow to stand for 10 minutes.
Blank Preparation— Pipette 20 ml of filtered test solution into a separate
50 ml volumetric flask. Add 10 ml of acid reagent, dilute to volume and shake.
Use this solution to adjust the spectrophotometer to zero optical density at
660 nm in a 1 cm cell.
Determine the optical density of the coloured solution against the blank.
This should be carried out between 10 and 30 minutes after the addition of
amidol reagent.
Convert optical density to mg P from the standard graph. Then p.p.m. P
Total Phosphate in Clarified Juice and Syrup

Sample Preparation—Determine the Brix of the material by refracto-
meter, and calculate the weight of material which contains 10 g of soluble
solids. Transfer this amount into a 200 ml volumetric flask, adjust the pH
to 4.0, dilute to volume and mix.
The solution is then filtered and analysed in the same manner as de-
scribed for the determination of phosphate in raw sugars.
Convert optical density to mg P from the standard graph. Then p.p.m. P
on solids = mg P x 1000.
Total Phosphate in Raw Juices

The same procedure as described for syrups is applied, with the exception
that a smaller aliquot of filtered sample is taken for colour development.
A 5 ml aliquot should be sufficient for normal juices, and the calculation in
this instance would then become:— p.p.m. P on solids = mg P x 4000.
Soluble and Insoluble Phosphate

The form in which phosphate is originally present, and the efficiency of
phosphate removal during clarification, bear an important relationship to the
filtering qualities of the raw sugar produced. While on one hand it is desirable
to have a relatively high concentration of phosphate present in raw juice, the
presence of phosphate in raw sugar is considered to be undesirable. A com-
plication also arises by virtue of the fact that some phosphates are present in
cane juice in a form that does not favour their precipitation and subsequent
removal during clarification. These are commonly referred to as insoluble
phosphates, although the term "organically bound phosphate" is more
precise.
Soluble phosphate is determined after filtration of the undiluted
product at its existing pH value. The level of soluble phosphate in clarified
juice is of value as an index of the efficiency of juice clarification, but
the figure should always be examined in conjunction with the level of phos-
phate in unlimed juice, as a marked decline in the latter can result in an in-
crease in the residual phosphate present after clarification.
t h e presence of sugar in a sample. T h e a l p h a - n a p h t h o l test is n o t r e c o m m e n d e d

for c o n t r o l p u r p o s e s w h e n facilities a r e a v a i l a b l e for u s i n g t h e p h e n o l -
sulphuric acid method.
Procedure—Pipette 5 ml of c o o l e d s a m p l e i n t o a c l e a n t e s t t u b e a n d a d d
five d r o p s o f a l p h a - n a p h t h o l s o l u t i o n . S w i r l t o m i x . Carefully a d d 5 m l o f
concentrated sulphuric acid to t h e inclined test t u b e so t h a t t w o clearly
defined l i q u i d l a y e r s a r e f o r m e d .
I f s u c r o s e i s p r e s e n t , a v i o l e t r i n g will f o r m a t t h e j u n c t i o n o f t h e t w o
liquids a n d t h e intensity of t h e colour of this ring is an indication of t h e
q u a n t i t y of sucrose present. T h e test is extremely delicate in t h a t 1 p.p.m.
of s u c r o s e will g i v e a slight c o l o r a t i o n . An i n t e n s e b l a c k r i n g will f o r m at a
c o n c e n t r a t i o n of a p p r o x i m a t e l y 100 p . p . m .
Quality of Mill L i m e
T h e q u a l i t y of lime supplied to sugar factories is an i m p o r t a n t b u t often
n e g l e c t e d f a c t o r i n t h e j u i c e clarification p r o c e s s . A p a r t f r o m t h e e c o n o m i c
a s p e c t , t h e u s e of inferior q u a l i t y l i m e c a n i n t r o d u c e significant q u a n t i t i e s of
undesirable impurities into process. T h e composite sampling a n d analysis of
all i n c o m i n g l i m e c o n s i g n m e n t s a r e f a c t o r s w o r t h y o f s e r i o u s c o n s i d e r a t i o n .
T w o d e t e r m i n a t i o n s a r e r e q u i r e d t o assess t h e s u i t a b i l i t y o f a m i l l l i m e .
These are t h e Neutralising Value—expressed as per cent CaO, a n d Available
CaO.
Sampling Procedure—An i n i t i a l b u l k s a m p l e , r e p r e s e n t i n g a p p r o x i m a t e l y
one p o u n d per t o n of lime received, is s u b s a m p l e d d o w n to a p p r o x i m a t e l y
o n e p o u n d . T h i s i s t h e n g r o u n d i n a m o r t a r a n d p a s s e d t h r o u g h a n 0.5 m m
sieve. I t i s i m p o r t a n t t h a t t h i s o p e r a t i o n b e c a r r i e d o u t a s r a p i d l y a s possible
so t h a t recarbonation is kept to an absolute minimum.
Sample Preparation—Two o u n c e s of t h e s i e v e d m a t e r i a l a r e o v e n d r i e d
for four h o u r s a t 100 °C. T h e s a m p l e i s t h e n s t o r e d i n a s m a l l a i r t i g h t
container.
Neutralizing Value
T r a n s f e r an a c c u r a t e l y d e t e r m i n e d w e i g h t a p p r o x i m a t i n g 1 g of s a m p l e
t o a 600 m l E r l e n m e y e r flask a n d a d d 4 0 . 0 m l o f 1.00 N HC1. C o v e r t h e m o u t h
o f t h e flask w i t h a w a t c h glass a n d h e a t o n a s t e a m b a t h for 1 5 m i n u t e s .
Filter, a n d w a s h t h e residue w i t h h o t distilled w a t e r . Dilute t h e n i t r a t e a n d
t o t a l w a s h i n g s t o a v o l u m e o f 100 m l a n d b o i l v e r y g e n t l y for five m i n u t e s .
A l l o w t o cool i n a w a t e r b a t h . A d d five d r o p s o f p h e n o l p h t h a l e i n i n d i c a -
t o r a n d t i t r a t e t o t h e e n d p o i n t w i t h 1.00 N N a O H .
Calculation—
Neutralizing Value ml of 1.00 N HC1 u s e d X 2.80
( e x p r e s s e d as p e r c e n t CaO) = w e i g h t of s a m p l e
Available Calcium Oxide
T h e following m e t h o d i s p r e s e n t e d for o b t a i n i n g a n a p p r o x i m a t e e s t i m a -
t i o n o f t h e p e r c e n t a g e c a l c i u m o x i d e t h a t will c o m b i n e w i t h s u c r o s e t o f o r m
a soluble calcium saccharate. It is i m p o r t a n t t h a t t h e s a m e s t a n d a r d sucrose
b e u s e d for all t e s t s , a n d for t h e p u r p o s e o f u n i f o r m i t y , i t i s r e c o m m e n d e d
t h a t B . D . H . A . R . sucrose only be used.
Procedure—Transfer 1.60 g of s a m p l e to a d r y s t o p p e r e d 2 0 0 ml E r l e n -
m e y e r flask. A d d 2 . 0 m l o f e t h y l a l c o h o l t o p r e v e n t t h e f o r m a t i o n o f a g g l o m e r -
a t e s . T h e n a d d 100.0 m l o f 1 0 p e r c e n t s u c r o s e s o l u t i o n p r e p a r e d f r o m B . D . H .
A . R . sucrose, t o f o r m a soluble s a c c h a r a t e . Seal t h e flask a n d s h a k e for 3 0
minutes.
F i l t e r . D i s c a r d t h e first 5 ml of filtrate. A d d t h r e e d r o p s of m e t h y l o r a n g e
i n d i c a t o r to a 50 ml a l i q u o t of t h e n i t r a t e a n d t i t r a t e a g a i n s t 1.00 N HC1.
Calculation —
Caustic Cleaning Solution

Determination of Concentration
Care s h o u l d b e t a k e n t o e n s u r e t h a t t h e s a m p l e o f c l e a n i n g s o l u t i o n i s
r e p r e s e n t a t i v e of t h e c o n t e n t s of t h e h o l d i n g vessel. P a r t i c u l a r e m p h a s i s
s h o u l d b e p l a c e d o n t h i s p o i n t , especially after m o r e solid c a u s t i c s o d a h a s
been added to increase the concentration of t h e solution.
T h e determination of caustic strength by a straight acid/base titration
c a n give e r r o n e o u s r e s u l t s if significant a m o u n t s of s u l p h a t e a r e p r e s e n t . T h i s
interference can be overcome by precipitation of t h e sulphates w i t h b a r i u m
c h l o r i d e a n d r e m o v a l o f t h e p r e c i p i t a t e b y filtration.
Procedure—To 50 ml of t h e s a m p l e a d d 20 ml of 4 p e r c e n t W / V b a r i u m
c h l o r i d e s o l u t i o n . Mix a n d filter.
T i t r a t e a 25 ml a l i q u o t of t h e filtrate a g a i n s t 0.50 N h y d r o c h l o r i c a c i d ,
using m e t h y l red as an indicator.
P e r c e n t s o d i u m h y d r o x i d e = t i t r e x N of HCI x 0.224
N.B.—The s t r e n g t h o f t h e s t a n d a r d a c i d c a n b e v a r i e d t o s u i t t h e c a u s t i c
solution being analysed.
C.S.R. L a b o r a t o r y S e t t l i n g T e s t
T h e l a b o r a t o r y s e t t l i n g t e s t i s u s e d t o d e t e r m i n e t h e clarifying p r o p e r t i e s
of individual juices a n d to predict factory settling rates. T h e multiple testing
o f f a c t o r y m i x e d j u i c e s also p e r m i t s t h e e s t a b l i s h m e n t o f s t a n d a r d s t o
e v a l u a t e f a c t o r y p e r f o r m a n c e ( B u r g e s s et al., 1962).
Special Apparatus—The following e q u i p m e n t is required:-—
Juice Heating — H e c l a 4 5 0 w a t t A.C. p e r c o l a t o r p l u s a
1500 w a t t i m m e r s i o n h e a t e r .
Stirring Mechanism — Laboratory type stirrer operating at ap-
p r o x i m a t e l y 1200 r e v / m i n .
Lime Addition — A 10 ml g r a d u a t e d pipette w i t h approxi-
m a t e l y 1 i n c h of flexible t u b i n g a t t a c h e d
to the delivery end. A hypodermic syringe
m a y be used as a suitable substitute.
H e a t e d S e t t l i n g B a t h — A s p e r C.S.R. specifications.
Settling Tubes — T h e s e s h o u l d be 1.50 i n c h e s i n t e r n a l d i a -
meter, and graduated in volume per cent
o v e r a l e n g t h of 16 i n c h e s .
Lime Requirement—The l i m e r e q u i r e m e n t v a r i e s c o n s i d e r a b l y b e t w e e n in-
d i v i d u a l juices, b u t a n a p p r o x i m a t e e s t i m a t e o f t h i s q u a n t i t y c a n b e o b t a i n e d
i n t h e following m a n n e r : — S e t u p a s t i r r e r a n d p H e l e c t r o d e s i n a b e a k e r c o n -
taining 600 ml of t h e sample. Slowly a d d t h e lime sucrose solution (Chapter
V I I I ) from a b u r e t t e until t h e desired pH is obtained. This q u a n t i t y of lime
saccharate is then used in t h e actual settling test. A refinement to this

procedure is t h e use of a m a g n e t i c stirrer hotplate. This a p p a r a t u s reduces
t h e r i s k o f e l e c t r o d e d a m a g e a n d also p e r m i t s t h e d e t e r m i n a t i o n t o b e c a r r i e d
out at elevated temperatures.
Procedure—Subsample t w o 600 m l a l i q u o t s o f j u i c e . D e t e r m i n e t h e l i m e
requirement on one portion.
Transfer t h e remaining 600 ml of juice to t h e percolator in which t h e
stirrer has already been positioned, a n d h e a t rapidly to boiling using t h e
percolator element a n d the immersion heater. The time between sampling
a n d boiling should n o t exceed seven m i n u t e s .
A f t e r t h e j u i c e h a s b o i l e d for t w o m i n u t e s , t u r n t h e s t i r r e r o n a n d a d d
the predetermined a m o u n t of lime at a constant r a t e to t h e outer edge of t h e
rotating stirrer blade. T h e addition of lime should t a k e approximately 15
s e c o n d s . C o n t i n u e s t i r r i n g a n d h e a t i n g for a f u r t h e r 1 5 s e c o n d s .
T u r n t h e h e a t e r a n d s t i r r e r off a n d t r a n s f e r t h e j u i c e t o a p r e h e a t e d s e t t -
ling t u b e i m m e r s e d i n b o i l i n g w a t e r . Fill t h e t u b e t o t h e 100 p e r c e n t g r a d u a -
tion m a r k , stopper a n d commence timing of the settling test. Record per cent
m u d v o l u m e a g a i n s t t i m e a t o n e m i n u t e i n t e r v a l s for 1 5 m i n u t e s a n d t h e n a t
2 0 a n d 2 5 m i n u t e s . C o m p l e t e t h e t e s t a t 3 0 m i n u t e s a n d r e c o r d t h e final m u d
v o l u m e . A s a m p l e of clarified j u i c e is t h e n r e m o v e d , cooled a n d a n a l y s e d for
pH, tubidity and phosphate.
Calculation of Settling Area Requirement—Plot a s e t t l i n g c u r v e of p e r c e n t
m u d v o l u m e v e r s u s s e t t l i n g t i m e i n m i n u t e s . U s e a scale s u c h t h a t 1 0 p e r c e n t
i n m u d v o l u m e i s e q u i v a l e n t t o a t i m e i n t e r v a l o f five m i n u t e s .
T h e " c r i t i c a l p o i n t " i.e. t h e p o i n t o f m i n i m u m f l u x , i s l o c a t e d b y t h e
following m e t h o d a s s h o w n i n F i g . 4 3 .
Determine underflow concentration h by the equation
a n d d r a w a h o r i z o n t a l line a t t h e u n d e r f l o w c o n c e n t r a t i o n level.
P r o d u c e t h e i n i t i a l s t r a i g h t line
s e c t i o n (free s e t t l i n g zone) of t h e
c u r v e t o c u t t h e u n d e r f l o w h line a t
point A. Bisect t h e outer angle
f o r m e d b y t h e e x t e n d e d free s e t t l i n g
line a t t h e i n t e r c e p t o n t h e h
line.
D r a w a line p e r p e n d i c u l a r t o
this bisector a n d tangential to t h e
settling curve. Produce this t a n g e n t
t o c u t t h e h line a t p o i n t C . R e a d off
the time corresponding to point C.
Designate this time as T.
The unit settling area require-
m e n t of the juice tested is t h e n given
by the equation:—
U n i t A r e a = 0.002 x T
square foot/gallon juice
/hour
It should be noted that this formula applies only to settling tubes of

the dimensions previously stated.
This unit area has been used to calculate the area required in factory
clarifiers by multiplying the unit area by the factory mixed juice flow, ex-
pressed in gallons per hour. However, while the concept has been a valuable
guide in the past, with the present extensive use of flocculating agents and
the consequent increase in settling rates obtained with these additives, the
areas predicted from this test must now be considered with a good deal of
reserve. The advent of flocculating agents has, however, introduced a further
use for this settling test as it enables the performance of various flocculants
to be compared under laboratory and factory conditions.
Due to variations in juice composition, and slight differences in test
procedure, a single test is of limited value, and the average of a number of
tests is required to provide a valid comparison with factory results.
As explained in Chapter I, a cyclone sample is a sample of the mother
liquid extracted from a massecuite. For the separation process the laboratory
Cyclone Sampling and Supersaturation
Fig. 44—Illustrating a pressure filter for separation of molasses from massecuite.

b a s k e t t y p e fugal w a s f o r m e r l y r e c o m m e n d e d . T h e u s e o f a fugal h a s t h e
d i s a d v a n t a g e t h a t a significant p r o p o r t i o n o f w a t e r i s e v a p o r a t e d f r o m t h e
m o l a s s e s i n t h e s e p a r a t i o n p r o c e s s . T h i s d o e s n o t influence p u r i t y o f t h e
m o l a s s e s b u t i t d o e s a l t e r t h e s u c r o s e a n d t o t a l solids c o n c e n t r a t i o n s . S u c t i o n
filters h a v e b e e n u s e d for t h e s e p a r a t i o n , b u t t h e s e d i s p l a y t h e s a m e d i s -
advantages.
T h e r e c o m m e n d e d d e v i c e for s e p a r a t i o n of c y c l o n e s a m p l e s is a p r e s s u r e
filter, of w h i c h o n e e x a m p l e is i l l u s t r a t e d in F i g u r e 4 4 . It c o n s i s t s s i m p l y of a
w a t e r j a c k e t e d p r e s s u r e vessel w i t h r e m o v a b l e t o p a n d b o t t o m c o v e r s . T h e
b o t t o m plate is provided with drainage channels leading to a central hole
a n d supports a screen on which t h e a c t u a l filtration is achieved. W h e n masse-
c u i t e i s p l a c e d i n t h e s e a l e d vessel a n d air p r e s s u r e a p p l i e d a t t h e t o p , t h e
m o l a s s e s i s forced o u t t h r o u g h t h e s c r e e n . E x c e p t i n t h e m o s t difficult cases,
t h e s e p a r a t i o n i s a c c o m p l i s h e d i n a few m i n u t e s a n d t h e c o m p o s i t i o n o f t h e
m o t h e r l i q u o r i s n o t a d v e r s e l y affected i n t h e p r o c e s s . C a r e m u s t b e t a k e n ,
however, to ensure t h a t the separation is carried out at t h e t e m p e r a t u r e of
s a m p l i n g o f t h e m a s s e c u i t e a n d t h e first 5 t o 1 0 m l o f s a m p l e s h o u l d b e
rejected.
Supersaturation
T h e d e t e r m i n a t i o n of t h e d e g r e e of s u p e r s a t u r a t i o n of m o l a s s e s is of
considerable i m p o r t a n c e in t h e s t u d y of p a n boiling a n d crystallization. T h e
e x p l a n a t i o n of t h e t h e o r y a s s o c i a t e d w i t h t h e d e t e r m i n a t i o n of coefficient of
s u p e r s a t u r a t i o n i n v o l v e s t h e u s e o f t e r m s w h i c h a r e defined a s f o l l o w s : —
(a) C o n c e n t r a t i o n . T h e p e r c e n t a g e r a t i o b y w e i g h t o f s o l u t e t o s o l v e n t
(unless o t h e r w i s e s t a t e d ) .
(b) S a t u r a t i o n . T h a t c o n d i t i o n i n w h i c h t h e q u a n t i t y o f s o l u t e d i s s o l v e d
in a solvent is t h e m a x i m u m which can be contained in stable equilibrium.
(c) S o l u b i l i t y . T h e c o n c e n t r a t i o n of s o l u t e in t h e s o l v e n t g i v i n g a c o n d i -
t i o n of s a t u r a t i o n . S o l u b i l i t y is r e s p o n s i v e to v a r i o u s influences, of w h i c h
t e m p e r a t u r e a n d t h e presence of other solutes in t h e solvent are i m p o r t a n t
in the present connection.
(d) S o l u b i l i t y Coefficient. T h e r a t i o of t h e s o l u b i l i t y of s u c r o s e in t h e
impure w a t e r of t h e sample to t h e solubility of sucrose in p u r e w a t e r at the
same t e m p e r a t u r e . Some impurities raise t h e solubility of sucrose in water,
o t h e r s lower it. T h e c o m b i n e d effect o f t h e i m p u r i t i e s p r e s e n t i n c a n e m o l a s s e s
is usually to lower t h e solubility of sucrose.
(e) Coefficient of S u p e r s a t u r a t i o n . T h e r a t i o of t h e a c t u a l c o n c e n t r a t i o n
of s u c r o s e p r e s e n t in a s a m p l e to t h e s o l u b i l i t y of s u c r o s e in t h e w a t e r of t h e
sample at the same temperature. Supersaturation is an unstable condition;
though, in practice, the tendency to revert to the equilibrium condition is
s o m e t i m e s v e r y feeble.
T h e m e t h o d of d e t e r m i n a t i o n of t h e coefficient of s u p e r s a t u r a t i o n , d e -
vised by H a r m a n , is based on t h e fact t h a t , if a s u p e r s a t u r a t e d solution is
h e a t e d , t h e s u p e r s a t u r a t i o n coefficient will fall, d u e t o t h e rise i n t h e s o l u b i l i t y
o f s u c r o s e w i t h t e m p e r a t u r e . A t s o m e t e m p e r a t u r e t h e s o l u t i o n will b e c o m e
s a t u r a t e d , a n d i f t h i s t e m p e r a t u r e i s e x c e e d e d , u n d e r s a t u r a t i o n will r e s u l t .
A n y c r y s t a l s o f s u c r o s e p r e s e n t i n t h e s o l u t i o n will t h e n c o m m e n c e t o d i s -
solve, a p h e n o m e n o n w h i c h m a y b e o b s e r v e d v i s u a l l y u n d e r s u i t a b l e
conditions.
For a p u r e solution of sucrose in water, s u p e r s a t u r a t e d at t e m p e r a t u r e t1

and found to be saturated at temperature t2 it m a y be claimed t h a t t h e
c o n c e n t r a t i o n o f s u c r o s e a c t u a l l y p r e s e n t i s t h a t c o r r e s p o n d i n g t o t h e solubil-
i t y of s u c r o s e at t2. T h e c o n c e n t r a t i o n of s u c r o s e r e q u i r e d to give a s a t u r a t e d
s o l u t i o n a t t 1 i s t h e s o l u b i l i t y a t t 1 . B o t h s o l u b i l i t y figures m a y b e a s c e r t a i n e d
for s e l e c t e d t e m p e r a t u r e s f r o m t a b l e s s u c h a s t h a t o f Charles (Table X I I I ) .
T h e n if S be t h e coefficient of s u p e r s a t u r a t i o n at t e m p e r a t u r e t 1
F o r i m p u r e solutions, t h e solubility of sucrose is altered due to t h e

presence of t h e impurities, and, at saturation, t h e actual concentration of
s u c r o s e will b e e q u a l t o t h e s o l u b i l i t y o f s u c r o s e i n p u r e w a t e r m u l t i p l i e d b y
t h e s o l u b i l i t y coefficient.
If k 1 is t h e s o l u b i l i t y coefficient at t 1 a n d k 2 t h e s o l u b i l i t y coefficient of
the same sample at t2 t h e n
H a r m a n points out t h a t , over t h e range of temperatures involved, k1

m a y b e t a k e n e q u a l t o k 2 w i t h o u t a p p r e c i a b l e e r r o r . H e n c e for i m p u r e solu-
t i o n s also
w h e r e s o l u b i l i t y is t h a t of s u c r o s e in w a t e r , i.e. g s u c r o s e p e r 100 g of w a t e r
(Table X I I I ) .
T h e s t a t e m e n t t h a t k 1 m a y b e t a k e n e q u a l t o k 2 c a n g i v e rise t o v e r y
serious e r r o r s i n s o m e cases.
W h e n c o r r e c t i o n s a r e m a d e for c h a n g i n g s o l u b i l i t y coefficient i t s h o u l d
b e n o t e d t h a t t h i s definition m u s t b e s t a t e d a s b e i n g for c o n s t a n t p u r i t y . I n
practice a solution when crystallized does not remain at constant purity, a n d
a m o r e f u n d a m e n t a l v a l u e of coefficient of s u p e r s a t u r a t i o n is o b t a i n e d by
e x p r e s s i n g it as
N o g a i n o r loss o f w a t e r i s a l l o w e d d u r i n g t h e c r y s t a l l i z a t i o n a n d s o t h i s
definition i m p l i e s a c o n s t a n t i m p u r i t i e s / w a t e r r a t i o .
Special Apparatus—In t h e d e t e r m i n a t i o n of s a t u r a t i o n t e m p e r a t u r e , a
" s a t u r a t i o n cell" is used. T h e t y p e favoured, as shown in Fig. 45, consists of a
s h a l l o w c y l i n d r i c a l cell of b a k e l i t e or similar m a t e r i a l . I n s i d e t h e cell is
mounted a metal table which supports the sample and accommodates a
t h e r m o m e t e r b u l b . A r o u n d t h e i n t e r n a l p e r i p h e r y o f t h e cell a n electric
h e a t i n g e l e m e n t is m o u n t e d . A glass w i n d o w in t h e b o t t o m of t h e cell a n d a
h o l e i n t h e c e n t r e o f t h e t a b l e a l l o w l i g h t t o p a s s u p t h r o u g h t h e cell.
T h e cell i s set o n a m i c r o s c o p e s t a g e , t h e t h e r m o m e t e r i n s e r t e d , t h e s a m -
p l e m o u n t e d o v e r t h e h o l e i n t h e t a b l e , a n d t h e cell c o v e r e d w i t h a s h e e t o f
clear glass. T h e s a m p l e , a s m a l l d r o p of m o l a s s e s , is m o u n t e d on a s m a l l
s q u a r e o f m i c r o s c o p e slide glass. I f n o t i n y c r y s t a l s a r e likely t o b e p r e s e n t ,
a l i t t l e finely g r o u n d s u g a r is s p r i n k l e d o v e r t h e s a m p l e a n d a t h i n c o v e r slip
is then placed over t h e sample a n d pressed down to give a t h i n film. T h e
m i c r o s c o p e i s t h e n focused o n t h e s a m p l e . ( A c o m b i n a t i o n o f 1 6 m m (2/3
inch) objective and a X25 eyepiece has been found to be very satisfactory).
The field is moved until several small sharp edged crystals are in view.
Procedure—The electric heater is turned on, and adjusted so that the
temperature rises about 3 °C per minute. Eventually erosion of the crystals
will be observed, and at the first sign of this, the temperature should be noted.
The experiment should then be repeated with the temperature rising
more slowly—about 0.5 °C per minute—in the vicinity of the critical temper-
ature noted earlier.
Hints on the Determination—Materials of high purity crystallize quickly

and excessive chilling may even lead to spontaneous crystal formation which
would spoil the sample. Such materials must be handled quickly, and before
the determination is commenced, the cell should be heated to within a few
degrees of the probable saturation temperature.
A sample of molasses may be separated from a massecuite by enclosing
a small ball of the massecuite in a pocket of a piece of cloth, and squeezing.
If the cloth is of fairly open texture, sufficient fine crystals for observation
purposes will nearly always be found in the sample. More satisfactory results
appear to be achieved with crystals originally present in the sample.
The observation is tedious and exacting. The use of a red filter improves
the ease of observation; polarized light is even better. Several crystals should
be studied in rotation, as there appears to be no means of predicting where
the erosion will first be noticed. Beware of a false end point; always maintain
the heating until erosion is obviously well advanced, thus verifying the
suspected onset of erosion.
The saturation cell may be checked for accuracy of temperature reading
by using it as a melting point apparatus for various pure chemicals, the actual
melting points of which may be established by a recognized method.
Boiler Water Analysis
The various constituents in both natural and make-up water can result
in severe scale formation, boiler corrosion and carry-over unless an effective
method of chemical treatment is adopted. Some of the common scale forming
constituents encountered in sugar factories are silica, calcium and mag-
nesium, oil and residues from the thermal degradation of sugars. These
deposits are undesirable because of their adverse effect on heat transfer, and
because their presence can lead to localised overheating of the metal with
consequent failure and risk of explosion. Corrosion is due to acid conditions
in the boiler or the presence of dissolved oxygen. The prevention of carry-over
by strict control on the level of total dissolved solids is also essential to prevent
damage to the equipment in which steam is utilized.
A detailed discussion on the application of recommended systems and
methods of boiler water treatment is contained in Chapter X I I . Chapter X I I
also permits the analyst to obtain an understanding of the functions of the
various chemicals added for effective water treatment and it is suggested
that the analyst should become familiar with its contents. The following
simple methods of analysis, most of which are extracted from the relevant
British Standard, are suitable for routine control of the boiler station. More
sophisticated methods of analysis are available in some cases, and if the
apparatus is available, these methods may be used at the discretion of the
analyst.
Alkalinity
Three different types of alkalinity determinations are carried out on
boiler waters. These are
(a) Alkalinity to phenolphthalein, end point at pH 8.3
(b) Alkalinity to methyl orange, end point at pH 4.5
(c) Alkalinity to phenolphthalein after barium chloride addition.
If organic matter is present in the sample, the alkalinity to methyl
orange is unreliable, and determination of alkalinity to phenolphthalein, both
before and after the addition of barium chloride, is carried out. Barium
chloride addition also corrects for the presence of any residual trisodium
phosphate which would register as alkalinity, unless precipitated.
Procedure (a) Alkalinity to Phenolphthalein (P)
Measure 100 ml of the sample and transfer to a white porcelain basin.
Add 1 ml of phenolphthalein indicator. A pink colour will form if the solution
is alkaline to phenolphthalein.
Titrate with 0.02 N sulphuric acid until the pink colour just disappears.
Retain the solution for procedure (b)
Alkalinity to phenolphthalein (P) =
Procedure (b) Alkalinity to Methyl Orange (M)

To the solution treated as described above, add 3 drops of methyl orange
indicator. Titrate slowly with 0.02 N sulphuric acid, while stirring continu-
ously, until the solution shows the first colour change from yellow to orange.
Record the total number of ml of acid used, i.e. including those used in
the previous titration with phenolphthalein.
Alkalinity to methyl orange (M) =
If the solution is so highly coloured that the indicator end points cannot
be detected, a pH meter may be used. When this procedure is adopted, the
i n d i c a t o r s o l u t i o n i s n o t a d d e d a n d t h e t i t r a t i o n v a l u e s a t p H 8.3 a n d p H 4.5
a r e r e c o r d e d for p h e n o l p h t h a l e i n a n d m e t h y l o r a n g e r e s p e c t i v e l y .
Procedure (c) Alkalinity to Phenolphthalein after Barium Chloride addition
T h e p r o c e d u r e for t h e n o r m a l i n d i c a t o r t i t r a t i o n i s a s f o l l o w s : —
M e a s u r e 100 m l o f s a m p l e a n d t r a n s f e r t o a w h i t e p o r c e l a i n b a s i n . A d d 1 m l
of p h e n o l p h t h a l e i n i n d i c a t o r , followed by a c r y s t a l of s o d i u m s u l p h a t e a n d
1 0 m l o f 1 0 p e r c e n t b a r i u m c h l o r i d e s o l u t i o n . S t i r well for t w o m i n u t e s a n d
t h e n t i t r a t e w i t h 0.02 N s u l p h u r i c a c i d u n t i l t h e p i n k c o l o u r j u s t d i s a p p e a r s .
Disregard a n y r e a p p e a r a n c e s of t h e p i n k colour.
Alkalinity to phenolphthalein after b a r i u m chloride addition
Phosphate
S e v e r a l m e t h o d s a r e a v a i l a b l e for t h e d e t e r m i n a t i o n o f p h o s p h a t e i n
boiler w a t e r s . T h e m a j o r i t y of t h e s e a r e b a s e d on t h e f o r m a t i o n of a b l u e
phospo-molybdate complex, t h e intensity of which is directly proportional
t o t h e a m o u n t o f P 0 4 ion p r e s e n t i n t h e s o l u t i o n . F o r r o u t i n e c o n t r o l w o r k ,
the chemist a n d engineer need only to k n o w t h a t a reserve of p h o s p h a t e is
p r e s e n t a n d t h a t t h e level i s w i t h i n a c e r t a i n r a n g e . T h i s p e r m i t s a r e d u c t i o n
in t h e time spent on carrying out t h e determination. T h e colour formed after
reagent addition is compared either in a L o v i b o n d t y p e c o m p a r a t o r or against
s t a n d a r d c o l o u r p l a t e s . A s u i t a b l e e x a m p l e of p h o s p h a t e c o l o u r p l a t e s is
shown on p a g e 49 of British S t a n d a r d s 1170:1957. A s p e c t r o p h o t o m e t e r
m a y be used, if available.
Apparatus—Two t e s t t u b e s a p p r o x i m a t e l y 6 i n c h e s in l e n g t h a n d half an
inch in diameter. T w o 250 ml bottles, each fitted with a r u b b e r t e a t p i p e t t e
g r a d u a t e d at a 2 ml d i s c h a r g e level. U s e o n e b o t t l e for d i s p e n s i n g a c i d
m o l y b d a t e a n d t h e o t h e r for c a r b o n a t e - s u l p h i t e . O n e 250 m l b o t t l e f i t t e d
w i t h a r u b b e r t e a t p i p e t t e g r a d u a t e d at a 1 ml d i s c h a r g e level for d i s p e n s i n g
h y d r o q u i n o n e . W h a t m a n N o . 5 filter p a p e r s .
Procedure—The t e m p e r a t u r e o f t h e s a m p l e a n d r e a g e n t s m u s t b e k e p t
b e t w e e n 2 0 a n d 3 0 °C.
F i l t e r a s a m p l e o f t h e cooled boiler w a t e r t h r o u g h t w o W h a t m a n N o . 5
filter p a p e r s . D i s c a r d t h e first 10 ml a n d refilter t h e e x t r a c t if a clear l i q u i d
i s n o t o b t a i n e d f r o m t h e first f i l t r a t i o n .
T r a n s f e r 5 ml of t h e s a m p l e to a t e s t t u b e , a d d 2 ml of a c i d m o l y b d a t e
and mix thoroughly. Then a d d 1 ml of hydroquinone and again mix thorough-
ly. Allow t h e c o n t e n t s o f t h e t u b e t o s t a n d for 5 m i n u t e s .
A d d 2 m l o f c a r b o n a t e - s u l p h i t e s o l u t i o n t o t h e o t h e r t e s t t u b e . Carefully
pour the contents of the first t u b e into the one containing the carbonate-
sulphite solution. Mix by cautiously transferring several times t h e contents
from one t u b e to t h e other.
Hold t h e test t u b e containing t h e sample a little distance a w a y from t h e
side of t h e s t a n d a r d colour plates, a n d e s t i m a t e t h e P 0 4 level in t h e solution.
It is advisable to use a t u n g s t e n filament l a m p when m a k i n g t h e comparison
a s i t i s n o t possible t o o b t a i n a g o o d c o m p a r i s o n b y d a y l i g h t o r fluorescent
light.
Interpretation of Results—A P 0 4 level b e t w e e n 30 a n d 70 p . p . m . is
usually considered to be satisfactory. Results are usually recorded as "low",
"satisfactory" or "high".
Sulphite
The presence of free sodium sulphite in a boiler water is an assurance
that all dissolved oxygen in the feed water has been eliminated. Special
attention must be given to the method of sampling for this determination,
as sulphite can be rapidly destroyed when the sample is exposed to atmos-
phere. This is more pronounced at elevated temperatures, but the effect can
be minimized if the following sampling procedure is carried out:—
A stainless steel or nickel-copper cooling coil which will reduce the outlet
temperature to below 30 °C is required. Position the outlet tube into the
bottom of the sample container, and allow water to flow until at least five
changes have occurred. Withdraw the outlet tube slowly so that the container
is filled to maximum capacity, and stopper with an effective sealing device.
Analyse the sample as soon as possible.
Procedure—Transfer 4 ml of 6.5 per cent V/V sulphuric acid to a white
porcelain basin. Add 100 ml of unfiltered boiler water sample and 1 ml of
starch indicator.
Titrate with potassium iodide-iodate solution and stir continuously
during the titration until a faint permanent blue colour is obtained.
Hardness
Refined methods are available for the determination of hardness in
boiler waters. The majority of these are time consuming, and for ordinary
routine control purposes sufficient accuracy can be obtained by titrating a
known volume of sample with standard soap solution. During this titration,
the soap combines with calcium and magnesium salts in the water until they
are precipitated as an insoluble curd, and when all these salts have been
converted, the addition of an extra drop of soap solution will produce a
permanent soap lather. Thus, the soap solution provides its own indicator,
and the formation of this permanent lather corresponds to the point where
colour changes occur when indicators are used for the more refined methods
of hardness determination.
Standardization of Soap Solution—Each batch of Wanklyn's reagent
should be checked by titrating the reagent against 100 ml of distilled water.
The amount of soap solution required to establish a permanent lather with
distilled water is then regarded as the blank, and is subtracted from all other
titrations carried out with that particular batch of reagent.
Procedure—Measure out 100 ml of filtered boiler water sample and
transfer into a glass stoppered bottle of approximately 250 ml capacity.
Titrate with Wanklyn's soap solution from a burette, 0.2 ml at a time,
replacing the stopper and shaking after each addition. Continue additions
until a permanent lather, i.e. one that remains at least 5 minutes, is obtained.
It is not necessary to wait 5 minutes between additions, as the immediate
breakdown of individual bubbles is an indication that the lather will not be
permanent. View the lather by laying the bottle on its side at eye level. It
will be noted that the lather rapidly becomes more permanent as the end
point is approached and additions of the reagent should then be made in
smaller quantities.
For a 100 ml sample aliquot,
Total Dissolved Solids

These may be determined either gravimetrically by weighing after dry-
ing, conductometrically, or by the determination of specific gravity using a
special hydrometer of the type supplied with "Alfloc" testing equipment.
The last method is recommended for routine control determinations because
of the simplicity of the technique.
Two factors which must receive special attention in the determination
of T.D.S. by the hydrometer are, firstly, that special care is required when
handling and cleaning the hydrometer, and, secondly, that the hydrometer
must be restandardized against the gravimetric method at regular intervals
to ensure its reliability.
Effect of Temperature—Changes in temperature during the determination
and a temperature difference between the instrument and surrounding solu-
tion can result in considerable discrepancies in the values determined. The
analyst must therefore ensure that sufficient time is allowed for each sample
to cool to near room temperature, and also for the hydrometer to attain the
temperature of the solution. The temperature corrections to be applied
to the standard 80 °F type hydrometer are listed in the following table.
—• Temperature Corrections—80 °F Type Hydrometer
Correction to Correction to Correction t o

Temp. observed reading Temp. observed reading Temp. observed reading
°F (divisions °F (divisions) °F (divisions)
44 Subtract 26 64 Subtract 19 84 Add 5

46 26 66 17 86 8
48 26 68 15 88 11
50 26 70 13 90 14
52 26 72 10.5 92 18
54 25.5 74 8 94 22
56 24.5 76 5.5 96 26
58 23.5 78 3 98 30
60 22.5 80 "Nil 100 34
62 21 82 Add 2
Procedure—Pour in a sufficient quantity of boiler water sample to fill the

hydrometer jar to approximately one inch from the top. Add six drops of
wetting agent and mix into the solution.
Lower the hydrometer carefully into the solution. If air bubbles are
observed to be adhering to the instrument, these can usually be removed
by gently spinning the hydrometer. Record the temperature of the solution
to the nearest °F.
Read the hydrometer scale by looking slightly down on the surface of
the liquid. Correct the scale reading for temperature by reference to the above
table.
Multiply the corrected reading by 100 and record as p.p.m. Total Dis-
solved Solids.
Sulphate
Sulphate is precipitated as barium sulphate by the addition of a known
amount of barium chloride to the acidified solution. The excess barium chlor-
ide is then determined by titrating against EDTA, using either solochrome
or eriochrome black as an indicator.
The test for sulphate is not applicable to waters containing appreciable

amounts of calcium and magnesium salts as these also react with EDTA.
The test is generally applicable to boiler waters with a hardness value below
20 p.p.m. CaC0 3 . In these circumstances the errors caused by hardness salts
can be ignored.
Procedure—Pipette 10 ml of the sample into a porcelain basin and
acidify with 1 ml of 0.5 N hydrochloric acid. Add exactly 10 ml of 0.04 N
barium chloride solution from a suitable automatic dispenser.
Pipette into a small beaker 3 ml of the sulphate buffer and add to it
0.2 g of solochrome black indicator. Mix well and pour into the basin con-
taining the sample.
Slowly titrate the contents of the basin with 0.02 N EDTA, stirring the
sample with a glass rod until the colour begins to change to purple. Then add
the EDTA solution, drop by drop, stirring continuously until all traces of red
colour have disappeared. The final colour at the end point is usually blue,
but with some waters a greyish coloured end point is obtained.
Water Analysis
Chlorides
Chloride is determined by titrating a neutral or slightly alkaline solution
against a standard silver nitrate solution in the presence of chromate indica-
tor. White silver chloride is precipitated, followed by reddish silver chromate
when the chloride end point has been reached. The presence of sulphites in
some waters can cause considerable interference to this determination. This
effect may be overcome by the addition of 1 ml of hydrogen peroxide (10 vol.)
prior to the commencement of the titration.
Procedure—Pipette 50 ml of sample into a white porcelain basin. Add
1 ml of potassium chromate indicator and commence titrating with
silver nitrate solution. Stir continuously with a rubber-tipped glass
stirring rod and continue the titration until the first permanent reddish colour
change is established. Record the volume of silver nitrate used.
Chloride = titre x 20 as p.p.m. CI.
REFERENCES
Aldrich, B. I. and Rayner, P. C, (1962), Cell-Breakage Determination in Prepared
Cane and Bagasse. Proc. I.S.S.C.T., eleventh Conf., 1004-1013.
Anderson, G. A. and Petersen, K. J., (1959), Operation of an Individual Fibre System.
Proc. Q.S.S.C.T., twenty-sixth Conf., 15.
B u r g e s s , I. G., Beardmore, R. H., Fortescue, G. E„ and Davis, G. W. (1962),
Development and Application of a Laboratory Clarification Test. Proc.
I.S.S.C.T. eleventh Conf., 920-927.
Deicke, R. (1959), Investigations with the Wet Disintegrator for Direct Analysis of
Cane. Proc. I.S.S.C.T. tenth Conf., 168-174.
De Whalley, H. C. S. (Editor) (1964), ICUMSA Methods of Sugar Analysis, Elsevier,
41-44.
Foster, D. second H., (1955),
Conf.,The Determination of Pol in Bagasse, Proc. Q.S.S.C.T., twenty
279-283.
CHAPTER X
THE DETERMINATION OF pH
Hydrogen Ion Concentration
Pure water exhibits a very high resistance to the passage of an electric
current, but its conductivity is markedly increased when substances known
as electrolytes are dissolved in it; electrolytes include all acids, bases and salts,
whereas substances such as sugars, alcohols and ketones are without influence
on the conductivity of the solution and are known as non-electrolytes. An
attempt to explain the effect of electrolytes led Arrhenius in 1887 to pro-
pound his Electrolytic Dissociation Theory. He postulated that when an
electrolyte is dissolved in water, some of the molecules of the substance dis-
sociate into electrically charged particles, which are known as ions. Thus a
molecule of hydrochloric acid gives in solution a positively charged hydrogen
ion H+, and a negatively charged chlorine ion Cl~. In all cases, the sum of
ionic charges must be zero, for the molecule is electrically neutral.
The molecules of all electrolytes are not dissociated to the same degree.
For example, a normal solution of hydrochloric acid is dissociated to the
extent of 80 per cent, while a solution of acetic acid of similar concentration
possesses but 0.43 per cent of its molecules in the ionised form. Electrolytes
which are highly dissociated in solution are known as strong electrolytes,
while those which are but slightly dissociated are called weak electrolytes.
The degree of dissociation is a function of the concentration of the solution;
the more dilute the solution the higher the percentage of dissociation.
Pure water does conduct an electric current in a feeble degree, and is
therefore itself a weak electrolyte. The equation for the electrolytic dis-
sociation of water may be represented:—
Since the degree of dissociation of water is so low, no appreciable error

will be introduced if the concentration of undissociated molecules be regarded
as constant, and therefore
[H+] [OH-] = K [HOH] = Kw
where Kw is known as the Dissociation Constant of Water.
Careful measurements have demonstrated that at 22 °C, pure water
possesses a concentration of hydrogen ions equal to 10 -7 gramme ions per litre.
It contains also a similar ionic concentration of hydroxyl ions. Thus at 22 °C
the dissociation constant of water is equal to 10 - 7 x 10 -7 or 10 -14 . It should
be observed, also, that in dilute aqueous solution the product of the concentrations
of H+ and O H - is for practical purposes a constant at constant temperature,
and equals 10 -14 at 22 °C.
As the concentration of hydrogen ions often has a very low value, in
order to avoid the nuisance of writing a long decimal expression to describe it,
it has been found useful to use an exponential notation. The term pH, first
proposed by Sorensen in 1909, is widely used today. It is defined as the
negative exponent of 10 which gives the hydrogen ion concentration.
T H E DETERMINATION OF pH 145
Thus,
F o r p u r e w a t e r a t 2 2 °C, [H+] e q u a l s 1 0 - 7 g r a m m e s p e r l i t r e , t h e r e f o r e t h e
p H is 7.
A n acid s o l u t i o n m a y b e defined a s o n e i n w h i c h t h e c o n c e n t r a t i o n o f
the H+ exceeds t h a t of O H - ; a n d conversely, an alkaline solution is one
w h i c h possesses an excess of O H - o v e r H + . A solution of pH 7.0 is, t h e r e f o r e ,
r e g a r d e d a s a n e u t r a l s o l u t i o n ; p H v a l u e s less t h a n 7.0 i n d i c a t e a n a c i d solu-
t i o n , while v a l u e s a b o v e 7.0 a r e c h a r a c t e r i s t i c of a l k a l i n e s o l u t i o n s . In
employing this convention, it must be remembered always t h a t pH is a
logarithmic f u n c t i o n ; a n d t h e r e f o r e a s o l u t i o n of pH 6.0 h a s a H+ c o n c e n t r a -
t i o n t e n t i m e s t h a t of a solution of pH 7.0.
I t will b e o b s e r v e d t h a t t h e v a l u e o f p H for w a t e r a t 2 2 ° C i s 7.0. T h i s
v a l u e does v a r y w i t h t h e t e m p e r a t u r e i n q u i t e a m a r k e d degree, a s i s s h o w n
by t h e following t a b l e for p u r e w a t e r : —
Temperature °C pH
16 7.10
20 7.03
22 7.00
25 6.95
40 6.71
100 6.12
The importance of temperature control must be borne in mind in carrying
o u t all p H d e t e r m i n a t i o n s ; s t r i c t l y t h e s e s h o u l d b e m a d e a t a c o n s t a n t
t e m p e r a t u r e , so as to be comparable with one another.
Measurement of pH
Two general m e t h o d s are employed in t h e determination of p H , the
c o l o r i m e t r i c m e t h o d a n d t h e e l e c t r o m e t r i c m e t h o d . E a c h possesses i t s
advantages and disadvantages; the latter requires a pH meter a n d is more
a c c u r a t e , while t h e former r e q u i r e s less s o p h i s t i c a t e d a p p a r a t u s .
Colorimetric method
C e r t a i n c h e m i c a l c o m p o u n d s h a v e t h e a b i l i t y t o c h a n g e colour w h e n t h e
p H o f t h e solution, i n w h i c h t h e y a r e dissolved, c h a n g e s o v e r c e r t a i n r a n g e s .
These compounds are known as indicators. Ostwald explained this ability to
c h a n g e colour b y a s s u m i n g t h a t c o m p o u n d s o f t h i s n a t u r e b e h a v e a s w e a k
acids or b a s e s , t h e m o l e c u l e s of w h i c h a r e a b l e to a b s o r b light of a definite
s p e c t r a l r a n g e , w h i l e t h e i r ions h a v e t h e a b i l i t y of a b s o r b i n g light of a n o t h e r
s p e c t r a l b a n d . A n a c i d i n d i c a t o r a t l o w p H v a l u e s will e x h i b i t t h e colour
c h a r a c t e r i s t i c s of t h e u n d i s s o c i a t e d molecules, w h i l e t h e n e u t r a l i z a t i o n of t h e
a c i d by t h e a d d i t i o n of a b a s e r e s u l t s in t h e p r o d u c t i o n of a h i g h l y d i s s o c i a t e d
s a l t (since all s a l t s a r e h i g h l y dissociated) a n d t h e s o l u t i o n e x h i b i t s t h e c o l o u r
o f t h e ions. I n d i c a t o r s a r e u s u a l l y utilized i n t h e m e a s u r e m e n t o f t h e p H o f
s o l u t i o n s by m e a n s of t e s t p a p e r s or a colour c o m p a r a t o r .
Test papers: T h e r e a r e n u m e r o u s different t y p e s of t e s t p a p e r s a v a i l a b l e
c o m m e r c i a l l y for t h e e s t i m a t i o n o f p H . " U n i v e r s a l " t e s t p a p e r s c o v e r t h e
r a n g e 1.0 t o 11.0 p H i n s t e p s o f 1.0 p H ; t h e c o l o u r c h a n g e c h a r t for t h e s e
p a p e r s i s p r i n t e d o n t h e inside o f t h e c o v e r . A n o t h e r useful t y p e for s u g a r
mill application is t h e " H y d r i o n " short range pH test paper covering t h e
r a n g e 6.0 t o 8.0 i n half u n i t s t e p s . T h e s e t e s t p a p e r s a r e p o r t a b l e a n d s p e e d y ,
but not extremely accurate.
146 T H E DETERMINATION OF pH
Comparator: The Lovibond or Hellige comparator comprises a plastic

housing into which can be fitted a disc of permanent colour standards to-
gether with two glass containers, one for the specimen under test and the
other for a blank (to compensate for inherent colour in the sample).
Each particular test requires the use of the appropriate disc which
contains a number of permanent glass colour standards (usually nine) re-
presenting the range of colours produced by different concentrations of the
material which is the subject of the test. The discs for pH determinations are
usually supplied complete with the appropriate indicator. A useful disc for
sugar mill work is the Bromothymol blue disc, containing nine steps of 0.2 pH
over the range 6.0 to 7.6. The comparator can only be used for fairly clear
solutions. It is slower than the test papers but more accurate.
Electrometric method
Electrometric methods are based upon the principle of measuring the
electromotive force generated, as a function of the hydrogen ion concentra-
tion (and temperature), between electrodes of various types immersed in a
solution to be tested and in a solution of known and definite characteristics
joined thereto by a liquid junction. The standard and classical electrometric
method employs the hydrogen electrode and while, because of the many
difficulties involved in its use, the hydrogen electrode has found no direct
application in the sugar industry, an understanding of its operation is useful
to give a clear picture of the method.
Hydrogen electrode: The hydrogen electrode consists of a platinum or
gold foil carefully plated with platinum, palladium, or iridium, and immersed
in the solution being tested, which is saturated to equilibrium with purified
hydrogen gas. The hydrogen is bubbled through the solution surrounding
the electrode. In order to measure the electric potential of the solution in
which the hydrogen electrode is placed, it is brought in contact by liquid
junction with another electrode or half-cell, which may be a similar hydrogen
electrode, or it may be one of the other types of standard half-cells, such as
one of the calomel electrodes. Thus, if two hydrogen electrodes are placed in
solutions containing different hydrogen ion concentrations, but joined by a
liquid junction, then the potential difference is given by the equation—
and therefore the potential difference is proportional to the difference in pH

between the two solutions. If E is measured, and one pH is known, the
unknown pH may be evaluated.
T h e e l e c t r o c h e m i c a l effects of i o n s in s o l u t i o n a r e influenced n o t o n l y
b y t h e c o n c e n t r a t i o n o f t h e ions b u t also b y t h e " a c t i v i t y coefficient", a n d
strictly speaking t h e pH is not directly related to t h e hydrogen ion concentra-
t i o n . H o w e v e r , for p r a c t i c a l p u r p o s e s t h e p H i s a c c e p t e d a n d i n t e r p r e t e d a s
b e i n g r e l a t e d t o t h e h y d r o g e n ion c o n c e n t r a t i o n .
As previously mentioned, it is not practicable to measure t h e pH of a
s o l u t i o n b y m e a n s o f h y d r o g e n electrodes, i t c a n , h o w e v e r , b e m e a s u r e d b y a
c o m b i n a t i o n of t w o o t h e r electrodes (half-cells) s u c h as t h e calomel e l e c t r o d e
a n d t h e glass electrode.
Calomel electrode: T h e c a l o m e l e l e c t r o d e is c o m p o s e d of m e r c u r y a n d
c a l o m e l ( m e r c u r o u s chloride) in a w a t e r solution of p o t a s s i u m chloride. T h e s e
m a t e r i a l s a r e c o n t a i n e d in a glass vessel of a s u i t a b l e design. O n e s u c h design
i s s h o w n i n F i g . 4 6 (b). P r o v i s i o n i s m a d e i n s o m e m a n n e r t o p r o t e c t t h e
Fig. 46—(a) Glass electrode. (b) Calomel electrode.
e l e c t r o d e from c o n t a m i n a t i o n b y diffusion o f t h e s o l u t i o n b e i n g t e s t e d
t h r o u g h t h e liquid j u n c t i o n . T h i s i s n o r m a l l y a c h i e v e d b y m a i n t a i n i n g t h e
s o l u t i o n i n s i d e t h e cell a t a h i g h e r level t h a n t h e t e s t s o l u t i o n , t h u s k e e p i n g
t h e l i q u i d j u n c t i o n flushed w i t h fresh p o t a s s i u m c h l o r i d e s o l u t i o n . E l e c t r i c a l
c o n t a c t t o t h e c a l o m e l cell i s o b t a i n e d t h r o u g h t h e m e r c u r y b y m e a n s o f a
p l a t i n u m wire, sealed t h r o u g h t h e b o t t o m o f t h e c a l o m e l e l e c t r o d e , o r fed
t h r o u g h t h e t o p o p e n i n g o f t h e vessel i n t o t h e m e r c u r y . T h e p o t e n t i a l o f a
calomel electrode is dependent upon t h e concentration of the potassium
chloride solution in contact with the calomel and mercury. One of three
concentrations may be used, namely, 0.1 normal, normal, or saturated. The
last is used most widely in practice because it is easily prepared; it has the
same salt concentration as the salt bridge (liquid junction) and hence
eliminates diffusion difficulties; and it has a high conductivity which increases
the sensitivity of the system.
Glass electrodes: Glass electrodes, as the name implies, are bulbs of thin-
walled glass of special composition blown on the end of a glass tube. Inside
this tube is an electrode of some type, such as a silver-silver chloride electrode
in a hydrochloric acid solution. A typical glass electrode is shown in Fig.
46 (a). It is believed that an actual transfer of hydrogen ions takes place
through the bulb, which makes it behave like a hydrogen electrode, and like
the hydrogen electrode it needs a reference electrode and salt bridge to
complete the hydrogen ion cell.
In many respects the glass electrode is considered ideal, in that nothing
has to be added to the solution which might alter its hydrogen ion concentra-
tion; also the electrode cannot become poisoned, and it can be used for
measuring the pH of all kinds of materials, including those which are semi-
solid in consistency and those which contain active reducing or oxidizing
substances. The range of application is normally from about 1 to 13 p H ;
however, errors may be introduced in alkaline solutions containing appreci-
able amounts of sodium salts. With frequent and proper calibration a limit
of error of about 0.02 pH is attainable with the glass electrode.
Before use, all glass electrodes should be immersed in distilled water for
at least 24 hours. When not in use, the glass electrode should be stored in
distilled water, as repeated wetting and drying impairs the action of the glass
membrane. Several makes of pH equipment using glass electrodes are on the
market, all of which operate on more or less similar principles, the main
differences between them being in structural detail.
pH Meters: Modern pH meters usually utilize the glass electrode, calomel

electrode combination. A typical modern pH meter is illustrated in Fig. 47.
Because the conductivity of glass is very low, even a thin membrane exhibits
very high resistance (108 ohms), it is necessary to amplify the potential
difference across the two electrodes, and to measure the voltage directly with
a calibrated galvanometer.
The overall potential developed by the complete electrode assembly is
of the form—
E = K pH + Eo
where E = overall measured potential
K = a thermodynamic constant varying with temperature
Eo = the result of a group of fixed potentials—half cell poten-
tials, asymmetry potential, liquid junction potentials,
etc. This also varies with temperature.
Due to the fact that asymmetry potential will vary from electrode to
electrode, and, even for the same electrode, from time to time, a pH meter
must be standardized before being used to measure the pH of an unknown
solution. This is carried out in the following manner. A standard buffer solu-
tion of known pH is used and the electrode assembly is immersed in the
buffer. The temperature effect of the standard buffer solution must be
compensated for either by the use of a platinum resistance thermometer
connected directly to the pH meter, in which case the compensation is auto-
matic, or by measuring the temperature and manually compensating for it
by adjusting the temperature compensating dial on the instrument. When
this has been done the correct value of K in the above equation is established
in the instrument. The meter is checked for zero reading and this is adjusted
if necessary, and then switched to the appropriate scale to measure the pH
of the standard buffer solution. By adjustment of a knob provided, the meter
is made to read the pH of the buffer solution used and this operation serves
to provide the correct value of Eo in the equation. The meter should then
indicate correctly the pH of an unknown solution. For strict accuracy the
buffer solution and any other solutions tested should be at the same temper-
ature, and the results obtained will then correspond to pH at this temperature.
Values of pH at one temperature cannot be converted to the basis of another
temperature unless the pH-temperature relationship of the solution is known.
Determination of pH values of Sugar Mill Products: The most important
aspect of pH measurement in a sugar mill is its use for the control of the
clarification process. Almost all mills have now installed automatic equip-
ment for the addition of lime to mixed juice, and this addition of lime is
controlled by pH measurements made on the limed juice. This pH measure-
ment is continuous and generally utilizes an industrial glass electrode, which
will operate at high temperature and withstand erosion, together with an
industrial calomel electrode, which maintains a slight pressure on the
potassium chloride solution to ensure that the liquid junction is not fouled.
The pH of the limed juice determines the final pH of clarified juice, and the
set point of the pH controller is altered up or down according to the value
determined on the clarified juice. The pH of clarified juice is the most im-
portant pH measurement in the factory, and for preference this quantity
should be measured continuously using a pH recorder. Whether a recorder
is used or not, periodic laboratory pH determinations should be carried out
on clarified juice, to determine its pH value, or to check the accuracy of the
recorder.
These determinations should be carried out with an accurate laboratory
pH meter, which is a most useful instrument for general laboratory work
and for measurements of pH on other factory products. Laboratory pH

measurements are carried out in the following manner:—
Check and restandardize the instrument at least once per shift with
standard buffer solution as described previously.
Cool the solution to room temperature or to the temperature at which
the instrument was restandardized.
Rinse the electrodes with a portion of the test solution prior to carrying
out the determination.
Fill the beaker or receptacle with test solution to a level which will
ensure that the electrodes and thermometer bulb are well covered.
Read the temperature of the solution and adjust the instrument temper-
ature compensator to the desired setting. (Reference tables may have to be
used on older model pH meters.)
Allow sufficient time for the system to come to equilibrium, and
determine the pH.
After the determination is completed, thoroughly wash the electrodes
with distilled water and keep them immersed in distilled water when not
in use.
N.B.—Glass electrodes are fragile and susceptible to breakage. Extreme
care should be taken when handling these electrodes.
CHAPTER XI
CALCULATIONS INVOLVED IN CHEMICAL CONTROL

The chemical control of any process is divisible into two fairly distinct
phases. One phase involves the study of a group of facts associated with the
process—quantities of materials entering process, leaving process or in pro-
cess; the compositions of original, intermediate and final products; the
necessary details of auxiliary materials used in the process; and the conditions
under which the various stages are operated. The second phase deals with
attempts to express in figures the merit of the results achieved. In industry
generally the purely quantitative relationships provide an adequate index of
performance, but this is not usually the case in sugar manufacture. For
instance, pol extraction and recovery which are purely quantitative figures
are not adequate measures of milling or manufacturing efficiency. Other
things being equal, a recovery of 86 per cent is better than one of 85 per cent,
but in practice other things are not equal and the lower recovery may re-
present the better performance.
In the majority of Queensland sugar factories the analytical and quan-
titative data are only approximate. Actual weights are available for only a
few of the materials involved, pol is used as an approximation for sucrose,
Brix instead of total soluble solids, and various empirical formulae are
introduced. This provides a set of figures which are substantially accurate
and trustworthy for certain "normal" conditions. Should the existing condi-
tions not conform to those assumed the data are rendered incorrect; and the
magnitude of the discrepancies which enter depends upon the extent of the
divergence from normal. The shortcomings of this control are generally
recognized by the mill chemist, but in the absence of means of securing
accurate data, the magnitude of the discrepancies at any time cannot be
gauged.
These shortcomings of the present empirical system for cane analysis
have been well known for many years, but there is no point in discarding an
accepted system unless some improved method is available. Several years ago
an intensive investigation into the juice weighing system of factory control
was carried out. The results of this investigation showed the system to be less
prone to the large seasonal variations of the empirical system, but it also
brought to light several disturbing sources of inaccuracy in the method.
Attention has now moved from juice weighing to the direct analysis of cane
using a wet disintegrator for the determination of Brix and pol, and a Spencer
or similar type of hot air circulating oven for the determination of moisture.
At the time of writing this edition the matter is under investigation, and it
may well be that the empirical method of analysis will be superseded by
direct analysis of cane.
Quantitative Data
Materials Balances—A materials balance involves a statement of (1) the
total quantity of a particular material entering a process from various
sources, and (2) the total quantity of the same material leaving the process
through various avenues. In the factory, materials balances may be drawn
up to cover a single stage of processing, several stages, or the whole operation,
and may deal with pol, Brix, impurities, fibre, crystal, etc.
152 CALCULATIONS INVOLVED IN CHEMICAL CONTROL
Pol Balance (Empirical System)

The most important materials balance is the pol balance of the factory.
Pol enters the factory only in the cane, and leaves mainly in bagasse, mud,
molasses and sugar. The total of these quantities of pol leaving will normally
be less than that of the pol entering, the discrepancy being due to mechanical
losses, destruction of pol in the process and errors in the measurements,
analyses and formulae. These losses are grouped under the title of "un-
determined" losses. For convenience, each quantity of pol leaving the factory
is expressed as a percentage of the quantity of pol entering the factory.
Stock—When a materials balance is taken out at an intermediate stage
of operation of a process some of the material involved may be only partly
treated and held in stock. Such material may be entered in the materials
balance as "in stock", but for the purposes of the pol balance it is customary
to presume that all the pol in stock will eventually leave the factory in sugar
or final molasses, and to calculate how much of the pol in stock should pass
into each of these channels. This involves the use of recovery formulae (see
later) or recovery tables. A recovery formula or table will predict the
percentage of the total pol in stock which may be expected later to pass out
in the sugar. It follows that, if x is the percentage "recovered" as sugar,
then 100 — x per cent will enter the molasses.
Normally when taking out a pol balance over a period, account must be
taken of stock at both the beginning and the end of the period. The quantities
of recoverable and unrecoverable pol in each stock are calculated and those
figures for the beginning of the period are subtracted algebraically from the
respective figures for the end of the period. The balances may be positive or
negative and are accordingly added to or subtracted from the respective
figures for pol in sugar and in molasses actually made during the period.
Hence the pol balance becomes:—
Pol in sugar, made and estimated, per cent pol in cane
Pol loss in bagasse per cent pol in cane
Pol loss in mud per cent pol in cane
Pol loss in molasses, made and estimated per cent pol in cane
Undetermined loss
100
Pol in Cane—The quantity of pol entering the factory is not measured

directly but determined from the weight of the cane and the analysis of the
first expressed juice, with the aid of an empirical formula—thus:—
Tons pol in cane = tons cane x pol per cent cane
where F = fibre per cent cane

Pol Loss in Bagasse—From the definition of pol extraction it follows that
Pol loss in bagasse = 100 — pol extraction.
Pol Loss in Mud—This is derived from the weight of mud and the pol
per cent mud.
Pol Loss in Molasses—This is derived from the weight of molasses and

the pol per cent molasses, with correction for stock.
CALCULATIONS INVOLVED IN CHEMICAL CONTROL 153
Pol loss in molasses =
Pol in Sugar—This is derived from the weight of sugar and the pol of
the sugar, with correction for stock.
Pol in Sugar =
Undetermined Loss—This is a residual, calculated by difference, either

in tons or per cent pol in cane.
Pol Balance (Direct Analysis)
The only difference between this system and the empirical system just
set out, is that pol per cent cane is determined directly, using the wet dis-
integrator. Thus the empirical formula for pol in cane is not used in this
method and one possible source of error is avoided.
The accuracy of the direct analysis system, as with all other analytical
systems, depends of course, on the accuracy and adequacy of sampling
techniques, plus strict adherence to good analytical procedures.
Overall Recovery—Overall recovery, frequently simply called recovery
is the tons of pol recovered in sugar expressed as a percentage of the tons of
pol in cane.
and is identical with the figure for pol in sugar per cent pol in cane.
Boiling House Recovery—In the boiling house recovery, the quantity
of pol in sugar, made and estimated, is expressed as a percentage of the
quantity of pol entering the boiling house, i.e., in the juice leaving the mills.
It follows by simple reasoning that
Extraction—This is an important figure from a commercial point of

view, since it relates the quantity of pol extracted by the milling plant to the
quantity of pol in the cane. It also provides an estimate of the percentage of
the pol in cane which enters the boiling house, and thus forms a basis for the
evaluation of boiling house recovery. The extraction is calculated from the
analysis of bagasse and cane as follows:—
Let— P c = pol per cent cane
Fc = fibre per cent cane
Pb = pol per cent bagasse
Bb = Brix per cent bagasse
W = moisture per cent bagasse
F b = fibre per cent bagasse
Then since bagasse consists of fibre, soluble solids and water—
Fb = 100— Bb — W
In practice Bb is frequently calculated by assuming t h a t t h e purity of the

juice in t h e bagasse is equal to t h e p u r i t y of last expressed juice, a n d from
this assumption:—
where C = p u r i t y of l a s t e x p r e s s e d j u i c e
This assumption is not usually correct, t h e p u r i t y of juice in t h e bagasse
b e i n g n o r m a l l y lower t h a n t h e p u r i t y o f l a s t e x p r e s s e d j u i c e , b u t t h e e r r o r
i n t r o d u c e d i s n o t large a n d i s f r e q u e n t l y t o l e r a t e d .
As no fibre is lost or g a i n e d in t h e process, t h e q u a n t i t y of fibre w h i c h
enters m u s t eventually appear in the bagasse. Therefore, there are Fc p a r t s
of fibre e n t e r i n g a n d p a s s i n g to t h e b a g a s s e , p e r 100 p a r t s of c a n e , so t h a t —
T h e e x t r a c t i o n o b t a i n e d b y i n d i v i d u a l mills s u b s e q u e n t t o N o . 1 mill c a n
also be c a l c u l a t e d as a p e r c e n t a g e of t h e pol in t h e b a g a s s e from t h e p r e v i o u s
mill i n t h e following m a n n e r : —
where en = pol e x t r a c t i o n at t h e wth mill e x p r e s s e d as a p e r c e n t a g e of

p o l in t h e b a g a s s e from t h e p r e v i o u s (n — 1) mill.
En = pol e x t r a c t e d p e r c e n t pol in c a n e for n mills of t h e t r a i n .
En - i = pol e x t r a c t e d p e r c e n t p o l in c a n e for n — I mills of t h e
train.
For example:—Consider t h e following list of p o l e x t r a c t i o n s p e r c e n t
pol i n c a n e .
No. 1 mill—70.0
No. 2 mill—82.0
No. 3 mill—90.0
No. 4 mill—95.0
T h e n extraction by n u m b e r t h r e e mill, expressed as a percentage of t h e pol
in n u m b e r t w o mill b a g a s s e : —
T h e e x t r a c t i o n o b t a i n e d b y e a c h i n d i v i d u a l mill e x p r e s s e d a s a p e r c e n t a g e
o f t h e p o l i n t h e feed t o t h e m i l l c a n b e c a l c u l a t e d b y c a r r y i n g o u t a m a t e r i a l s
balance over t h e milling train.
Maceration—The quantity of maceration is logically considered as a

percentage of fibre. It is strongly recommended that the maceration water
be weighed or measured, since this gives an accurate figure for the water used,
which moreover is immediately available as a guide to the correct regulation
of the added water. The maceration water per cent fibre for any period is
then readily calculated from the weight of water, weight of cane and average
fibre in cane for the period.
The proportion of water added is often conveniently reported in terms
of "dilution", i.e., the portion of the maceration water which passes into the
mixed juice. This may be expressed as a percentage of undiluted juice or as
a percentage of fibre in cane.
Dilution per cent Undiluted Juice—This is calculated by a Brix balance,
since the added water introduces no solids and the quantity of Brix in the
diluted juice is identical with that in the undiluted juice.
Let— 100 — weight of undiluted juice,
B = Brix of undiluted juice,
b = Brix of diluted juice,
x = weight of maceration water in diluted juice,
and 100 + x = weight of diluted juice (mixed or clarified
juice).
Dilution per cent Fibre—This is obtained by multiplying the dilution

per cent undiluted juice by the weight of undiluted juice extracted from cane,
expressed as per cent fibre, thus—
Dilution % fibre =
The expression for undiluted juice in cane is derived from the first part
of the c.c.s. formula from which we have—
Filter Washing Water—The water used in washing filter cake (or in

diluting mud prior to filtering) should be metered and the quantity expressed
as a percentage of the dry substance in filter cake. The weight of filter cake
is determined for rotary niters as described under sampling.
Pol Added to Filter Cake by Bagacillo—Some of the pol contained
in rotary filter cake was present in the bagacillo added to assist nitration
and theoretically had been accounted for as pol lost in bagasse. Hence a
portion of the pol in the bagacillo is included in both the pol loss in bagasse
and the pol loss in mud.
A method of correcting the observed pol loss in mud to the basis of

original mud without added bagacillo was outlined in a previous edition of
this Manual. Some of the reasoning involved in the calculation is open to
question and the method is not recommended for adoption. The actual
correction is of the order of ten per cent of the observed mud loss and there-
fore is a relatively small factor on the actual pol balance.
Retention (Rotary Filters)—The calculation of retention is based on
the assumption that all fibre (bagacillo) in the feed is retained in the cake.
Let— Mf and M c be the mud solids contents per cent,
and Ff and F c the fibre (bagacillo) contents per cent,
in feed and cake respectively.
Then—
In measuring retention, the values Mf and Mc, Ff and F c are determined

as described in Chapter IX. There are other methods of obtaining an estimate
of retention, one of which was shown in the previous edition of this manual.
However, the method listed above is the only mathematically correct one
which can normally be carried out in practice, and it is recommended that
this method be used in preference to the more approximate alternatives.
Clarified Juice per cent Cane—This quantity is obtained by means
of a pol balance, thus—
Tons pol in clarified juice = tons pol in cane — tons pol in bagasse — tons
pol in mud
Concentration and Evaporation Formulae—These formulae are

similar to those for Dilution, and are calculated as follows:—
Let— 100 = weight of original juice, etc.
b = Brix of original juice, etc.
B = Brix of final product,
x = water evaporated, as percentage by weight of
original juice,
Then— 100 b = (100— x)B
Overall Evaporation Coefficient of Effets—This figure represents

the weight of water, in pounds, evaporated per hour per square foot of
heating surface, and is readily calculated with the aid of the two preceding
formulae as follows:—
N.B.:—The calculation of heating surface area for effets or other vessels

must be clearly defined if comparisons between different installations are
to be m a d e . T h e m e t h o d of c a l c u l a t i o n of h e a t i n g surface is l a i d d o w n in t h e
S.A.A. Boiler Code, A S . C B 1 , w h e r e a p p e n d i x A , s e c t i o n R - 9 s t a t e s : —
"Evaporators, Vacuum Pans, Etc.—For evaporators, vacuum pans,
h e a t e r s a n d o t h e r similar unfired vessels, t h e h e a t i n g surface shall i n c l u d e
t h e t o t a l a r e a o f t u b e s , i n c l u d i n g c i r c u l a t i n g t u b e s (if a n y ) , t h e t u b e p l a t e s
e x c l u d i n g t h e a r e a of t h e t u b e holes, a n d in t h e case of b a s k e t c a l a n d r i a s ,
t h e a r e a of t h e shell.
F o r t h i s p u r p o s e t h e a r e a o f t h e t u b e s shall b e b a s e d o n t h e e x t e r n a l
d i a m e t e r o f t h e t u b e s a n d t h e i r l e n g t h b e t w e e n t h e o u t e r surfaces o f t h e t u b e
p l a t e s . T h e n e t t u b e p l a t e a r e a shall b e t h e t o t a l a r e a o f t h e t u b e p l a t e ,
calculated on t h e external diameter of the calandria, minus the area of t h e
t u b e holes. I n t h e case o f b a s k e t c a l a n d r i a s t h e u p p e r t u b e p l a t e , m i n u s t h e
t u b e holes, a n d t h e a r e a o f t h e s t e a m inlet shall b e m e a s u r e d , a n d also, i n
t h e b a s k e t t y p e , t h e a r e a o f t h e shell shall b e b a s e d o n t h e o u t s i d e d i a m e t e r
a n d t h e l e n g t h b e t w e e n t h e o u t e r surfaces o f t h e t u b e p l a t e s . I n t h e case o f
e v a p o r a t o r s w i t h coils, h e a t i n g surface shall b e b a s e d o n t h e e x t e r n a l d i a -
m e t e r o f t h e coil a n d t h e coil l e n g t h b e t w e e n t h e inlet a n d t a i l p i p e . "
R e c o v e r y F o r m u l a e — T w o r e c o v e r y f o r m u l a e are i n c o m m o n u s e ; t h e
S.J.M. a n d t h e W i n t e r - C a r p . E a c h i s t a k e n t o r e p r e s e n t t h e p e r c e n t a g e o f
t h e pol i n t h e original m a t e r i a l r e c o v e r a b l e a s pol i n s u g a r . T h e S.J.M.
f o r m u l a is d e r i v e d as f o l l o w s : —
L e t — 100 = w e i g h t of p r i m a r y p r o d u c t ,
J = p u r i t y of p r i m a r y p r o d u c t ,
P = pol of p r i m a r y p r o d u c t ,
S = p u r i t y of s u g a r p r o d u c e d ,
M = p u r i t y of final molasses,
x = r e c o v e r y of pol p e r c e n t pol in p r i m a r y p r o d u c t ,
The Winter-Carp formula was originally derived from the assumption

that for every 100 parts of impurity in juice 40 parts of sucrose would be
rendered unrecoverable. (Compare this with the c.c.s. formula.)
To derive the Winter-Carp formula consider a juice of purity J containing
100 parts of sucrose. Then
It is found that by substituting S = 100 and M = 28.57 in the S.J.M.

formula, the Winter-Carp formula may be derived thus—
Hence arises the common impression that the Winter-Carp formula is a

special case of the S. J.M. formula. Originally intended to express the recovery
of raw sugar, the Winter-Carp formula is now used, like the S.J.M., to express
the recovery of pol from the quantity of pol present in the original material.
Example—
Given 130 tons of massecuite of Brix 95 and pol 66.5—hence 70 per cent
purity, calculate the quantity of sugar recoverable.
S.J.M. Formula—Assuming 100 purity for sugar, and molasses
purity of 35—
Molasses in Stock—The estimation of molasses in stock follows simply

from the calculation of recoverable pol, for—
Tons pol in molasses = tons pol in stock — tons recoverable pol.
The figure for pol in molasses thus derived may be used directly in the
calculation of the pol balance. If it be desired to express the quantity as
molasses, then
Taking Stock—All pans, tanks, and other holding vessels should be

calibrated so that the volume of the product in stock may be determined
readily. Stocktaking is then usually carried out by recording the volume and
temperature of each product, analysing a sample for Brix and pol, and
entering the results into a table of the following form:—
Stock Sheet
*Brix Weight
Temp. Gal- at ** Fac- Purity in Tons Tons
Material °C lons Brix T°C tor Pol Tons Brix Pol
1 2 3 4 5 6 7 8 9 10
A Massecuite
AB Massecuite
B Massecuite
C Massecuite
A Molasses
AB Molasses
B Molasses
Syrup
Juice
Magma
Totals
* Brix corrected for temperature from tables supplied.

** From tables.
Column 1 shows the actual temperature of the material when the volume
(column 2) is measured. Columns 3, 6, and 7 are obtained from the analytical
data. The values for column 4 must be corrected to the value corresponding
to the actual temperature of the material when sampled. The factors of column
5 are obtained from Table XX. The weight in tons (column 8) is obtained by
multiplying column 2 by column 5 and dividing by 100, while columns 9 and
10 are calculated by multiplying column 8 by columns 3 and 6 respectively.
Totals are obtained for columns 9 and 10, and their ratio multiplied by 100
shows the average purity of the materials in stock. Then from this value and
the total tons of pol, the recoverable sugar may be calculated by applying
the Recovery Formula. The volume of molasses expected may also be
estimated, as outlined above.
The method of measuring stock outlined above is not applicable to final
molasses, which, after brief storage, is usually found to be highly aerated.
The quantity of molasses in storage should be determined using a weight
measuring device such as the pneumercator. This device has been available
for a number of years and is well described in the paper by W. R. Dunford,
P r o c e e d i n g s Q.S.S.C.T. 1967. If s u c h a d e v i c e is n o t u s e d , g r e a t c a r e m u s t be
t a k e n w h e n s a m p l i n g final m o l a s s e s , i n o r d e r t o e n s u r e t h a t a r e a s o n a b l y
accurate estimate of the actual average Brix m a y be obtained. For advice in
measuring stocks u n d e r these conditions t h e reader is referred to t h e p a p e r by
N . S m i t h , P r o c e e d i n g s Q.S.S.C.T. 1941.
In recent years, with the advent of bulk sugar handling, one further
stock q u a n t i t y has to be calculated, t h a t of the sugar held in the bulk bin at
t h e e n d of a p e r i o d . To o b t a i n an a c c u r a t e e s t i m a t e of t h i s s t o c k , a b e l t
w e i g h e r o n t h e b e l t feeding i n t o t h e s u g a r b i n , o r a b i n w e i g h i n g d e v i c e , s u c h
a s t h e l o a d cell a r r a n g e m e n t i n s t a l l e d a t o n e Q u e e n s l a n d mill, s h o u l d b e
employed, and these are to be recommended.
F o r w e e k l y mill c o n t r o l p u r p o s e s c o n s i d e r a t i o n h a s t o b e g i v e n t o t h e
d e g r e e o f a c c u r a c y r e q u i r e d w h e n e s t i m a t i n g s t o c k . F o r a w e e k l y figure t h e
a m o u n t o f t i m e a n d effort s p e n t i n s t o c k t a k i n g m a y n o t b e c o m m e n s u r a t e
w i t h t h e i n c r e a s e d a c c u r a c y o b t a i n e d , b e a r i n g i n m i n d t h e fact t h a t a n y
e r r o r s i n s t o c k o n l y affect t h e figure f r o m w e e k t o w e e k . F o r t h i s r e a s o n
difficult a n d t i m e c o n s u m i n g s t o c k t a k i n g p r o c e d u r e s , w h i c h o n l y r e s u l t i n a
v e r y s m a l l i n c r e a s e i n a c c u r a c y , a r e n o t u s u a l l y e m p l o y e d . I n m a n y mills,
where there are no large variations in t h e p u r i t y of materials in process,
a n a l y s e s a r e n o t c a r r i e d o u t o n all i t e m s o f s t o c k , t h e w e e k l y a v e r a g e a n a l y s i s
for t h e m a t e r i a l c o n c e r n e d i s t a k e n a s t h e a n a l y s i s o f t h e m a t e r i a l i n s t o c k
a t t h e e n d o f t h e w e e k . W h e n a d o p t i n g s u c h p r a c t i c e s , h o w e v e r , careful
consideration m u s t be given to t h e errors introduced to ensure t h a t the overall
e r r o r i n s t o c k does n o t r e a c h a level w h e r e i t m a t e r i a l l y affects t h e w e e k l y
r e c o v e r y figure.
M a s s e c u i t e C o m p o s i t i o n — I n order to determine the relative q u a n -
t i t i e s of s y r u p a n d m o l a s s e s r e q u i r e d to p r o d u c e a m a s s e c u i t e of a definite
p u r i t y , t h e following f o r m u l a gives a close a p p r o x i m a t i o n . I t i s b a s e d o n t h e
assumption t h a t t h e Brix values of b o t h syrup a n d molasses are equal, an
approximation which is usually experienced in practice, particularly when
t h e quantities are m e a s u r e d in t e r m s of t h e volumes of massecuite boiled on
the respective materials.
L e t — p = p u r i t y of m o l a s s e s ,
P = p u r i t y of s y r u p ,
M = p u r i t y of m a s s e c u i t e ,
x = p e r c e n t a g e of s t r i k e d e r i v e d f r o m m o l a s s e s ,
y = 100 — x = p e r c e n t a g e of s t r i k e d e r i v e d from s y r u p .
Assuming uniform Brix—
T h e s e f o r m u l a e c a n b e a p p l i e d t o a n y m i x t u r e o f m a t e r i a l s o f different
p u r i t i e s , a n d t h e c a l c u l a t i o n i s often c o n v e n i e n t l y c a r r i e d o u t b y u s i n g t h e
"cross" m e t h o d as follows:—
call this A.
call t h i s B.
When it is desired to know the actual quantities of molasses and syrup

necessary to give the strike, the following procedure should be followed:—
Let— B — Brix of massecuite,
b = Brix of syrup and molasses,
X = quantity of molasses used per 100 massecuite,
Y = quantity of syrup used per 100 massecuite.
Expected Purity of Molasses—A formula derived statistically by the

staff of the Sugar Research Institute is designed to give a target purity which
is the lowest purity of molasses which could normally be expected to be
attained from the material being processed. The expected true purity is
calculated from the reducing sugar to ash ratio of the molasses in the following
manner:—
Expected purity = 40.67 — 17.80 log X
where X = Reducing sugar/ash ratio
Equivalent Standard Granulated (E.S.G.)—Not all the pol in raw
sugar is recoverable, some being destined to pass out of the refinery in
molasses. E.S.G. is intended to represent that portion of the pol in a raw
sugar which is recoverable as pure sucrose. In the calculation of E.S.G. use
is made of the Winter-Carp formula to derive the E.S.G. factor.
Recovery and boiling house recovery may be expressed in terms of

E.S.G. instead of pol by multiplying each by the E.S.G. factor of the s u g a r -
Recovery E.S.G. = pol recovery x E.S.G. factor
In recent years the importance placed on E.S.G. figures has declined,
and these figures are now seldom seen in literature.
Crystal Content of Massecuite—The crystal content of a massecuite
may be calculated from the analyses of the massecuite and the mother liquor
of the massecuite. For the purposes of deriving formulae for crystal content
it may be assumed that "crystal" has a dry substance content or a sucrose
content or a true purity of 100 per cent. Thus three formulae may be derived,
based on true analyses. Add to this the three formulae which may be drawn
up on the basis of the apparent analyses, Brix, pol, and apparent purity,
and it is found that six formulae are available for the calculation of crystal
content.
Suppose that the massecuite and mother liquor be analysed for sucrose
contents. Then the crystal content may be derived as follows:—
Suppose 100 parts of massecuite, of sucrose content S mass per cent,
contain C per cent of crystal. Let the sucrose content of the mother
liquid be S mol. Then, from a sucrose balance
The formulae involving dry substance, Brix and pol are derived similarly
and are analogous in form.
If purity be adopted as a basis of calculation, the derivation is slightly
different. It is convenient to regard crystal content as the recoverable sucrose,
of 100 purity, per cent massecuite. The S. J.M. formula may be used to derive
the recoverable sucrose per 100 sucrose in massecuite and this may be
converted simply to the basis of per 100 parts of massecuite.
Let the purities of massecuite and molasses be P mass and P mol respec-
tively, the dry substance per cent massecuite D.S. mass and the sucrose per
cent massecuite Smass.Then
Note that the form of the first term is analogous to that of the previous
formulae, but the dry substance per cent massecuite is also involved in the
complete expression.
100 parts total solids in massecuite. This is a useful figure, particularly as it

may be calculated using only purity figures, which are the most commonly
available for pan products. The crystal contents set out in Table XVIII are
calculated by this formula.
With six formulae available to calculate crystal content, the question
arises as to the order of merit of the formulae in practice. Sucrose and true
purity figures provide the best bases of calculation; pol and apparent purity
figures yield results sufficiently accurate for routine work; dry substance gives
reasonably satisfactory results; Brix gives unreliable results and should not
be used to calculate crystal contents. If the method of separation of the mother
liquor from the massecuite involves any significant degree of concentration or
dilution, crystal content calculations must be based on purity.
Rapid Method for Determining Weighted Average from Previous
Average and Value for N e w Period—In preparing the weekly report, the
chemist is required to give "To Date" values for each item, which involves
considerable time and labour by the usual arithmetical method. The following
is a simple, short method, and should be of interest to those chemists who are
not acquainted with the procedure:—
The previous "To Date" total (cane, molasses, or sugar) is divided by
the new total, thus providing a factor. The value for each item in the new
period is then subtracted from the previous average, and the difference is
multiplied by the factor. The value so obtained is added to the new value
to give the new average. If the value for any item, is greater in the new period
than in the previous average, the difference will be negative, and the amount
is actually subtracted. This is demonstrated by the following example:—
Cane
Tons Cane
Fibre Pol
% %
Previous "To Date" values 172,108 13.42 16.81
New Period 18,307 14.08 15.75
To Date 190,415 13.48 16.71
Fibre Calculation— Pol Calculation—

13.42 — 14.08 = -0.66 16.81—15.75 = 1.06
—0.66 x 0.9039 = -0.60 1.06 x 0.9039 = 0.96
14.08 + (-0.60) = 13.48 15.75 + 0.96 = 16.71
Obviously the method cannot be applied to calculated values such as

dilution, crushing rate, percentage lost time, etc.; these must be determined
by employing the usual formulae.
Performance Criteria
Milling-—Numerous formulae have been devised to measure milling
efficiency, but only two have been adopted in Queensland—Reduced Extrac-
tion and Lost Undiluted Juice per cent Fibre.
Reduced Extraction—In the extraction formula it may be seen that, for
constant values of pol in cane and pol and fibre in bagasse, the higher the
fibre in cane, the lower the extraction. Accepting this as true in practice, the
Reduced Extraction formula sets out to eliminate the effect of variations due
to fibre per cent cane by "reducing" this figure to a standard 12.5 per cent.
The formula was derived by Deerr, who argued along the following lines:—
If e is the actual extraction, and / the fibre per cent cane, then v the
absolute juice per cent fibre in bagasse is given by the expression
criticism for it implies that the pol of the absolute juice is uniform, throughout
the cross section of the cane stalk. This is far from correct though a parallel
assumption in regard to Brix is much more reasonable.
The main weakness of the formula is the implicit assumption that the
higher the fibre content of the cane, the lower the extraction. If the higher
fibred canes display improved response to milling and maceration the relation-
ship may actually be reversed. The reduced extraction formula would then
become even worse than pol extraction as a measure of milling efficiency.
Lost Undiluted Juice in Bagasse per cent Fibre—Since from the technical
or operating point of view the work of a milling plant consists of the separa-
tion of juice from fibre, and since loss of juice in bagasse is caused only by
fibre, the logical method of evaluating the technical efficiency of the milling
station is by expressing the loss in bagasse in terms of undiluted juice per cent
fibre. Obviously the comparison of results on a basis of pol extraction with
differing fibre and pol contents of cane can be quite misleading if used as a
criterion of efficiency of milling work.
The lost undiluted juice per cent fibre is calculated by expressing the
Brix in bagasse in terms of an equivalent amount of undiluted cane juice
(the Brix of which is taken as equal to that of first expressed juice), as
follows:—
Lost undiluted juice per cent fibre =
or, using the same nomenclature as for calculating extraction, and Bf for
Brix of first expressed juice—
It will be noted that the quantities involved in this expression are all
determined directly and involve neither the assumptions of the c.c.s. formula
nor the use of the figure for fibre in cane.
Like reduced extraction, lost undiluted juice per cent fibre compensates
for the quantity of fibre handled but can take no account of its quality. This
formula is based on sounder principles than the reduced extraction formula,
but suffers from the disadvantage of providing a value of zero for the limit
of perfection and an upper limit approaching 1000. On this scale relative
merits are not easily appreciated.
In the absence of any complete criterion of the milling quality of cane,
milling efficiency figures must continue to give only moderate satisfaction.
Boiling House Efficiency—The influence of the purity of the raw
material on recovery is so pronounced that recovery figures serve as a poor
guide to efficiency. In Boiling House Efficiency the actual boiling house
recovery is expressed as a percentage of the recovery indicated by the
Winter-Carp recovery formula. Strictly the Winter-Carp recovery should be
based on the purity of mixed juice, but as this is not generally available, the
purity of first expressed juice is taken instead.
T h e w e a k n e s s o f t h e boiling h o u s e efficiency f o r m u l a i s t h a t i t a c c e p t s
all t h e p o l i n t h e s u g a r a s r e c o v e r a b l e pol. T o c o m p e n s a t e for t h i s t h e E . S . G .
R e c o v e r y m a y b e t a k e n , t h e figure d e r i v e d b e i n g Boiling H o u s e Efficiency
E . S . G . , o r Boiling H o u s e P e r f o r m a n c e . A n o t h e r w e a k n e s s i s t h a t t h e b a s i c
r e c o v e r y d e p e n d s o n l y u p o n t h e p u r i t y o f t h e original j u i c e , t h e r e b y t a k i n g
account of the quantity, b u t not the nature of the impurities.
V a r i o u s a t t e m p t s h a v e b e e n m a d e t o e l i m i n a t e t h e effects o f p u r i t y o f
original m a t e r i a l on recovery, by " r e d u c i n g " t h e p u r i t y of t h e m i x e d juice
t o a s t a n d a r d o f 8 5 p e r c e n t . H e n c e s u c h t e r m s a s R e d u c e d Boiling H o u s e
Recovery a n d R e d u c e d Overall Recovery h a v e been derived. There is dis-
a g r e e m e n t o v e r t h e r e a s o n i n g i n v o l v e d i n r e d u c i n g t h e recoveries t o a s t a n d a r d
based on juice of 85 per cent purity, and, as t h e reduced recoveries are not
used in Queensland, t h e formulae h a v e been o m i t t e d from this Manual.
B e c a u s e of t h e n u m e r o u s deficiencies in t h e Boiling H o u s e Efficiency
formula it is not normally considered to be of great importance.
C o e f f i c i e n t o f W o r k — A s s t a t e d i n t h e Definitions,
I r r e s p e c t i v e of i t s m e r i t s as a c r i t e r i o n of f a c t o r y p e r f o r m a n c e , t h e
coefficient of w o r k is t h e m o s t i m p o r t a n t figure in mill c o n t r o l in Q u e e n s l a n d
since i t r e l a t e s t h e s u g a r m a d e t o t h e c a n e c r u s h e d i n t e r m s o f t h e b a s i s o n
w h i c h t h e s e c o m m o d i t i e s a r e b o u g h t a n d sold. H e n c e t h e figure h a s h i g h
significance financially. As a m e a s u r e of f a c t o r y p e r f o r m a n c e t h e coefficient
of w o r k e m b o d i e s t h e deficiencies of t h e c.c.s. a n d n e t t i t r e f o r m u l a e a n d
must be accepted with caution.
As s t a t e d earlier, t h e c.c.s. f o r m u l a p o s t u l a t e s a s t a n d a r d loss of sucrose
in process. W o r k i n g to t h i s s t a n d a r d , a mill t r e a t i n g 100 t o n s of c.c.s. w o u l d
r e c o v e r 100 t o n s o f p u r e s u g a r (100 n . t . ) , w h i c h w o u l d b e e q u i v a l e n t t o n e a r l y
106.4 t o n s of 94 n . t . s u g a r . T h e coefficient of w o r k w o u l d be n e a r l y 106.4.
T h i s is s o m e t i m e s r e g a r d e d as t h e u p p e r l i m i t of t h e coefficient of w o r k . T h e
i d e a s t h a t (1) t h e u p p e r l i m i t of coefficient of w o r k is 100, a n d (2) t h e u p p e r
l i m i t i s a b o u t 106.4 a r e b o t h e r r o n e o u s . T h e u p p e r limit i s v a r i a b l e , b u t
r e p r e s e n t s a p e r f o r m a n c e in w h i c h all t h e sucrose in t h e c a n e is r e c o v e r e d as
p u r e s u g a r . A coefficient of w o r k of 106.4 a p p r o x i m a t e l y is t h e minimum v a l u e
at which this condition could exist. This m i n i m u m value would be obtained
f r o m c a n e w i t h a m a x i m u m c.c.s. for i t s pol c o n t e n t , i.e. c o n t a i n i n g no i m -
p u r i t i e s i n t h e j u i c e . I f all t h e sucrose i n t h e c a n e c o u l d b e r e c o v e r e d f r o m
c a n e c o n t a i n i n g i m p u r i t i e s in i t s juice, a coefficient of w o r k h i g h e r t h a n 106.4
w o u l d be o b t a i n e d , e.g. consider c a n e of t h e following analysis.
pol p e r c e n t c a n e = 16.0
Brix per cent cane = 18.0
c.c.s. = 15.0
P o l r e c o v e r e d a s p u r e s u g a r f r o m 100 t o n s c a n e = 16.0 t o n s
16.0 t o n s at 100 n . t . = 17.02 t o n s at 94 n . t .
T o n s of c.c.s. f r o m 100 t o n s c a n e = 15.0
CHAPTER X I I
THE BOILER S T A T I O N
Introduction
The large quantity of steam required by the factory for power and
heating purposes is supplied by a boiler station where the chemical energy
stored in the fuel is released by combustion in the furnaces and as much
as possible transferred, in the form of heat, to the boilers proper. The steam
generated by the boilers provides a very flexible medium for applying heat
wherever it may be wanted and, when generated at a suitable working
pressure, it may first be used in prime movers to supply all the mechanical
and electrical power needed by the various factory processes.
Boiler Efficiency
It should be the aim in every factory to operate the boiler station at
an efficiency which enables all steam requirements to be met by burning
only the bagasse fuel which is available from the milling process.
Boiler efficiencv for any period of time may be stated as:
To carry out an efficiency test it would be necessary to measure the

quantities of steam produced and fuel used during the time of the test and
to determine the heat required per lb of steam and the calorific value of the
fuel used. Suggestions covering these items will now be given.
Steam Produced
For the measurement of steam output, a positive type meter on the
feedwater is recommended, together with a recording thermometer. Where
any blowing down is done during the period concerned, the weight of water
blown down must be estimated and deducted from the total weight of feed
water. This is readily done by noting the depth of water removed from the
boiler drum each time by blowing down, and calculating its volume and
weight from the dimensions of the drum. With most mills the normal amount
of blowing down during a weekly working period will probably be negligible
(well below 1 per cent of total steam) and the blow-down need be estimated
only in abnormal circumstances. Steam output may also be measured by
flow meters; this, however, necessitates careful correction of the flow meter
records for variations in steam pressure and temperature, as well as frequent
checking of the meter. In this case no correction foi blowing down is required;
on the other hand, steam blown off through the safety valves will, if of suffi-
cient amount, cause an error in the figures for steam output.
Heat Required per lb of Steam
The pressure and (when superheated) temperature of the steam should
be registered and also the temperature of the feed water. Average values for
the period of test are then calculated.
For superheated steam the heat required per lb = H —(t — 32),*
where H is the total heat of superheated steam in Btu per lb at the average
temperature and pressure obtaining during the test period and t is the
average feedwater temperature in °F.
•Steam tables using the British system of units are based on a datum of 32 °F.
Fuel Used
The most accurate way of determining the amount of fuel used is by
direct weighing. Hand weighing by feeding the bagasse into a large box
mounted on platform scales and then hand feeding the furnaces would be
quite feasible for an efficiency test of a few hours' duration on a single boiler,
but would be almost impossible for a test on the whole station. A continuous
weigher would be ideal for such an overall test and when these weighers are
installed for the purpose of chemical control the testing of boiler station
efficiency will be very much simplified. In the meantime it is necessary to
determine the weight of bagasse from the weight of cane crushed, and the
percentages of fibre in the cane and the bagasse during the period, thus—
, weight of cane x fibre per cent cane
Weight of bagasse = —~ -^-^
fibre per cent bagasse
Should the above method be used for determining the weight of fuel,
allowance must be made for any bagasse removed from the boiler station
for other purposes, also for any bagasse which might be saved during the
period of the test. It is suggested that such quantities may be determined
with sufficient accuracy by volume measurement allowing 10 lb/ft 3 for piled
bagasse.
Allowance has also to be made for any extraneous fuel used during a
test. However, as the furnaces are designed essentially for bagasse burning
it would be more satisfactory to conduct any tests at a time when the mill
had settled down to a steady crushing rate. There would then be little likeli-
hood of the boiler's requiring extraneous fuel.
Calorific Value of the Fuel

When a fuel is burned, heat is generated, and the quantity of heat
liberated per unit weight of fuel is known as the calorific value and expressed
in Btu per pound. Most fuels contain hydrogen which, when it burns, yields
water in vapour form; furthermore, any water originally present in the fuel
is also converted to vapour. This water vapour contains latent heat, re-
presenting a portion of the heat liberated by the combustion. If the water
vapour be condensed the latent heat becomes available for inclusion in the
total quantity of heat released. The calorific value determined under these
conditions is known as the Gross Calorific Value, represented by the symbol
Bh. The heat released per pound of fuel, not including any latent heat in the
products of combustion, is known as the Net Calorific Value, designated Bi.
It is customary to base all boiler calculations on gross calorific value,
but comparisons between fuels, as between, say, bagasse and coal, or between
bagasses of different moisture contents, are more reliably drawn on the basis
of net calorific value. In practical boilers only the heat corresponding to the
168 T H E BOILER STATION
net calorific value is available for absorption, but, as stated above, boiler
efficiencies and allied figures are related to gross calorific values.
Bagasse.—Formulae giving the calorific value of bagasse have been
worked out from determinations on Queensland bagasse and are as follows:
Gross cal. value (Bh) = 8345 — 22 • 1 pol — 83-45 water
Net „ „ {Bi) = 7783 — 22-1 pol — 88-27 water
In these formulae pol and water represent the percentage of pol and
moisture obtained from the analyses of final bagasse leaving the milling
plant. Strictly speaking, a correction should be made for a reduction in
moisture by evaporation between the mills and the boiler station. While such
a collection may readily be established and applied, it is suggested that for
routine calculations the figures for the bagasse leaving the final mill may be
employed. This would under-estimate somewhat the calorific value (Bh) of
the bagasse and so over-estimate the boiler efficiency and, in effect, credit
the boiler house with any drying of bagasse between the final mill and the
boilei furnaces. In any case the discrepancy in Bh would be fairly uniform
and of no consequence for comparative purposes.
Values of Bh for normal ranges of pol and moisture are given in Table
XXXV.
Wood.—The calorific value of wood depends mainly on its condition, i.e ,
how much moisture it contains. If no other information is available a B ^
value of 6000 may be taken for air-dried wood containing 20 to 40 per cent
moisture. The corresponding B\ is about 5300.
Furnace Oil and Diesel Fuel.—The average gross calorific values of these
fuels can be taken as 18,800 and 19,200 respectively.
Molasses.—The calorific value of molasses depends on its moisture
content and ash. The average values oi Bh and B\ for normal molasses can be
taken as 5380 and 4600 respectively.
Coal and Tar.—Coal and tar are about the only remaining substances
which are likely to be used as supplementary fuels in the sugar industry. The
gross calorific values can be taken as 11,000 and 16,500 respectively.
Equivalent Bagasse.—Equivalent bagasse is assumed to be bagasse
having a net calorific value of 3300 Btu per pound, calculated from bagasse
of 50 per cent moisture and three per cent pol. This value is accepted as the
standard for bagasse and all extraneous fuels. Therefore to calculate tons
equivalent bagasse, the weight of bagasse produced is multiplied by the net
calorific value (Table XXXV(b)) divided by 3,300.
The extraneous fuels are calculated to equivalent bagasse, from the
following formulae:—
Tons equivalent bagasse = tons wood X 1.6
= tons molasses x 1.4
= tons coal X 3.5
= tons oil X 5.5
Measuring Boiler Efficiency Indirectly
A certain proportion of the theoretical heat available from the bagasse
fed into a boiler furnace is used to generate steam while the remainder is
absorbed by various losses. It is possible to calculate the major losses fairly
accurately while a reasonable estimate of the minor losses may be made from
results obtained in previous tests on boilers of similar type. As the losses are
T H E BOILER STATION 169
e x p r e s s e d as a p e r c e n t a g e of t h e Bh v a l u e of t h e b a g a s s e , t h e efficiency =.
100 — losses. T h e m e t h o d gives a r e a s o n a b l y a c c u r a t e w a y of m e a s u r i n g
b o i l e r efficiency w i t h o u t t h e l a b o u r o f w e i g h i n g a n d h a n d feeding b a g a s s e a n d
w i t h o u t t h e difficulty o f m e a s u r i n g t h e s t e a m p r o d u c e d . Moreover, for a n y
p a r t i c u l a r boiler, t h e losses w h i c h a r e e s t i m a t e d c a n , u n d e r n o r m a l w o r k i n g
c o n d i t i o n s , b e e x p e c t e d t o r e m a i n c o n s t a n t while t h e losses w h i c h a r e c a l c u -
lated include those which are u n d e r t h e operator's control. T h e m e t h o d there-
fore gives a t r u e g u i d e as to h o w efficiently a boiler is b e i n g w o r k e d .
T h e v a r i o u s losses a r e discussed below a n d f o r m u l a e g i v e n for t h o s e
which can be calculated.
Condensation Loss
T h e t e r m c o n d e n s a t i o n loss i s a p p l i e d t o t h e h e a t lost i n t h e flue g a s
d u e t o w a t e r v a p o u r . P a r t o f t h i s v a p o u r c o m e s from t h e o r i g i n a l b a g a s s e
a n d p a r t i s f o r m e d i n t h e c o m b u s t i o n process.
100 (562 + 4 . 8 2 w )
C o n d e n s a t i o n loss = = p e r c e n t Bh-
Bh
where w = p e r c e n t m o i s t u r e in b a g a s s e .
Sensible Heat Loss
T h e f l u e g a s l e a v e s t h e boiler a t a t e m p e r a t u r e a b o v e t h a t o f t h e a t m o -
s p h e r e , a n d t h u s p a r t o f t h e h e a t o f c o m b u s t i o n leaves t h e boiler a s sensible
heat in the flue gas.
Table of values for lOOOK for use in formula for sensible heat loss.
Per cent COa in Per cent moisture in bagasse, w

flue gas, mt
404 0 42 44 46 48 50 52 54 56
5 78.9 79.3 79.6 80.0 80.5 81.0 81.5 82.1 82.7

6 67.3 67.7 68.1 68.4 68.8 69.4 69.9 70.5 71.0
7 58.9 59.3 59.7 60.0 60.4 60.9 61.4 61.9 62.5
8 52.6 52.9 53.4 53.7 54.1 54.6 55.1 55.7 56.2
9 47.6 48.0 48.5 48.8 49.2 49.6 50.1 50.7 51.3
10 43.8 44.1 44.5 44.9 45.3 45.8 46.3 46.8 47.4
10.5 42.1 42.4 42.8 43.2 43.6 44.1 44.6 45.1 45.7
11 40.6 40.9 41.3 41.7 42.1 42.6 43.1 43.6 44.2
11.5 39.2 39.6 39.9 40.4 40.7 41.2 41.7 42.2 42.8
12 37.9 38.2 38.6 39.1 39.4 39.9 40.4 41.0 41.5
12.5 36.7 37.1 37.4 37.9 38.3 38.7 39.2 39.7 40.3
13 35.6 36.0 36.4 36.9 37.2 37.6 38.2 38.7 39.3
13.5 34.7 35.0 35.4 35.9 36.2 36.7 37.2 37.7 38.3
14 33.7 34.1 34.4 34.9 35.2 35.7 36.2 36.7 37.3
14.5 32.9 33.2 33.6 34.1 34.4 34.9 35.4 35.9 36.5
15 32.1 32.4 32.7 33.2 33.6 34.1 34.5 35.1 35.6
15.5 31.3 31.6 32.0 32.5 32.9 33.3 33.8 34.3 34.9
16 30.6 31.0 31.3 31.7 32.1 32.6 33.1 33.6 34.2
16.5 29.9 30.2 30.6 31.1 31.4 31.9 32.4 33.0 33.5
17 29.3 29.6 30.0 30.5 30.8 31.3 31.7 32.3 32.9
Sensible h e a t loss = K (tF—tA) p e r c e n t Bh-

w h e r e K is a c o n s t a n t d e p e n d i n g on t h e C O a c o n t e n t of t h e flue g a s
a n d t h e w a t e r c o n t e n t o f t h e b a g a s s e (values for 1000K a r e
given in t h e accompanying Table).
tp = flue g a s temperature °F.
tA = air temperature ° F .
Unburnt Gas Loss

In the combustion of hydrocarbon fuels gaseous intermediate products
are formed. The existence of such products in the flue gas represents a loss
of heat. The most common instance is of carbon burning to CO instead of C0 2 -
The unburnt gas loss may be determined from the following formula:—
m2 = average reading of per cent unburnt gas registered by

a Mono or similar type of recorder.
The CO 2 and per cent unburnt may best be determined from a flue gas
analyser of the Mono type. The Mono is a recording instrument and very
convenient to use as the difference between the readings of alternate strokes
of the pen gives a measure of the unburnt gas. It is reasonable to assume that
this unburnt gas is made up of CO and H 2 , in which case the actual quantity
of unburnt would be two-thirds of the percentage shown by the difference
between alternate strokes.
Miscellaneous Losses
These are made up of radiation loss, sensible heat loss in the ash, unburnt
material in the ash and unburnt material in the fly ash. It is almost impossible
to measure these losses, but in a series of tests cairied out by the Bureau on
five water tube boilers they were found to have an average value of 8 • 3 per
cent Bh at an average rate of evaporation of 4 -9 lb per ft2 of heating surface
per hour.
Two of the miscellaneous losses relate to ash. Rough calculations show
that the sensible heat lost when hot ashes drop through the grate and are
raked out of the ashpit would be of the order of 0 • 1 per cent Bh- Observations
show that the amount of unburnt in the ash would also be very small when
stated as a percentage of heat available in bagasse. It is therefore suggested
that these two ash losses be neglected and the miscellaneous losses regarded
as being made up of fly ash and radiation losses.
Experiments carried out in 1950 indicate that fly ash loss is proportional
to boiler rating and that a reasonable figure to adopt for a water tube boiler
would be 2 per cent at a rating of 4 • 9 lb per ft2 of heating surface per hour.
If the actual steam consumption of the factory is not known the following
estimates of steam (from and at 212 °F)* per ton of cane could be used to
arrive at the boiler rating:—
Using quadruple evaporation without bleeding 61 per cent steam on cane
Using quadruple with bleeding 58
Using quintuple without bleeding 57 ,, ,,
Using quintuple with bleeding 55
It is generally accepted that radiation loss, expressed as per cent Bh,
does not increase with rating, but, if anything, tends to decrease. Reasonable
results should be obtained, however, if this loss be taken at 8-3—2 = 6 - 3
per cent Bh for all ratings.
Large boilers with water wall furnaces would tend to have a still smaller
radiation loss and in such boilers it is probable that the miscellaneous losses
would not exceed 6 per cent Bh-
•Steam raised from water at 212 °F without any change in temperature. The heat
required for this conversion is 970.6 Btu/lb.
THE BOILER STATION 171
Flue Gas
Flue Gas Composition
For any particular flue gas temperature, boiler efficiency will improve
as the amount of excess air going into the furnace is reduced—provided
always that the air is supplied in such a way that there is little if any unburnt
in the flue gas. The adjacent Table shows the relationship between the C0 2
reading, which is really a measure of excess air, and the sensible heat loss.
The last column also shows the importance of complete combustion, e.g.., the
reduction in heat loss brought about by improving the C 0 2 from 11 to 14
per cent would be completely nullified if the combustion efficiency deteriorated
sufficiently to yield an unburnt gas reading of one per cent on a Mono or
similar recorder.
Table showing sensible heat and unburnt gas losses.
(Based on a flue gas temperature of 500 °F and a bagasse
moisture of 50 per cent.)
Sensible heat Loss caused by

co2 Excess air loss in flue gas 1 per cent unburnt
per cent per cent Bh in flue gas per cent Bh
20.3
17
0
19 13.0
_2 . 5
16 27 13.5 2.6
15 35 14.1 2.8
14 44 14.8 3.0
13 56 15.6 3.2
12 68 16.5 3.5
11 84 17.6 3.8
10 102 19.6 4.2
Flue Gas Temperature

The higher the flue gas temperature the greater will be the sensible heat
loss. The temperature must go up as the boiler rating is increased and the
operator has no control over the efficiency in this regard. He can, however,
obtain maximum efficiency at any given rating by making sure that the
heating surfaces, on both water and gas sides, are kept as clean as possible.
The sensible heat loss when the bagasse contains 50 per cent moisture
and the flue gas 12-5 per cent C 0 2 varies with temperature as follows:—
Flue gas temperature °F 300 400 500 600 70C
Sensible heat loss per cent B h 8-5 12-4 16-2 20-2 24•(
Operation at moderate rating would give a temperature of between
500 and 600 °F. By fitting an economiser or air heater this could be brought
down to 350 °F, which shows that such a unit can be worth up to about
8 per cent in efficiency.
Volume of Flue Gas
To specify the capacity of an induced draught fan or fans for a boilei
station it is necessary to determine the volume of flue gas which will t*
produced per minute when the factory is working at maximum crushing rate
and all the bagasse is being burnt in the furnaces. The weight of flue gas
which will be produced by each pound of this bagasse may be found from the
following formula:—
where w = per cent moisture in bagasse

m
\ == P e r cent CO 2 in flue gas.
Over the range of C 0 2 and moisture values likely to be met, the specific
volume of the flue gas may be taken as 25 • 1 ft 3 /lb at 500 °F. For any other
It is suggested that the fan capacity be determined for a C 0 2 figure of

12 1/2 per cent and increased by 10 per cent to allow for depreciation in service.
The flue gas temperature could be taken as 600 °F. At full capacity the fan
should be capable of giving a draught of 2 in water at the back of all boilers.
The draught at the fan inlet should, for a simple installation and reasonably
well designed flues, not have to exceed 2 1/2 in. If an economiser or fly ash
eliminator be fitted extra draught must be provided to compensate for the
resistance of these units.
Horsepower Required for a Fan

The following formula gives the horsepower required for a fan:—
Effect of Density on Fan Performance

It is necessary to remember that most manufacturers state fan per-
formance in terms of "standard air" which has a density of 0-075 lb/ft 3
The volume delivered by a fan at a certain speed is independent of
density but the pressure (or draught) will be proportional to the density.
Therefore if a pressure of 3 in is required when handling flue gas at 500 °F
(specific volume 25-1 ft 3 /lb = 0 - 0 4 lb/ft 3 density) a fan giving a pressure
Forced Draught Fans

To determine the capacity of a forced draught fan the maximum rate
of burning of bagasse in the furnace must first be estimated and air required
found from the following formula:—
The volume of air per minute may then be determined.

However, if the fan is to be used with an air heater, the capacity must
be increased to allow for a certain amount of recirculation as the only sure
T H E BOILER STATION 173
way to avoid corrosion in a tube or plate type air heater is to arrange foi
the in-going air to be at a temperature at least equal to the dewpoint temper-
ature of the flue gas. This dewpoint temperature depends on the moisture
content of bagasse and per cent CO2 in the flue gas. At 50 per cent moisture
and 12.5 per cent C 0 2 it would be 148 °F and sufficient hot air must be added
to the in-going atmospheric air to give a mixture of this temperature. Taking
an atmospheric temperature of 70 °F and a hot air temperature of 370 °F
the recirculation needed would be
The combustion air required under the assumed conditions of moisture

and C 0 2 would be 4.65 lb per lb of bagasse = 7 1 - 5 ft3 at 148 °F. Therefore3
the volume of air to be handled by the fan would be 71.5 x 1.35 = 96.5 ft
per lb of bagasse burnt. This figure is suggested as being suitable for average
Queensland conditions.
Bagasse Moisture
Bagasse moisture has a very big influence on the steaming capacity of
the boilers and if steam troubles are being experienced an effort should be
made to arrange mill settings so that the moisture in final bagasse does not
exceed 50 per cent. Apart from making the bagasse easier to burn, reducing
the moisture content is equivalent to increasing the fuel supply. For moistures
in the neighbourhood of 50 per cent, one per cent reduction is equivalent to
obtaining one per cent more fuel from the same quantity and quality of cane.
The Treatment of Water for Boilers*

The supply of unsuitable water to steam generating plants is not only
uneconomical, but may be dangerous if adequate steps are not taken to
minimize the cumulatively deleterious results. The desirable feed to all boilers
is a suitably conditioned water, free from all unwanted salts and gases, and
the maximum possible amount of such suitable water as is available must be
fed to boiler plant. Where raw make-up or other unsuitable water must be
fed to boilers there is, however, no excuse for allowing the impurities in this
water to remain in the boiler in a harmful form.
The problems of boiler water treatment have become magnified in recent
years with the advent of large, modern, bent-tube, water-walled, high
capacity boilers into the industry. Such boilers are particularly prone to
damage from overloading and inadequate water conditioning, and it is false
economy to run the risk of ruining or damaging an investment worth some
half a million dollars for the sake of a small outlay on boiler feed water
treatment.
There are a number of British Standards available dealing with the
subject of water treatment and it is strongly recommended that the following
standards be purchased.
B.S. 2486 "Treatment of Water for Land Boilers"
B.S.1427 "Routine Control Methods of Testing Water Used in
Industry"
B.S. 1328 "Methods of Sampling Water Used in Industry"
*The recommendations made under this section are approved by the Chief Inspector
of Machinery.
174 T H E B O I L E R STATION
There are also a number of reputable commercial firms with long experi-
ence in this field, and, providing their recommendations are within the limits
prescribed by British Standards, the advice of such firms can be profitably-
followed. The indiscriminate addition of boiler water additives whose com-
position is not specified by the manufacturer, should, however, be avoided.
The objects of boiler water treatment are threefold, namely:—
1. The prevention of scale on heating surfaces
2. The prevention of corrosion and caustic embrittlement
3. The production of clean steam free from entrained water or solids
and these three criteria will now be discussed separately.
The Prevention of Scale on Heating Surfaces

The avoidance of scale on heating surfaces is most important, for, as well
as reducing the efficiency of heat transfer to a boiler, heavy scale will cause
overheating of the tube metal which, if sufficiently severe, can cause tube
failure.
Scale can be described as a hard adherent deposit on heating surfaces
and is caused by the presence of three main chemical substances in the water;
salts of calcium, magnesium, and silica.
It is therefore important to provide a boiler feed water containing as few
of these impurities as possible but, if the impurities must unavoidably be
introduced, as they are in small quantities even in very efficient steam plants,
they must be removed from the water before feeding it to the boiler, or
additives must be introduced to the water so that scale will not form.
The ideal answer to the problem is not to introduce water containing these
compounds to the boiler. This is done, as far as possible, by returning con-
densed steam to the boiler as feed water wherever this can be obtained in an
uncontaminated form. This practice reduces the usage of raw water, i.e.
untreated water from outside the steam-condensate cycle, as far as possible.
The use of clean condensate is the greatest single factor in the avoidance of
boiler feed treatment problems. Where raw water make-up containing scale
forming constituents must be added the scale-forming constituents of this
water can be dealt with in three ways either singly or in combination, by
distillation {i.e. evaporation), external water treatment (softening or ion
exchange), or by internal water treatment.
The use of distillation processes or external water treatment systems is,
however, not economical under sugar industry conditions, and boiler water
conditioning is carried out by what is known as internal treatment.
Internal treatment entails the chemical treatment of the boiler water
in such a manner that the scale forming substances are not deposited on the
heating surface as scale, but precipitated as a mobile sludge which flows to
the lowest point in the boiler and is removed in the blowdown. This is
usually achieved by adding phosphate to the boiler water and by maintain-
ing an excess of alkalinity, by the addition of caustic soda. Under the
alkaline conditions prevailing, the phosphate precipitates any calcium present
as calcium phosphate sludge. The caustic alkalinity precipitates magnesium
salts as magnesium hydroxide, also a mobile sludge. Any silica present will
normally be absorbed on the magnesium hydroxide precipitate and removed,
or may co-precipitate with magnesium as magnesium silicate. Thus all harm-
ful concentrations of scale forming compounds can be removed from the boiler
in the blowdown, providing the correct concentrations of phosphate and

alkalinity are maintained at all times.
The consumption of phosphate and alkali obviously depends on the
quantity of scale forming compounds fed to the boiler, so that the cost of the
treatment depends entirely on this factor. It is therefore of great importance
that the maximum possible amount of good condensate be returned to the
boiler and the minimum of poor quality water added. Thus make-up should
be kept to a minimum and, where alternative sources of make-up water are
available, the best source should be used.
There is also a secondary reason for the avoidance of feed contamination
by scale forming materials. The scale forming materials add solids to the
boiler water and the chemicals added to control the scaling add further solids.
This necessitates increased blowdown to maintain a safe solids level in the
boiler water, as will be discussed in a subsequent section, and this results in
some of the treatment chemicals being lost in blowdown. This causes an
increased chemical demand to maintain the correct chemical concentrations,
and this adds further solids to the water and so on. The net result is that the
system can reach a stage where it chases its own tail, so to speak, and
chemical costs are high due to wastage of chemicals in blowdown. Therefore
the maximum usage of good condensate for boiler feed is of the utmost
importance.
The Prevention of Corrosion and Caustic Embrittlement

Corrosion—Corrosion in a boiler is produced by two main causes, acidity
and oxygen.
Acidic conditions are corrosive to iron and steel, so that the material of a
boiler will be eaten away if acid conditions are allowed to prevail for any
length of time. The control of this problem is a relatively simple one. The
boiler water must be kept alkaline at all times. This is in conformity with the
internal method for the prevention of scale, as discussed in the previous
section, and the provision of the correct alkalinity serves a dual purpose.
The presence of dissolved oxygen in a boiler can cause very severe
corrosion. Corrosion from this source, and sometimes from acids as well,
normally occurs in the form of pits in the boiler shell or as wasting away at
the tube ends. The fact that the corrosion is concentrated in small areas and
not evenly distributed over the whole surface means that the effects are more
severe. In extreme cases of pitting, the boiler drum finally becomes holed by
pits which extend right through the metal. The theory of corrosion caused by
the presence of oxygen is rather complex, but the process is actually a form
of galvanic action. Due to stresses in a boiler shell, and to lack of complete
uniformity of metal composition, under operating conditions certain areas of
a boiler become anodes while others become cathodes. A current will pass
between the anodic and the cathodic areas and this will cause the removal of
metal from the anodic areas. The metal removed forms an hydroxide, under
the alkaline conditions in the boiler, but in order to proceed, the galvanic
action requires oxygen. If oxygen is present the action can continue indefinite-
ly and the anodic areas can be continually denuded of metal. The anodic
areas, once established, remain localized, and severe corrosion occurs at these
localized points, giving the typical pitting of oxygen corrosion.
The answer to this problem is obviously to ensure that the boiler water
contains no dissolved oxygen. The oxygen enters the boiler in the feed water
and so conditions in the feed should be maintained so that a minimum amount
of dissolved oxygen is present. The solubility of oxygen in water depends
176 T H E B O I L E R STATION
upon temperature and pressure. The solubility decreases with temperature,

at a given pressure, so that it is obviously advantageous to maintain the boiler
feed water at as high a temperature as possible. It is also essential to provide
venting to the atmosphere in the feed system, so that any oxygen or other
gases released from condensate, or raw water make-up, can be expelled.
The vent should release a certain amount of vapour, in order that no atmo-
spheric oxygen can enter the system. Condensate collection vessels and feed
tanks should be covered, except for the venting, and pump glands maintained
in good order for the same reason. Thus once again the need for a maximum of
steam condensate return is paramount, and for the purposes of oxygen content
the condensate should be as hot as possible. In any steam plant some make-up
must be used to replace unavoidable losses and the make-up should also be
as hot as possible in order to have the minimum oxygen content.
In large boiler plants feed de-aerators are used to remove oxygen before
feed entry into the boiler. These units consist essentially of a combination
heater and flash tank in which the boiler feed is heated and flashed, to allow
dissolved oxygen to be released and removed. The residual oxygen left in the
feed after the de-aerator is treated inside the boiler.
For sugar mill installations de-aerators are usually uneconomical, as
the oxygen present in the feed water can be removed chemically inside the
boiler. This is normally achieved by the use of hydrazine or sodium sulphite.
Hydrazine, a compound of nitrogen and hydrogen, N 2 H 4 , is used in
high pressure installations where dissolved solids are a problem, because both
products of the reaction are inert, one being water and the other nitrogen.
The latter goes out in the steam and is vented through the non-condensible
gas vents. The commonly used substance for internal oxygen removal is
sodium sulphite. This chemical absorbs oxygen to form sodium sulphate.
The sodium sulphate formed is not scale forming and is beneficial from
the point of view of embrittlement control, as will be seen later. This chemical,
if added in the correct manner and in such quantities as to keep a reserve of
sulphite in the boiler at all times, can completely remove all significant oxygen
corrosion and, coupled with alkalinity control, should result in the complete
avoidance of boiler corrosion. Once again, as with scale-forming materials,
the feeding of oxygen or acids to the boiler should be avoided, as these cause
increased dosage of chemicals, with consequent higher solids, greater blow-
down and the resultant chemical wastage.
Caustic Embrittlement—There has been a certain amount of argument as
to the existence and severity of cracking caused by a caustic environment,
but it is now generally agreed t h a t caustic embrittlement can only occur
under the following conditions:—
(a) The water in the boiler must contain free hydroxide alkalinity.
(b) The caustic soda must become concentrated to an extent which is
usually only possible in a joint or seam where evaporative leakage
can take place.
(c) The tensional stress in the steel must be high at the point where the
concentration of caustic soda is occurring.
There are several ways of ensuring that this cracking does not occur.
If the phosphate level is high enough in a boiler, all the free hydroxide will be
reacted with to form the harmless compound tri-sodium phosphate. This
needs a very fine degree of chemical control, and while most of the alkalinity
in a boiler will, under correct conditions, be in the form of tri-sodium phos-
phate, inhibitors are usually added to ensure that embrittlement cannot
occur. Three c o m m o n inhibitors are used, sodium sulphate, sodium nitrate,

and quebracho tannins. Providing these are used correctly t h e incidence of
c a u s t i c e m b r i t t l e m e n t , w h i c h i s r a r e i n a n y case, c a n b e d i s c o u n t e d .
T h e Production of Glean S t e a m Free f r o m Entrained Water or Solids

T h e p r e v e n t i o n o f p r i m i n g , o r c a r r y o v e r , i n boilers d e p e n d s u p o n t h r e e
main factors:—
(a) T h e d i s s o l v e d solids c o n c e n t r a t i o n i n t h e w a t e r .
(b) T h e p r e s e n c e of f o a m p r o d u c i n g solids.
(c) T h e d e g r e e a n d s e v e r i t y of l o a d fluctuations.
A boiler w a t e r c o n t a i n i n g a h i g h solids c o n t e n t is m o r e p r o n e to f o a m
t h a n o n e w i t h a l o w solids w a t e r , a n d to t h i s e n d , t h e solids c o n t e n t of a boiler
water m u s t be kept under control. This is achieved by means of blowdown.
All feed w a t e r will c o n t a i n s o m e dissolved solids, a n d o b v i o u s l y , if s t e a m free
from e n t r a i n e d solids i s b e i n g p r o d u c e d , t h e solids will c o n c e n t r a t e i n t h e
boiler w a t e r . To c o u n t e r a c t t h i s , s o m e of t h e boiler w a t e r is b l o w n d o w n o u t of
t h e boiler, a n d r e p l a c e d b y low solids feed. T h e a m o u n t o f b l o w d o w n neces-
s a r y will t h u s o b v i o u s l y d e p e n d u p o n t h e solids c o n t e n t o f t h e feed w a t e r a n d
t h e a c c e p t a b l e solids level i n t h e boiler. B l o w d o w n s h o u l d b e k e p t t o a
m i n i m u m , a s s t r e s s e d before, t o a v o i d c h e m i c a l losses, a n d t h e r e f o r e t h e solids
content of the feed water should be kept to a m i n i m u m . Yet another reason
for t h e u s e of u n c o n t a m i n a t e d c o n d e n s a t e for feed.
T h e a l l o w a b l e solids level in a boiler will v a r y w i t h t h e t y p e of boiler in
use a n d t h e c o n d i t i o n s u n d e r w h i c h i t o p e r a t e s . T h e n e w e r w a t e r wall boilers
o f h i g h h e a t l o a d i n g will n o t t o l e r a t e t h e solids level a c c e p t a b l e i n t h e o l d e r
t y p e s o f boiler a n d m u s t b e w a t c h e d m o r e carefully, p a r t i c u l a r l y u n d e r c o n -
d i t i o n s o f f l u c t u a t i n g l o a d . F l u c t u a t i n g l o a d causes v a r i a t i o n s i n h e a t t r a n s f e r
across t h e boiler h e a t i n g surface a n d v a r i a t i o n s i n p r e s s u r e i n t h e boiler d r u m .
A s u d d e n i n c r e a s e in l o a d c a u s e s d r u m p r e s s u r e to d r o p w h i c h r e s u l t s in a
r a p i d rise in w a t e r level, w h i c h , if severe, c a n c a u s e c o n s i d e r a b l e p r i m i n g .
T h e m a i n f o a m p r o d u c i n g c o n d i t i o n s a r e excessive a l k a l i n i t y a n d t h e
p r e s e n c e o f oil. E x c e s s i v e a l k a l i n i t y c a n b e a v o i d e d b y c h e m i c a l c o n t r o l a n d
t h e i n c i d e n c e o f oil s h o u l d b e k e p t t o a m i n i m u m b y e l i m i n a t i n g oil c o n t a m i n -
a t i o n of t h e s t e a m as far as possible. S o m e of t h e oil u n a v o i d a b l y fed to a
boiler will b e c a r r i e d d o w n w i t h t h e a l k a l i - p h o s p h a t e p r e c i p i t a t e , b u t oil
c o n t a m i n a t i o n s h o u l d b e m i n i m i z e d a s i t h a s a n o t h e r serious effect. Oil
globules c a n a t t a c h t h e m s e l v e s t o t h e h e a t i n g surfaces o f t h e boiler. I f t h i s
occurs, t h e h e a t transfer resistance at this point increases m a r k e d l y a n d t h e
t u b e m a y o v e r h e a t a n d fail. S o m e t i m e s a n t i - f o a m c h e m i c a l s , u s u a l l y c o m p l e x
polyamides or polyoxides, are introduced into t h e boiler to reduce t h e danger
of f o a m i n g .
B l o w d o w n f r o m a boiler also s e r v e s t o r e m o v e t h e alkali p h o s p h a t e
p r e c i p i t a t e , s o t h a t b l o w d o w n p o i n t s a r e p l a c e d a t t h e l o w e s t levels i n t h e
boiler. T h e s e p o i n t s a r e o p e n e d a t i n t e r v a l s , t h e f r e q u e n c y a n d i n t e r v a l o f
opening depending upon the a m o u n t of blowdown required. In some of the
m o d e r n b o i l e r s a c o n t i n u o u s b l o w d o w n i s i n s t a l l e d a s well, u s u a l l y i n t h e t o p
d r u m , t o effect c o n t i n u o u s r e m o v a l o f s o m e o f t h e h i g h solids w a t e r .
Sampling, Methods of Analysis and Chemical Dosage
B . S . 1328 " M e t h o d s o f S a m p l i n g W a t e r u s e d i n I n d u s t r y " c o v e r s t h e
s u b j e c t o f s a m p l i n g fully a n d i t will suffice t o s a y t h a t t h e w a t e r i n e a c h boiler
m u s t b e s a m p l e d s e p a r a t e l y a n d t h e s a m p l e cooled before collecting. Coil t y p e
coolers a r e u s u a l l y u s e d for t h i s p u r p o s e . T h e s a m p l e i s g e n e r a l l y t a k e n from
T H E B O I L E R STATION
the boiler shell or from the water gauge. The sampling container should be a
closed vessel, for accuracy of sulphite results, and it is axiomatic that the
water from the sampling point should be allowed to run for a sufficient time
before the sampling commences, to ensure that a representative sample is
obtained.
For good control it is recommended that the samples should be analysed,
at least once a day, for: —
Alkalinity,
Phosphate,
Sulphite,
Hardness,
Total Dissolved Solids
Determination of pH at more frequent intervals can indicate whether any
abnormal incidence of contamination has occurred.
If sulphate is used for caustic embrittlement control, the sulphate to
caustic ratio should be determined periodically.
The methods of carrying out these analyses and the levels recommended
in the boiler may vary slightly between treatment systems, but can be
generally stated as follows:—
Alkalinity—This is best determined by titration, as this is a more accu-
rate and sensitive method than pH measurement, although pH is useful for
quick checks on boiler conditions. There are several methods of carrying out
alkalinity titrations and the limits of alkalinity set out in the treatment being
used should be adhered to. A minimum alkalinity is required for acidity
control and for the correct operation of the alkali-phosphate treatment. This
usually coincides with an alkalinity, to phenolphthalein, of approximately
150 p.p.m. expressed as CaC0 3 . A maximum alkalinity is obviously set to
avoid foaming, and this is normally at about 800 p.p.m. of total alkalinity.
These figures coincide with a pH range of approximately 10.5 to 11.5.
Phosphate—Once again set limits vary a little but a figure of 50 to 60
p.p.m. expressed as P 0 4 is normal. Excess phosphate is not harmful except
in that it adds solids to the water.
Sodium sulphite—The limits necessary for this compound to act effect-
ively depend upon the reaction time available and whether or not a catalysing
agent is used. Sodium sulphite takes a definite time to absorb oxygen depend-
ing on the temperature and, if possible, the reaction should have time to
proceed before the feed enters the boiler. The sulphite is thus best added well
back in the feed system, but should be added after the system is vented.
Adding sulphite before venting results in wastage of chemicals, because the
sulphite will absorb oxygen which would have been removed in any case by
venting. The rate of reaction can be speeded up by two methods, an increase
of sulphite concentration and the presence of a catalyst (usually a cobalt salt)
with the sulphite. The first method has the only objection that the solids
content of the boiler is increased and more sulphite is lost in blowdown,
while the catalyst has the drawback t h a t the sulphite must sometimes be
added and given time to react before the caustic is added, as high alkalinity
may precipitate certain types of catalyst. With the first method a sulphite
reserve of 100 to 200 p.p.m. as Na 2 S0 3 , is usually kept in the boiler,
while with the second method a minimum reserve of some 40 p.p.m. is kept.
The analysis for sulphite is a titration method which is a little more complex
than an alkalinity determination, and is based on an iodimetric titration using
starch as an indicator.
Hardness—If t h e a l k a l i n i t y level a n d p h o s p h a t e level a r e c o r r e c t , boiler

w a t e r h a r d n e s s will always be zero. A s o a p m e t h o d is sufficiently a c c u r a t e for
t h i s d e t e r m i n a t i o n , a n d i t i s m e r e l y u s e d a s a d o u b l e c h e c k for p h o s p h a t e
a n d alkalinity.
Total Dissolved Solids—This is m o s t c o n v e n i e n t l y d e t e r m i n e d as a r o u t i n e
m a t t e r b y u s i n g a special t y p e o f h y d r o m e t e r . T h i s m e t h o d s h o u l d b e c h e c k e d
p e r i o d i c a l l y by a l a b o r a t o r y m e t h o d i n v o l v i n g t h e e v a p o r a t i o n of a s a m p l e
o f w a t e r a n d w e i g h i n g t h e r e s i d u e . T h e l i m i t s for t o t a l dissolved solids v a r y ,
a s s t a t e d before, d e p e n d i n g o n t h e t y p e o f boiler, t y p e o f w a t e r , s t e a d i n e s s
o f t h e l o a d a n d use o f a n t i f o a m . T h e m a n u f a c t u r e r ' s r e c o m m e n d a t i o n s s h o u l d
b e a d h e r e d t o i n t h i s case. A n t i f o a m s , w h e n used, a r e n o r m a l l y a d d e d i n a
fixed r a t i o t o feed w a t e r f l o w .
Caustic Embrittlement Control—Where t a n n i n s a r e u s e d t h e s e a r e n o r -
m a l l y a d d e d w i t h , a n d i n a fixed p r o p o r t i o n t o p h o s p h a t e . N i t r a t e , w h e n
used, is a d d e d so t h a t t h e ratio of n i t r a t e to alkalinity is a certain m i n i m u m
figure. T h e s a m e i s t r u e o f s u l p h a t e . T h e r a t i o o f s o d i u m s u l p h a t e t o c a u s t i c
soda should be a m i n i m u m of 2.5. A n y sulphate required, additional to t h a t
produced by the oxidation of sulphite, is added as sodium sulphate. These
n i t r a t e a n d sulphate tests need normally only be done occasionally a n d
a r e often c a r r i e d o u t , a s a service, b y t h e c h e m i c a l t r e a t m e n t s u p p l i e r .
T h e a n a l y s e s r e q u i r e d for t h e s e d e t e r m i n a t i o n s a r e r a t h e r c o m p l e x i n n a t u r e .
D e t a i l s of s i m p l e m e t h o d s of a n a l y s i s for a l k a l i n i t y , p h o s p h a t e , s u l p h i t e ,
h a r d n e s s , t o t a l dissolved solids, a n d s u l p h a t e will b e f o u n d i n t h e r e l e v a n t
c h a p t e r o f t h i s m a n u a l a n d f u r t h e r i n f o r m a t i o n c a n b e f o u n d i n B . S . 1427
a n d B.S. 2690. O t h e r suitable l a b o r a t o r y m e t h o d s m a y be used at t h e discre-
t i o n of t h e o p e r a t o r .
Methods of Chemical Dosage—Chemicals c a n be a d d e d to a boiler c o n -
t i n u o u s l y o r i n slug doses. I n o r d e r t o m a i n t a i n c h e m i c a l c o n c e n t r a t i o n a t a n
e v e n level, c o n t i n u o u s d o s i n g i s u s e d w h e r e v e r possible. T h u s c a u s t i c s o d a ,
s o d i u m s u l p h i t e a n d a n t i f o a m (where used) a r e n o r m a l l y d o s e d c o n t i n u o u s l y .
I f t h e s o d i u m s u l p h i t e i s n o t u s e d w i t h a c c e l e r a t o r all t h r e e c h e m i c a l s
c a n b e m i x e d t o g e t h e r a n d a d d e d c o n t i n u o u s l y after t h e feed v e n t . I f
accelerator is used, t h e sulphite should be added, by a separate dosing p u m p ,
a s e a r l y i n t h e s y s t e m a s possible, a n d t h e c a u s t i c a d d e d j u s t before t h e feed
e n t e r s t h e boiler. T h e q u a n t i t i e s a d d e d a r e c a l c u l a t e d from t h e a n a l y s e s o f ,the
w a t e r a n d b a s e d o n e s t i m a t e d d e m a n d . Sufficient c h e m i c a l s for t h e n e x t 2 4
hours are usually mixed in a predetermined q u a n t i t y of water, and the dosing
p u m p set to deliver this volume in t h e 24 h o u r period.
U n f o r t u n a t e l y , p h o s p h a t e c a n n o t b e a d d e d c o n t i n u o u s l y t o t h e feed
lines, a s u n d e r t h e s e c i r c u m s t a n c e s , c a l c i u m p h o s p h a t e c a n b e p r e c i p i t a t e d
i n t h e feed lines t h u s g r a d u a l l y b l o c k i n g t h e m . A h i g h p r e s s u r e slug d o s i n g
p u m p , w i t h individual connections t o e a c h boiler, i s n o r m a l l y u s e d t o a d d
p h o s p h a t e a c c o r d i n g t o e a c h b o i l e r ' s d e m a n d . T h i s p u m p i s also c o n v e n i e n t l y
u s e d t o a d d c a u s t i c o r s u l p h i t e t o i n d i v i d u a l boilers t o m a i n t a i n b a l a n c e d
c o n c e n t r a t i o n s b e t w e e n boilers, i f t h e y v a r y d u e t o v a r y i n g l o a d o r feed
c o n d i t i o n s . S l u g d o s a g e o n c e in 24 h o u r s is n o r m a l l y sufficient, b u t if t h i s is
n o t so, a p H a n d t o t a l dissolved solids c h e c k c a n b e t a k e n once a shift, t o
decide w h e t h e r a n y t h i n g abnormal has occurred, and further action t a k e n
if r e q u i r e d .
P r o b l e m s of Boiler Feed Treatment Peculiar to the Sugar Industry
T h e r e a r e c e r t a i n p r o b l e m s o f boiler feed t r e a t m e n t w h i c h a r e p e c u l i a r
t o t h e s u g a r i n d u s t r y . A s well a s h a v i n g t o c o n t e n d w i t h t h e u s u a l c o n t a -
minants, such as scale-forming compounds and oxygen, contamination of

condensates by the material being processed may be caused by leaking heater
tubes, and other faults. This results in sugar entering the feed water and,
unfortunately, from the point of view of boiler feed treatment, this is most
undesirable. Sugar and reducing sugars, under the influence of heat, break
down in solution to form a series of acidic compounds known collectively as
saccharic (or sugar) acids. It has been stressed, in the section under corrosion,
that acid conditions are most corrosive to steel. Sugar contamination to any
extent can result in very acid conditions in the boiler, and this will cause
serious corrosion. To counteract the acidity from sugar contamination
more caustic soda must be added to the boiler, resulting in increased, and
sometimes dangerously high, solids levels in the boiler. This can cause carry-
over of water and solids. Cases of serious turbine trouble, due to carbon and
other products building up on the turbine blades, are not unknown. The
elimination of sugar contamination is therefore most important. To this end
checks for sugar must be made regularly on the feed water and, if sugar in
any significant concentration is found, the source must be located by further
testing. The most serious contamination can be obtained from a split juice
heater tube, as the juice in the heater is under pressure, and this can lead to
gross contamination of condensates. Leaking effet and pan tubes can, of
course, cause serious trouble, but this normally only occurs when the effets
or pan concerned are shut down.
Condensate checking can be carried out by various chemical means,
from the simple, roughly quantitative alpha-naphthol test, to the more
precise and complex methods. Obviously an instrument to monitor condensate
contamination continuously, is the ideal answer. Various instruments using
chemical methods have been developed for this purpose but, as yet, they are
slow in reaction and rather tedious to maintain. Sugar contamination in a
raw sugar factory is always in the form of impure solutions which carry other
materials besides sugar. Many of these impurities are electrolytes, that is,
they are ionized in solution, and are conductors of electric current. Thus the
conductivity of a condensate can be a guide to its sugar content. At present
sizeable contamination can be detected in this way, and the method can be
used in conjunction with a multipoint conductivity recorder, which can
monitor every source of boiler feed in rapid succession, and operate automatic
valves to divert any contaminated condensate away from boiler feed.
It can therefore be seen that for a sugar mill, the boiler feed should
consist mainly of hot, un-contaminated exhaust steam condensate. Some
make-up is always required and the make-up water should ideally be hot,
to avoid dissolved oxygen, and as free from contamination as possible, to
avoid scaling problems. The best source of make-up is usually the condensate
from the steam space of the second effet vessel. This water is hotter and
usually less contaminated with entrained juice than is water from vessels
further down the set. At times, cold, raw water must be used as make-up.
If possible, this should be heated and vented before pumping to the feed
tank, so that the entry of dissolved oxygen is reduced to a minimum. The use
of raw water can also be minimized by the provision of a reasonable amount
of feed storage, as this can tide the boilers over short mill stops. A storage
capacity approaching an hour's feed supply is desirable, if possible, and raw
water should only be added once this storage is exhausted.
If boiler water conditions are maintained correctly, at all times, the
incidence of corrosion should be negligible, and the cleaning of boiler tubes
completely avoided.
CHAPTER X I I I
FIRST AID
Shock
Shock occurs with all injuries to a greater or lesser extent and may be
serious enough to cause death. The symptoms are paleness, moist skin and
trembling, and an expression of extreme anxiety. Keep the patient warm
and cover with blankets or coats. The patient should lie flat, preferably with
a pillow or two under the lower limbs. Lowering the head is usually un-
comfortable and not always essential. Do not move unnecessarily. Do not give
fluids of any kind by mouth. Remove from danger, check haemorrhage, make
comfortable. Await ambulance.
Electric Shock
Quickly switch off the current or cautiously remove contact from the
patient with an insulator, e.g., a dry stick or dry towel. Start artificial
respiration and external cardiac massage immediately (see later). Keep the
patient warm with blankets and jars of hot water. Do not regard early rigidity
as a sign for ceasing artificial respiration. It should be maintained for at least
four hours.
Heat Exhaustion
After it is certain that the patient has collapsed due to heat exhaustion,
plenty of cold water in which a salt tablet has been dissolved may be given,
provided the patient is not nauseous or vomiting. Removal to hospital is
imperative.
Fainting
The patient should lie flat as indicated under "Shock". Loosen the
clothing round the patient's neck and see that he gets plenty of fresh air.
Sprinkle face and chest with cold water. Give stimulants when the patient
can swallow.
Burns
Dry Heat and Scalds—In the treatment of burns the main object is to
exclude the air as quickly as possible from the injured part. For minor burns
wash with plenty of soap and water. For such burns on the face and hands
apply dressings with gauze or lint impregnated with sterile vaseline. On other
parts of the body burns should be covered with tannic acid jelly. No dressing
should be applied and cloths must not be replaced until the coagulum is dry.
For serious burns apply sterile vaseline on gauze and remove to hospital.
Acid—Wash immediately and thoroughly with cold water and then with
dilute sodium bicarbonate solution. Apply picrate or boric ointment or
acriflavine solution.
Alkali—Wash immediately with large quantities of water then with a
five per cent solution of acetic acid. Dress with picrate or boric ointment or
sterile vaseline.
Prepared in collaboration with the Division of Industrial Medicine, Department of

Health.
182 FIRST AID
Burns in the Eyes—Flush immediately with large quantities of water.

Irrigation of the eye should be continued for at least ten minutes, and often
for longer periods after alkali splashes. Cover eye, refer to hospital for further
treatment.
Wounds
Even severe bleeding may be stopped by the application of a very firm
pressure bandage over the wound. A tourniquet should only be applied if
it is obvious that the wound is unmanageable. If the wound is on the arm,
leg, hand or foot and the blood is scarlet, apply the tourniquet four inches
below the armpit or four inches below the groin. If the blood is dark and
purplish apply the tourniquet below the wound. A piece of rubber tubing or
a necktie will make a good tourniquet. NOTE—Under no conditions should
the tourniquet be held tight for longer than 15 minutes at a time. Loosen it
and allow blood to flow for a few seconds, then retighten it. Loosen but do
not remove the tourniquet as soon as the blood clots.
If the bleeding is copious and the wound is in a position where a tourni-
quet cannot be applied, place a pad of sterile gauze, soaked with acriflavine
in the wound and apply a bandage.
For slight cuts, clean the wound with acriflavine solution (1 in 1000)
and apply a dressing of this material.
General: All cases must be removed to hospital as soon as possible after
first aid treatment is carried out.
Poisoning
Strong Acids—Mouth and lips may be stained. Do not induce vomiting.
Give magnesium oxide, milk of magnesia or lime water immediately. Repeat
at short intervals and wash out the mouth with one of the above materials.
Do not give carbonates but milk or white of egg should be given. Combat
collapse by placing patient in reclining position, and applying blankets, hot
water bottles, etc.
Alkalies—Mouth and lips may be stained. Do not induce vomiting, but
give a five per cent solution of acetic acid, or vinegar until the alkali appears
to be neutralised. Give white of egg or milk and combat collapse.
Note—Cream or any vegetable oil may be given in each case.
Carbolic Acid—Give milk or vegetable oil, induce vomiting, repeat oil,
remove to hospital.
Cyanide—Speed is essential.
A doctor should be telephoned immediately and advised that intra-
venous antidotes and the necessary syringes are held by the laboratory
concerned if such is the case. Unless cyanide accidents are more than a remote
possibility, it should not be necessary to hold ampoules of the antidotes, but
the capsules described hereunder are essential.
If cyanide has been swallowed or if the patient has been poisoned in a
contaminated atmosphere, observe the following procedure:—
(1) Remove patient immediately to uncontaminated atmosphere.
(2) Break capsule of amyl nitrite under the patient's nose every five (5)
minutes.
(3) Inject ten ml of sodium nitrite three per cent intravenously, followed
immediately by 50 ml of sodium thiosulphate 25 per cent.
FIRST AID 183
(4) Artificial respiration must be maintained continuously if patient is

not breathing.
Phosphorus—Induce vomiting, give four oz of mineral oil, followed by
saline purge, e.g. Epsom salts. Note—To induce vomiting, give fairly large
amount of milk, water, coca-cola etc. and push finger far down back of tongue.
Gases and Fumes
Corrosive Gases—Carry the patient into fresh air and apply artificial
respiration if necessary. Combat collapse. Give oxygen if available.
Carbon Monoxide, Hydrogen Sulphide and Nitrous Fumes—Remove the
patient to fresh air. Apply artificial respiration and give oxygen. Combat
collapse.
Artificial Respiration
Artificial respiration may be applied in any circumstances where the
patient has ceased to breathe, e.g., drowning, electrocution, cyanide poison-
ing, gassing or other causes.
Mouth-to-mouth resuscitation is the most effective method and may be
applied as follows:—
Place patient on his back and rapidly clear obstructions in the mouth.
Stretch the neck by tilting the head back as far as possible.
Hold the head back at all times.
Pinch nostrils closed with thumb and fore-finger of one hand and keep
the jaw open and the chin up with the other hand.
Take a deep breath, open your mouth wide, and seal your lips around
the patient's mouth.
Blow air into the patient and watch to see that his chest rises.
If this does not happen, tilt the head further and lift the chin up again.
If the chest rises, remove your mouth and the patient's chest will collapse.
Continue inflation in this way at least ten to 12 times a minute.
External Cardiac Massage
If the patient is unconscious, not breathing and apparently pulseless,
immediately initiate both mouth-to-mouth resuscitation as above, and car-
diac (heart) massage. Place patient face up. Get someone else to proceed with
mouth-to-mouth resuscitation. Kneel beside patient. Apply palm of one hand
over the bottom of the chest plate (breast bone). Bring palm of the other hand
on top of the first. Now bring your weight rhythmically down at about a rate
of 50 to 60 times a minute. Continue for 20 minutes.
Foreign Body in the Eye
If possible remove with corner of a clean handkerchief, but use great
care; if not, wash out with boracic lotion. Apply a pad and bandage firmly
to prevent movement of the eyelid. If the surface of the eyeball is injured
use only irrigation and send for a doctor.
Alternate treatment—Apply eyedrops of albucid soluble ten per cent in
water (sodium sulphacetamide) by pulling forward lower lid and using a small
rubber sponge. Remove foreign body with the sponge if possible. If this fails
apply a pad and bandage as before and send for expert treatment. If the
surface of the eyeball is injured apply the albucid drops, the pad and bandage,
and send for a doctor.
REFERENCE T A B L E S
Table No. TITLE Page
I Temperature Corrections to Readings of Brix Hydrometers (Cali-
brated at 20 °C.) 186
II Schmitz's Table for Sucrose (Pol) in Juice for Use in the Dry Lead
Method with Undiluted Solutions. Normal Weight of 26.000 g. 188
III Pol Bagasse from Polariscope Reading (400 mm Tube) and Moisture
Content. (Ratio of water to bagasse =10:1). (Clarified with dry lead). 193
IV Milligrammes of Reducing Sugars Required to Reduce 10 ml Feh-
ling's Solution (Lane and Eynon Method). 195
V Milligrammes of Reducing Sugars Required to Reduce 10 m
Fehling's Solution (Lane and Eynon Method) at Low Sucrose
Concentrations. To be Used with the Chemical Method of Sucrose
Analysis. 196
VI Specific Rotation of Sugars. 197
VII Refractive Indices of Sugar Solutions at 20 °C in Air at 20 °C,
760 mm Pressure and 50 per cent Relative Humidity. 198
VIII International Table of Temperature Corrections for the Abbe Re-
fractometer Calibrated at 20 °C. 199
IX Clerget Divisors. 200
X Subtractive Temperature Corrections for Clerget Divisors. 200
XI Dilution Indicator of Raw Sugar. 201
XII Solubility of Sucrose in Water in g Sucrose (S) per 100 g Water
According to Charles, Amer. Chem. S o c , 1958 Abst. of Papers
p. 100. Reported in Honig "Principles of Sugar Technology", 2, 228. 201
XIII Solubility of Sucrose in Water in g Sucrose (S) per 100 g Solution 202
(Charles).
XIV Densities of Solutions of Cane Sugar at 20 °C in g/ml. (This table
is the basis for standardizing hydrometers indicating per cent of
sugar at 20 °C). 203
XV Brix, Apparent Density, Apparent Specific Gravity, and Grammes
of Sucrose per 100 ml of Sugar Solutions. (NBS—C440, 1942, p. 632). 206
XVI Weight per Unit Volume of Sugar Solutions at 20 °C. 216
XVII Degree of Supersaturation—All Values Being Prefixed by 1. 217
XVIII Crystal Content of Massecuites. 218
X I X (a) Stock Recovery. 219
X I X (b) Stock Recovery. 220
X I X (c) Stock Recovery. 221
XX Factors to be Used in Calculating Weight per Gallon of Molasses. 222
XXI Weights as Decimals of Ton. 222
XXII Density (g/ml) of Water at Temperatures from 0 to 102 °C. Ac-
cording to M. Thiesen, Wiss. Abh. der Physikalisch-Technischen
Reichsanstalt, 4, No. 1; 1904. 223
XXIII Corrections for Temperature (in g) to Be Added to Weight of Water
Contained to Obtain Volume (in ml) of Vessel at 20 °C. Nominal
Capacity 1,000 ml. (For vessels made of soda glass). 224
R E F E R E N C E TABLES
Table No.
XXIV Corrections for Atmospheric Pressure (in g) to Be Added to or Sub-
tracted from the Weight of Water Contained to Obtain Volume
(in ml) of Vessel at Standard Temperature and Pressure. 225
XXV Requirements for Apparatus for Use in the Analysis of Cane for
Payment Purposes. 226
XXVI Properties of Saturated Steam. 229
XXVII Temperature Conversion Table. 231
XXVIII Equivalents
Volume and Capacity Equivalents.
Mass Equivalents.
Density Equivalents.
Linear Measure Equivalents.
Surface and Area Equivalents.
Pressure Equivalents.
Heat, Energy and Work Equivalents.
Heat Flow Equivalents. 232
XXIX Mensuration of Surfaces and Solids. 234
XXX Circles: Diameters, Areas, Circumferences. 235
XXXI Capacities of Vertical Cylindrical Tanks (UK gal). 235
XXXII Capacities of Rectangular Tanks (UK gal) for Each Foot of Depth. 236
XXXIII Capacity of Horizontal Cylindrical Tanks at Varying Levels. 237
i = depth of liquid,
d = diameter of vessel.
XXXIV Amount of CaO in Milk of Lime of Various Densities at 15 °C. 237
XXXV Fuel Value of Bagasse. 238
XXXVI Boiling Point Elevation of Sugar Solutions and Cane Juices (°F) at
760 mm Pressure. 239
XXXVII Table for Rapid Filterability Test. 240
XXXVIII International Atomic Weights, 1966 (Published by the C.R.C.
Handbook of Chemistry and Physics). 242
Table I—Temperature Corrections to Readings of Brix Hydrometers (Calibrated at 20 °C) £
Temperature °C Observed per cent of sugar

'
0 5 10 15 20 25 30 35 40 45 50 55 60 65 70 75 80 85 90
Subtract from observed per cent.
0 0.30 0.49 0.65 0.77 0.89 0.99 1.08 1.16 1.24 1.31 1.37 1.41 1.44 1.47 1.49 1.50 1.50 1.51 1.51
5 0.36 0.47 0.56 0.65 0.73 0.80 0.86 0.91 0.97 1.01 1.05 1.08 1.10 1.12 1.14 1.16 1.17 1.18 1.19
0 0.32 0.38 0.43 0.48 0.52 0.57 0.60 0.64 0.67 0.70 0.72 0.74 0.75 0.76 0.77 0.78 0.79 0.80 0.81
1 0.31 0.35 0.40 0.44 0.48 0.51 0.55 0.58 0.60 0.63 0.65 0.66 0.68 0.69 0.70 0.71 0.72 0.73 0.74
12 0.29 0.32 0.36 0.40 0.43 0.46 0.50 0.52 0.54 0.56 0.58 0.59 0.60 0.61 0.62 0.63 0.64 0.64 0.65
13 0.26 0.29 0.32 0.35 0.38 0.41 0.44 0.46 0.48 0.49 0.51 0.52 0.53 0.54 0.55 0.56 0.56 0.57 0.57
14 0.24 0.26 0.29 0.31 0.34 0.36 0.38 0.40 0.41 0.42 0.44 0.45 0.46 0.46 0.47 0.47 0.48 0.48 0.48
15 0.20 0.22 0.24 0.26 0.28 0.30 0.32 0.33 0.34 0.36 0.36 0.37 0.38 0.38 0.39 0.39 0.40 0.40 0.41
16 0.17 0.18 0.20 0.22 0.23 0.25 0.26 0.27 0.28 0.28 0.29 0.30 0.31 0.31 0.32 0.32 0.33 0.33 0.34
17 0.13 0.14 0.15 0.16 0.18 0.19 0.20 0.20 0.21 0.21 0.22 0.23 0.23 0.24 0.24 0.25 0.25 0.25 0.26
18 0.09 0.10 0.10 0.11 0.12 0.13 0.13 0.14 0.14 0.14 0.15 0.15 0.15 0.16 0.16 0.16 0.16 0.17 0.17
19 0.05 0.05 0.05 0.06 0.06 0.06 0.07 0.07 0.07 0.07 0.08 0.08 0.08 0.08 0.08 0.09 0.09 0.09 0.09
50 Add to observed per cent.
21 0.04 0.05 0.06 0.06 0.06 0.07 0.07 0.07 0.07 0.08 0.08 0.08 0.08 0.08 0.09 0.09 0.09 0.09 0.09
22 0.10 0.10 0.11 0.12 0.12 0.13 0.14 0.14 0.14 0.15 0.16 0.16 0.16 0.16 0.16 0.17 0.17 0.17 0.17
23 0.16 0.16 0.17 0.17 0.19 0.20 0.21 0.21 0.22 0.23 0.24 0.24 0.24 0.24 0.24 0.25 0.25 0.25 0.25
24 0.21 0.22 0.23 0.24 0.26 0.27 0.28 0.29 0.30 0.31 0.32 0.32 0.32 0.32 0.32 0.33 0.33 0.33 0.33
25 0.27 0.28 0.30 0.31 0.32 0.34 0.35 0.36 0.38 0.38 0.39 0.39 0.40 0.40 0.39 0.39 0.39 0.38 0.38
26 0.33 0.34 0.36 0.37 0.40 0.40 0.42 0.44 0.46 0.47 0.47 0.48 0.48 0.48 0.48 0.49 0.49 0.48 0.48
27 0.40 0.41 0.42 0.44 0.46 0.48 0.50 0.52 0.54 0.54 0.55 0.56 0.56 0.56 0.56 0.57 0.57 0.56 0.56
28 0.46 0.47 0.49 0.51 0.54 0.56 0.58 0.60 0.61 0.62 0.63 0.64 0.64 0.64 0.64 0.65 0.65 0.64 0.64
29 0.54 0.55 0.56 0.59 0.61 0.63 0.66 0.68 0.70 0.70 0.71 0.72 0.72 0.72 0.72 0.73 0.73 0.72 0.72
JO 0.61 0.62 0.63 0.66 0.68 0.70 0.73 0.76 0.78 0.78 0.79 0.80 0.80 0.80 0.81 0.81 0.81 0.81 0.81
M 0.69 0.70 0.71 0.74 0.76 0.79 0.82 0.84 0.86 0.87 0.88 0.88 0.89 0.89 0.89 0.89 0.89 0.89 0.89
12 0.76 0.78 0.79 0.82 0.85 0.87 0.90 0.93 0.95 0.95 0.96 0.97 0.97 0.97 0.97 0.97 0.97 0.97 0.97
J3 0.84 0.85 0.87 0.90 0.93 0.96 0.99 1.01 1.03 1.04 1.05 1.05 1.06 1.06 1.06 1.06 1.06 1.06 1.05
\4 0.91 0.93 0.95 0.98 1.02 1.04 1.07 1.10 1.12 1.12 1.13 1.14 1.14 1.14 1.14 1.14 1.14 1.14 1.13
\5 0.99 1.01 1.02 1.06 1.10 1.13 1.16 1.18 1.20 1.21 1.22 1.22 1.23 1.23 1.22 1.22 1.22 1.22 1.21
Table I—continued.
Tmperature Observed per cent of sugar

°C
0 5 10 15 20 25 30 35 40 45 50 55 60 65 70 75 80 85 90
Add to observed per cent.
1.07 1.09 1.12 1.15 1.19 1.22 1.25 1.27 1.29 1.30 1.31 1.31 1.32 1.32 1.31 1.31 1.30 1.30 1.29
p 1.15 1.17 1.21 1.24 1.28 1.31 1.34 1.36 1.38 1.39 1.39 1.39 1.40 1.40 1.39 1.39 1.39 1.39 1.38
1.24 1.26 1.29 1.33 1.36 1.39 1.42 1.44 1.46 1.47 1.48 1.48 1.49 1.49 1.48 1.48 1.47 1.47 1.46
1.33 1.35 1.38 1.42 1.45 1.48 1.51 1.53 1.55 1.56 1.56 1.56 1.57 1.57 1.56 1.56 1.56 1.56 1.55
1.42 1.45 1.47 1.51 1.54 1.57 1.62 1.62 1.64 1.65 1.65 1.65 1.66 1.66 1.65 1.65 1.64 1.64 1.63
1.51 1.54 1.56 1.60 1.63 1.67 1.69 1.71 1.73 1.74 1.74 1.74 1.75 1.75 1.74 1.73 1.72 1.72 1.71
1.61 1.64 1.66 1.70 1.73 1.76 1.79 1.81 1.82 1.83 1.83 1.83 1.84 1.83 1.82 1.82 1.81 1.80 1.79
1.71 1.74 1.76 1.80 1.83 1.86 1.88 1.90 1.92 1.92 1.92 1.92 1.92 1.92 1.91 1.90 1.89 1.89 1.88
1.81 1.84 1.86 1.90 1.93 1.95 1.98 2.00 2.01 2.01 2.01 2.01 2.01 2.00 1.99 1.99 1.98 1.97 1.96
1.91 1.94 1.96 2.00 2.03 2.05 2.07 2.09 2.10 2.10 2.10 2.10 2.10 2.09 2.08 2.07 2.06 2.05 2.04
2.01 2.05 2.07 2.11 2.14 2.15 2.17 2.19 2.20 2.20 2.20 2.19 2.19 2.18 2.17 2.16 2.14 2.13 2.12
2.12 2.16 2.18 2.21 2.24 2.26 2.27 2.29 2.30 2.29 2.29 2.29 2.28 2.27 2.26 2.24 2.23 2.21 2.20
2.23 2.26 2.28 2.32 2.35 2.36 2.38 2.39 2.39 2.39 2.39 2.39 2.38 2.36 2.34 2.33 2.31 2.30 2.28
2.35 2.37 2.39 2.42 2.45 2.47 2.48 2.49 2.49 2.48 2.48 2.48 2.47 2.45 2.43 2.41 2.40 2.38 2.36
2.46 2.48 2.50 2.53 2.56 2.57 2.58 2.59 2.59 2.58 2.58 2.57 2.56 2.54 2.52 2.50 2.48 2.46 2.44
2.58 2.60 2.62 2.64 2.67 2.68 2.69 2.69 2.69 2.68 2.68 2.67 2.65 2.63 2.61 2.59 2.57 2.54 2.52
2.70 2.72 2.74 2.76 2.78 2.79 2.80 2.80 2.79 2.78 2.78 2.76 2.75 2.72 2.70 2.68 2.65 2.63 2.60
2.81 2.83 2.85 2.87 2.90 2.90 2.90 2.90 2.90 2.88 2.87 2.86 2.84 2.82 2.79 2.76 2.74 2.71 2.69
2.93 2.95 2.97 2.99 3.01 3.01 3.01 3.01 3.00 2.98 2.97 2.95 2.94 2.91 2.88 2.85 2.82 2.80 2.77
3.05 3.07 3.09 3.12 3.12 3.12 3.12 3.11 3.10 3.08 3.07 3.05 3.03 3.00 2.97 2.94 2.91 2.88 2.85
3.18 3.20 3.22 3.23 3.24 3.24 3.23 3.22 3.20 3.18 3.17 3.15 3.12 3.09 3.06 3.03 3.00 2.97 2.93
3.31 3.33 3.35 3.35 3.36 3.35 3.34 3.33 3.31 3.29 3.27 3.25 3.22 3.19 3.15 3.12 3.09 3.05 3.02
3.43 ! 3.46 3.47 3.48 3.48 3.47 3.45 3.43 3.41 3.39 3.37 3.34 3.31 3.28 3.25 3.21 3.17 3.14 3.10
3.56 ! 3.59 3.60 3.60 3.60 3.58 3.56 3.54 3.52 3.50 3.47 3.44 3.41 3.38 3.34 3.30 3.26 3.22 3.19
3v69 3.72 3.73 3.73 3.72 3.70 3.67 3.65 3.62 3.60 3.57 3.54 3.50 3.47 3.43 3.39 3.35 3.31 3.27
This table is calculated using the data on thermal expansion of sugar solutions by Plato assuming the instrument to be of Jena 16111 glass.
The table should be used with caution and only for approximate results when the temperature differs much from the standard temperature or
from the temperature of the surrounding air.
Table H—Schmitz's Table for Sucrose (Pol) in Juice for Use in the Dry Lead Method with Undiluted Solutions.
Normal Weight of 26.000 g.
Polariscope Degrees Brix Polariscope
reading reading
10 15 20 2 5 30 3 5 40 4 5 5 0 5 5 6 0 6 5 7 0 7-5 8 0 8-5 9 0 9 5 10 0 10 5 11 0
_
-
2
0-26
0-52
0-26
0-52
026
0-52
026
0-52
0-26
0-62
0-26
0-51
0-26
0-51
0-26
0-51
026
051
0'26
0-51
0-25
0-51
0-25
0-51
0-25
0-51
0-25
0-51
025
0-51
0-25
0-50
0-25
0-60
025
0-50
0-25
0-50
0-25
0-50
0-25
0-50 2
3 0-78 0-78 0-78 0-78 0-77 0-77 0-77 0-77 0-77 0-77 0-76 0-76 0-76 076 0-76 0-76 0-76 0-75 0-75 0-75 0-75 3
4 104 1-04 1-04 103 103 1-03 103 103 102 102 102 102 1-02 1-01 1-01 1-01 1-01 101 1-00 1-00 100 4
5 1-30 130 1-29 129 1-29 1-29 1-28 1-28 1-28 1-28 1-27 1-27 1-27 1-27 1-26 1-26 1-26 1-26 1-25 1-25 1-25 5
6 1-56 1-55 1-55 1-55 1-54 1-54 1-54 1-54 1-53 1-53 1-53 1-52 1-52 1-52 1-51 1-51 151 1-51 1-50 150 6
7 1-82 1-81 1-81 1-81 1-80 1-80 1-80 1-70 1-79 1-78 1-78 1-78 1-77 1-77 1-77 1-76 1-76 1-76 1-75 1-75 7
8 2-07 207 2-06 2-06 2-06 2-05 205 2-04 204 2 04 203 203 202 2 02 2-02 2-01 201 2 00 2-00 8
9 2-33 2-32 232 2-31 2-31 2-30 2-30 2-29 2-29 2-29 2-28 2-28 2-27 2-27 226 2-26 2-25 2-25 9
10 258 2-57 2-57 2-56 2-56 2-55 2-55 2-54 2-54 253 2-53 2-52 2-52 2-51 2-51 2-50 2-50 10
11 2-84 2-83 2-83 2-82 2-82 2-81 2-80 2-80 2-80 2-79 2-78 2-78 2-77 2-77 2-76 275 2-75 11
12 3-09 308 308 3>07 3-07 306 305 3 05 3-04 304 303 302 3 02 3-01 301 300 12
13 3-35 3-34 3-33 333 3-32 3-31 331 3-30 3-29 329 3-28 3-28 3-27 3-26 3-26 3-25 13
14 3-60 3-59 3-58 3-58 3-57 3-56 3'56 3-55 3-54 3-53 353 3-52 3-51 351 3-50 14
15 3-85 3-85 3-84 3-83 3-82 3-82 3-81 3-80 3-79 3-79 3-78 3-77 3-76 3-76 3-75 15
16 4-10 410 4-09 4-08 4-07 406 4-06 4-05 4'04 403 4-02 4-02 401 400 16
17 4-36 4-35 4-34 4-33 433 4-32 4-31 4-30 4-29 4-28 4-27 4-27 4-26 4-25 17
18 4-61 460 4-59 4-58 4-57 4-56 4-55 4-54 4-54 4-53 4-52 4-51 4-50 18
19 4-86 4-85 4-84 4'83 4-82 4-82 4-81 4-80 4-79 4-78 4-77 4-76 4-75 19
20 511 5-10 5-09 508 5-07 5-06 5-05 5-04 5-03 5-02 5-01 500 20
21 5-36 5-35 534 5-33 5-32 5-31 5-30 5-29 5-28 527 5-26 5-25 21
22 5-61 5-60 5-59 5-58 5-56 5-55 554 5-53 5-52 5-51 5-50 22
23 5-86 5-85 5-84 5-83 5-82 5-81 5-79 5-78 5-77 5-76 5-75 23
24 611 6 09 6-08 6-07 6 06 605 6 03 6-02 601 6-00 24
25 6-36 6-35 634 6-32 6-31 6-30 6-29 627 6-26 6-25 25
26 6-60 6-59 6-58 656 6-55 6-54 6-52 6-51 6-50 26
27 6-86 6-84 6-83 6-82 6-80 6-79 6-78 6-76 6-76 27
26 7-10 7-08 707 7-05 7-04 7-03 7-01 700 28
29 7-35 7-34 7-32 7-31 7-29 7-28 7-26 7-25 29
30 7-59 7-57 7-56 7-54 7-53 7-51 7-50 30
31 BRixl-OtolOO 7-84 7-83 7-81 7-79 7-78 7-76 7-75 31
32 8-08 8-06 8 05 803 801 8-00 32
33 Tenths of the Tenths of the 8-33 8-31 8-30 8-28 8-26 8-25 33
34 polariscope Per cent polariscope Per cent 8-57 8-55 8-63 8-52 8-50 34
35 reading sucrose reading sucrose 8-82 8-80 8-78 8-77 8-75 35
36 0-1 0-02 0-6 0-15 9-05 9 03 902 900 36
37 0-2 0-05 0-7 0-18 9-30 9-29 9-27 9-25 37
38 0-3 0-07 0-8 0-20 9-54 9-52 9 5 0 38
39 0-4 0-10 0-9 0-23 9-79 9-77 9-75 39
40 0-5 0-13 1 10-02 10-00 40
Table II—continued.
Polariscope 1 Degr ees Brix Polariscope

reading
readmg 11-5 1 12-0 1 12-5 1 13-0 13-5 14-0 145 15 0 15-5 16 0 16 5 17 0 17-5 18 0 18 5 190 19 5 20 0
1 0-25 0-25 0-25 0-25 0-25 0-25 0-25 1
2 0-50 0-50 0-50 0-50 0-49 0-49 049 2
34 0-75 0-75 0-74 0-74 0-74 0-74 0-74 0 : 74 3
1-00 1-00 0-99 0-99 0-99 0-99 0-99 0-98 0:98 4
1-25 1-24 1-24 1-24 1-24 1-23 1-23 1-23 1-23 5
5
1-50 1-49 1-49 1-49 1-48 1-48 1-48 1-48 1-47 1-47 6
7 1-75 1-74 1-74 1-74 1-73 1-73 1-73 1-72 1-72 1-71 7
8 2-00 1-99 1 1-99 1-98 1-98 1-98 1-97 1-97 1-96 1-96 1-96 8
9 2-24 2-24 2-24 2-23 2-23 2-22 2-22 2-21 2-20 2-20 2-20 9
10 2-49 2-49 2-48 2-48 2-47 2-47 2-46 2-46 2-45 2-45 2-44 2-44 10
11 2-74 2-74 2-73 2-73 2-72 2-72 2-71 2-71 2-70 2-69 2-69 11
12 2-99 2-99 2-98 2-98 2-97 2-96 2-96 2-95 2-95 2-94 2-93 2-93 2 : 92 12
13 3-24 3-24 3-23 3-22 3-22 3-21 3-20 3-20 319 3-18 318 317 317 13
14 3-49 3-49 3-48 3-47 3-46 3-46 3-45 3-44 3-44 3-43 3-42 3-42 3-41 3-40 14
15 3-74 3-73 3-73 3-72 3-71 3-70 3-70 3-69 3-68 3-67 3-67 3-66 3-65 3-64 15
16 3-99 3-98 398 3-97 3-96 3-95 3-94 3-94 3-93 3-92 3-91 3-90 3-90 3-89 3-88 16
17 4-24 4-23 4-22 4-22 4-21 420 4-19 4-18 417 416 4-16 415 414 413 412 17
18 4-49 4-48 4-47 4-46 4-45 4-45 4-44 4-43 4-42 4-41 4-40 4-39 4-38 4-37 4-36 4-'36 18
19 474 4-73 4-72 4-71 4-70 4-69 4-68 4-67 4-66 4-65 4-64 4-64 4-63 4-62 4-61 4-60 19
20 499 1 4-98 4-97 4-96 4-95 4-94 4-93 4-92 4-91 4-90 4-89 4-88 4-87 4-86 4-85 4-84 4-83 20
21 5-24 5-23 5-22 5-21 5-20 5-19 5-18 5-17 5-15 5-14 513 512 511 510 5 09 508 507 21
22 5-49 5-48 5-47 5-45 5-44 6-43 5-42 5-41 5-40 5-39 5-38 5-37 5-36 5-35 5-33 5-32 5-31 5-30 22
23 5-74 5-73 5-71 5-70 5-69 5-67 5-66 565 5-63 5-62 5-61 5-60 5-59 5-58 5-57 5-55 6-54 23
24 6-99 5-97 5-96 5-95 5-94 5-93 5-92 5-90 5-89 5-88 5-87 5-86 5-84 5-83 5-82 5-81 5-80 5-78 24
25 6-24 6-22 6-21 6-20 6-19 6-17 6-16 6-15 614 612 611 610 6-09 6-07 606 605 604 6-02 25
26 6-49 6-47 646 6-45 6-43 6-42 6-41 6-39 6-37 6-36 6-34 6-33 6-32 6-30 6-29 6-28 6-27 26
27 6-74 6-72 6-71 669 6-68 6-67 6-65 6-64 6-63 6-61 6-60 6-59 6-57 6-56 6-55 6-53 6-52 6-51 27
28 6-98 6-97 6-96 6-94 6-93 6-91 6-90 6-89 6-87 6-86 6-85 6-83 6-82 6-80 6-79 6-78 6-76 6-75 28
29 7-23 7-22 7-21 7-19 7-18 7-16 7-15 7-13 7-12 7-10 7-09 7-08 706 7 05 7-03 7-02 7-00 6-99 29
30 7-48 7-47 7-45 7-44 7-42 7-41 7-39 7-38 7-36 7-35 7-33 7-32 7-30 7-29 7-27 7-26 7-24 7-23 30
31 7-73 7-72 7-70 7-69 7-67 7-66 7-64 7-62 7-61 7-59 7-58 7-56 7-55 7-53 7-52 7-50 7-49 7-47 31
32 7-98 7-97 7-95 7-93 7-92 7-90 7-89 7-87 7-85 7-84 7-82 7-81 7-79 7-78 7-76 7-74 7-73 7-71 32
33 8-23 8-22 8-20 8-18 8-17 8-15 8-13 8-12 8-10 8-08 8-07 8-05 8-03 8-02 8-00 7-99 7-97 7-95 33
34 8-48 8-46 8-45 8-43 8-41 8-40 8-38 8-36 8-35 8-33 8-31 8-30 8-28 8-26 8-24 8-23 8-21 819 34
35 8-73 8-71 8-70 8-66 6-64 8-63 8-61 8-59 8-57 8-56 8-54 8-52 8-50 8-49 8-47 8-45 8-43 35
36 8-98 8-96 8-94 8-93 8-91 8-89 8-87 8-85 8-84 8-82 8-80 8-78 8-77 8-75 8-73 8-71 8-69 8-68 36
37 9-23 9-21 919 9-17 9-16 9-14 912 9-10 908 906 9 05 903 901 8-99 8-97 8-95 8-94 8-92 37
38 9-48 9-46 9-44 9-42 9-40 9-38 9-37 9-35 9-33 9-31 9-29 9-27 9-25 9-23 9-21 9-20 918 916 38
39 9-78 9-71 9-69 9-67 9-65 9-63 9-61 959 9-57 9-55 9-53 9-51 9-50 9-48 9-46 9-44 9-42 9-40 39
40 1 9-98 1 9-96 1 9-94 0-92 9-90 9-88 9-86 I 9-84 I 9-82 9-80 9-78 9-76 9-74 9-72 9-70 9-68 9-66 9-64 40
R E F E R E N C E TABLES 191
REFERENCE TABLES
Table IIA—Table of Factors for the Calculation of Pol Per Cent Juice from Pol
Reading for U s e in the Dry Lead Method with Undiluted Solutions
Pol Reading
Pol per cent juice =
Pol Factor
Degrees Factor Degrees Factor

Brix Brix
0.5 3.84273 16.5 4.09450

1.0 3.85023 17.0 4.10285
1.5 3.85769 17.5 4.11119
2.0 3.86519 18.0 4.11962
2.5 3.87273 18.5 4.12804
3.0 3.88027 19.0 4.13650

3.5 3.88785 19.5 4.14496
4.0 3.89546 20.0 4.15350
4.5 3.90308 20.5 4.16204
5.0 3.91077 21.0 4.17062
5.5 3.91842 21.5 4.17923

6.0 3.92615 22.0 4.18788
6.5 3.93388 22.5 4.19658
7.0 3.94165 23.0 4.20527
7.5 3.94942 23.5 4.21400
8.0 3.95723 24.0 4.22277

8.5 3.96512 24.5 4.23158
9.0 3.97296 25.0 4.24042
9.5 3.98088 25.5 4.24931
10.0 3.98881 26.0 4.25819
10.5 3.99677 26.5 4.26712

11.0 4.00473 27.0 4.27608
11.5 4.01277 27.5 4.28508
12.0 4.02081 28.0 4.29412
12.5 4.02885 28.5 4.30315
13.0 4.03696 29.0 4.31227

13.5 4.04508 29.5 4.32138
14.0 4.05327 30.0 4.33054
14.5 4.06146 30.5 4.33973
15.0 4.06965 31.0 4 34896
15.5 4.07792 31.5 4.35823
16.0 4.08619 32.0 4.36750
The values have been calculated to sixteen significant figures and rounded to six significant figures
using the rounding rule in British Standards 1957
NOTE 2.— Due to rounding errors and differences in original data there may be discrepancies in the
second decimal place of pol between values calculated using these factors and those obtained from Table
II. Providing sufficient significant figures are used in the calculation the values obtained using the pol
factors of this table are to be considered the correct results.
Table III'—Pol Bagasse from Polariscope Reading (400 mm Tube) and Moisture Content.
(Ratio of water to bagasse = 10:1). (clarified with dry lead).
Table III—continued.
Table IV—Milligrammes of Reducing Sugars Required to Reduce 10 ml

Fehling's Solution (Lane and Eynon Method).
•Calculated by extrapolation.
196 R E F E R E N C E TABLES
T a b l e V — M i l l i g r a m m e s o f R e d u c i n g S u g a r s Required t o R e d u c e 1 0 m l
Fehling's Solution (Lane a n d Eynon Method) at Low Sucrose
Concentrations.
T a b l e VI—Specific R o t a t i o n of S u g a r s .
T a b l e VII—Refractive I n d i c e s of S u g a r S o l u t i o n s at 20 °G in A i r at
2 0 °G, 760 m m P r e s s u r e a n d 5 0 p e r c e n t R e l a t i v e H u m i d i t y .
The following values are according to t h e smoothed measured values of t h e Physi-
kalisch-Technische Bundesanstalt in West Germany, and have been computed from t h e
polynomial adopted by t h e ICUMSA 1966.
P = sugar concentration as percentage by weight in air at 20 °C 760 mm pressure

and 50 per cent relative humidity.
L a b o r a t o r y M a n u a l for Q u e e n s l a n d S u g a r M i l l s
T a b l e IX—Glerget D i v i s o r s .
W h e n analyses are conducted according to Jackson Gillis Method IV, t h e presently
accepted formula for conversion of polariscope (saccharimeter) readings to sucrose con-
centration is:
where S = sucrose per cent in sample.

P1 = direct reading calculated to basis of normal solution.
P = invert reading calculated to basis of normal solution.
m = concentration of dissolved solids in g per 100 ml of solution as read
in polariscope.
t = temperature in °C.
The basic value 132.63 applies to the Walker method of inversion (heat to 65 ° C ,
a d d acid, allow to cool). For inversion by t h e U.S. Customs method (add acid, immerse
in 60 °C bath, stir for 3 min, hold for 7 more min, cool quickly) t h e basic value is 132.56,
whilst for inversion at room temperature (24 h) the value is 132.66.
For invertase inversion the Clerget divisor is given by t h e formula—
132.1 + 0.0833 (m — 13) — 0.53 (/ — 20).
Using the Walker method of inversion some useful Clerget divisors, at 20 ° C , a r e :
J u i c e s — T h e divisor is related to t h e Brix as follows:
T a b l e IX (a)
S u g a r s — F o r all sugars the value 132. 63 at 20 °C m a y be adopted.

M o l a s s e s — F o r normal samples of molasses t h e value 131.88 at 20 °C m a y be
adopted.
For other materials or other methods of inversion the divisor m u s t be calculated
from t h e specific data. All Clerget divisors must be corrected for temperature according
to t h e table.
T a b l e X — S u b t r a c t i v e T e m p e r a t u r e C o r r e c t i o n s for C l e r g e t D i v i s o r s .
REFERENCE TABLES 201
Table XI—Dilution Indicator of R a w S u g a r .
T a b l e XII—Solubility of Sucrose in Water in g Sucrose (S) per 100 g

Water A c c o r d i n g to Charles, A m e r . C h e m . S o c , 1958 Abst. of P a p e r s p.
10D. Reported in Honig "Principles of S u g a r Technology", 2, 228.
202 REFERENCE TABLES
Table XIII—Solubility of Sucrose in Water in g Sucrose (S) per 100 g

Solution.* (Charles.)
°c S °C S °C S °C S °C S
0 64.41 19 66.47 37 69.45 55 73.11 73 77.15
1 64.48 20 66.61 38 69.64 56 73.33 74 77.38
2 64.56 21 66.75 39 69.83 57 73.55 75 77.60
3 64.64 22 66.90 40 70.02 58 73.77 76 77.83
4 64.73 23 67.05 41 70.22 59 73.99 77 78.06
5 64.82 24 67.21 42 70.41 60 74.21 78 78.29
6 64.92 25 67.36 43 70.61 61 74.43 79 78.52
7 65.02 26 67.52 44 70.81 62 74.66 80 78.75
8 65.11 27 67.69 45 71.01 63 74.88 81 78.97
9 65.22 28 67.85 46 71.21 64 75.10 82 79.20
10 65.33 29 68.02 47 71.42 65 75.33 83 79.43
11 65.44 30 68.19 48 71.63 66 75.56 84 79.66
12 65.56 31 68.36 49 71.84 67 75.78 85 79.88
13 65.68 32 68.54 50 72.05 68 76.01 86 80.11
14 65.80 33 68.72 51 72.26 69 76.24 87 80.33
15 65.93 34 68.89 52 72.47 70 76.46 88 80.56
16 66.06 35 69.08 53 72.68 71 76.69 89 80.78
17 66.19 36 69.26 54 72.90 72 76.92 90 81.01
18 66.33
*Beware of confusion between this Table and Table XII.

Table XIV—Densities of Solutions of Cane Sugar at 20 °C in g/ml.*.
(This table is the basis for standardizing hydrometers indicating per cent of sugar at 20 °C).
Per Tenths of per cent Per

cent
sugar .0 .1 .2 .3 .4 .5 .6 .7 .8 .9 sugar
0 0.998234 0.998622 0.999010 0.999398 0.999786 1.000174 1.000563 1.000952 1.001342 1.001731 0
1 1.002120 1.002509 1.002897 1.003286 1.003675 1.004064 1.004453 1.004844 1.005234 1.005624 1
2 1.006015 1.006405 1.006796 1.007188 1.007580 1.007972 1.008363 1.008755 1.009148 1.009541 2
3 ' 1.009934 1.010327 1.010721 1.011115 1.011510 1.011904 1.012298 1.012694 1.013089 1.013485 3
4 1.013881 1.014277 1.014673 1.015070 1.015467 1.015864 1.016261 1.016659 1.017058 1.017456 4
5 1.017854 1.018253 1.018652 1.019052 1.019451 1.019851 1.020251 1.020651 1.021053 1.021454 5
6 1.021855 1.022257 1.022659 1.023061 1.023463 1.023867 1.024270 1.024673 1.025077 1.025481 6
7 1.025885 1.026289 1.026694 1.027099 1.027504 1.027910 1.028316 1.028722 1.029128 1.029535 7
8 1.029942 1.030349 1.030757 1.031165 1.031573 1.031982 1.032391 1.032800 1.033209 1.033619 8
9 1.034029 1.034439 1.034850 1.035260 1.035671 1.036082 1.036494 1.036906 1.037318 1.037730 9
10 1.038143 1.038556 1.038970 1.039383 1.039797 1.040212 1.040626 1.041041 1.041456 1.041872 10
11 1.042288 1.042704 1.043121 1.043537 1.043954 1.044370 1.044788 1.045206 1.045625 1.046043 11
12 1.046462 1.046881 1.047300 1.047720 1.048140 1.048559 1.048980 1.049401 1.049822 1.050243 12
13 1.050665 1.051087 1.051510 1.051933 1.052356 1.052778 1.053202 1.053626 1.054050 1.054475 13
14 1.054900 1.055325 1.055751 1.056176 1.056602 1.057029 1.057455 1.057882 1.058310 1.058737 14
15 1.059165 1.059593 1.060022 1.060451 1.060880 1.061308 1.061738 1.062168 1.062598 1.063029 15
16 1.063460 1.063892 1.064324 1.064756 1.065188 1.065621 1.066054 1.066487 1.066921 1.067355 16
17 1.067789 1.068223 1.068658 1.069093 1.069529 1.069964 1.070400 1.070836 1.071273 1.071710 17
18 1.072147 1.072585 1.073023 1.073461 1.073900 1.074338 1.074777 1.075217 1.075657 1.076097 18
19 1.076537 1.076978 1.077419 1.077860 1.078302 1.078744 1.079187 1.079629 1.080072 1.080515 19
20 1.080959 1.081403 1.081848 1.082292 1.082737 1.083182 1.083628 1.084074 1.084520 1.084967 20
21 1.085414 1.085861 1.086309 1.086757 1.087205 1.087652 1.088101 1.088550 1.089000 1.089450 21
22 1.089900 1.090351 1.090802 1.091253 1.091704 1.092155 1.092607 1.093060 1.093513 1.093966 22
23 1.094420 1.094874 1.095328 1.095782 1.096236 1.096691 1.097147 1.097603 1.098058 1.098514 23
24 1.098971 1.099428 1.099886 1.100344 1.100802 1.101259 1.101718 1.102177 1.102637 1.103097 24
25 1.103557 1.104017 1.104478 1.104938 1.105400 1.105862 1.106324 1.106786 1.107248 1.107711 25
26 1.108175 1.108639 1.109103 1.109568 1.110033 1.110497 1.110963 1.111429 1.111895 1.112361 26
27 1.112828 1.113295 1.113763 1.114229 1.114697 1.115166 1.115635 1.116104 1.116572 1.117042 27
28 1.117512 1.117982 1.118453 1.118923 1.119395 1.119867 1.120339 1.120812 1.121284 1.121757 28
29 1 1.122231 1 1.122705 1.123179 1 1.123653 1.124128 1.124603 1.125079 1.125555 1.126030 1.126507 29
*All weights in vacuo—International Critical Tables 2, 343. ©
REFERENCE TABLES
TABLE XV
B r i x , A p p a r e n t Density, A p p a r e n t Specific Gravity, a n d G r a m m e s
of S u c r o s e p e r 100 ml of S u g a r S o l u t i o n s
(NBS—C440, 1942, p. 632)
Column 1 gives Brix»or percentage of sucrose in the solution.
Column 2 gives apparent density, t h a t is, the weight in air with brass weights of 1 ml
of solution at 20 °C. The values in this column correspond to the values of true density
(table XIV), having been obtained by means of the formula
which m a y be utilized for converting apparent density into true density, and vice
versa, by considering t h a t M, the weight in vacuo, and W, the apparent weight, refer
to 1 ml, since true density is defined as the weight in vacuo of 1 ml, and the apparent
density as the weight of 1 ml of substance in air with brass weights, p is the density of
air, which has been taken as 0.0012046; d 1 the density of the solution, d 2 the density
of the weights, which has been taken as 8.4 g/ml.
Column 3 gives the a p p a r e n t specific gravity at 20 C C. The values in this column were
obtained by dividing the apparent density in column 2 by the apparent density of
water at 20°C, which was taken as 0.997174.
Column 4 gives the grammes sucrose (weighed in vacuo) per 100 ml of solution.
The values in the table were calculated in three sections by different individuals;
t h u s from 40 to 60 Brix by Peters and Phelps (BS Tech. Paper T338, 1927); 60 to
83.9 Brix by Brewster and Phelps (NBS Research Paper RP536, 1933); and the re-
maining values, 0 to 40 and 84 to 93 Brix by Snyder, Saunders, and Golden of t h e
National Bureau of Standards. After the computations were completed, the tabulations
were made by rounding off the values to the last figure given. The values are considered
exact to ± 1 in the fifth decimal.
Grammes of | Grammes of
Percentage Apparent Percentage Apparent sucrose
of sucrose Apparent specific per 100 ml of sucrose Apparent per 100 ml
by weight density at gravity at weight 1 by weight density at gravity at weight
(Brix) 20 °C 20 °C/20 °C (Brix) 20 °C 20 °C/20 °C
1 2 3 4 1 2 3 4
0.0 0.99717 1.00000 0.000 2.0 1.00495 1.00780 2.012

.1 .99756 .00039 .100 .1 .00534 .00819 .113
.2 .99795 .00078 .200 .2 .00574 .00859 .215
.3 .99834 .00117 .300 .3 .00613 .00898 .317
.4 .99872 .00156 .400 .4 .00652 .00937 .418
.5 .99911 .00194 .500 .5 .00691 .00977 .520
.6 .99950 .00233 .600 .6 .00730 .01016 .622
.7 .99989 .00272 .701 •7 .00769 .01055 .724
.8 1.00028 .00312 .801 .8 .00809 .01094 .826
.9 .00067 .00351 .902 .9 .00848 .01134 .928
1.0 1.00106 1.00390 1.002 3.0 1.00887 1.01173 3.030
.1 .00145 .00429 .103 •1 .00927 .01213 .132
.2 .00184 .00468 .203 .2 .00966 .01252 .234
.3 .00223 .00507 .304 .3 .01006 .01292 .337
.4 .00261 .00546 .405 .4 .01045 .01331 .439
.5 .00300 .00585 .506 .5 .01084 .01371 .542
.6 .00339 .00624 .607 .6 .01124 .01410 .644
.7 .00378 .00663 .708 .7 .01163 .01450 .747
.8 .00417 .00702 .809 .8 .01203 .01490 .850
.9 .00456 .00741 .911 .9 .01243 .01529 .953
T a b l e XV—continued
Grammes of Grammes of
Percentage Apparent sucrose Percentage Apparent sucrose
of sucrose Apparent specific per 100 ml Apparent per 100 ml
by weight density at gravity at weight by weight density at gravity at weight
(Brix) 20 °C 20 °C/20 °C (Brix) 20 °C 20 °C/20 °C in vacuo
1 2 3 4 1 2 3 4
54.0 1.25084 1.25439 67.601 59.0 1.27958 1.28320 75.555

54.1 141 495 .757 59.1 1.28017 379 .718
54.2 197 552 .912 59.2 075 437 .880
54.3 254 609 68.069 59.3 134 497 76.043
54.4 311 666 .225 59.4 193 556 .207
54.5 1.25367 1.25723 .381 59.5 251 614 .369
54.6 424 780 .537 59.6 309 672 .533
54.7 481 836 .694 59.7 367 731 .696
54.8 538 893 .851 59.8 426 789 .860
54.9 594 950 69.008 59.9 485 849 77.024
55.0 1.25651 1.26007 69.164 60.0 1.28544 1.28908 77.188
55.1 708 064 .322 60.1 602 966 .351
55.2 765 122 .479 60.2 661 1.29025 .515
55.3 822 179 .636 60.3 720 084 .680
55.4 879 236 .794 60.4 779 143 .844
55.5 1.25936 1.26293 69.951 60.5 838 203 78.009
55.6 1.25993 350 70.109 60.6 897 262 .173
55.7 1.26050 408 .267 60.7 956 321 .338
55.8 108 465 .425 60.8 1.29015 380 .503
55.9 165 522 .583 60.9 074 439 .668
56.0 1.26222 1.26580 70.742 61.0 1.29133 1.29498 78.833
56.1 279 637 70.900 61.1 193 559 .999
56.2 337 695 71.059 61.2 252 618 79.165
56.3 394 752 .217 61.3 311 677 .330
56.4 452 810 .376 61.4 370 736 .496
56.5 1.26509 1.26868 .535 61.5 430 796 .662
56.6 566 925 .694 61.6 489 855 .828
56.7 624 1.26983 71.854 61.7 548 915 .995
56.8 682 1.27041 72.013 61.8 608 975 80.161
56.9 739 098 .173 61.9 667 1.30034 .328
57.0 1.26797 1.27156 72.332 62.0 1.29726 1.30093 80.494
57.1 854 214 .492 62.1 786 153 .661
57.2 912 272 .652 62.2 845 212 .828
57.3 970 330 .812 62.3 905 273 .995
57.4 1.27028 388 72.973 62.4 966 334 81.162
57.5 1.27086 1.27446 73.133 62.5 1.30025 393 .329
57.6 143 504 .293 62.6 085 453 .497
57.7 201 562 .454 62.7 145 513 .665
57.8 259 620 .615 62.8 205 573 .833
57.9 317 678 .776 62.9 265 633 82.001
58.0 1.27375 1.27736 73.937 63.0 1.30325 1.30694 82.169
58.1 433 794 74.098 63.1 385 754 .337
58.2 492 853 .260 63.2 446 815 .506
58.3 550 911 .421 63.3 506 875 .674
58.4 608 1.27969 .583 63.4 566 936 .843
58.5 1.27664 1.28028 .744 63.5 626 994 83.012
58.6 724 086 74.906 63.6 686 1.31055 .180
58.7 782 145 75.068 63.7 747 117 .360
58.8 841 203 .230 63.8 807 177 .519
58.9 899 262 .393 63.9 867 237 .688
Percentage Apparent Percentage j Apparent
of sucrose Apparent specific per 100 ml of sucrose j Apparent specific per 100 ml
(Brix) 20 °C 20 °C/20 °C in vacuo (Brix) 20 °C 20°C/20°C
1 2 3 4 1 2 3 4
64.0 1.30927 1.31297 83.858 69.0 1.33992 j 1.34371 92.524

64.1 988 359 84.028 69.1 1.34054 433 .701
64.2 1.31048 418 .198 69.2 116 495 .878
64.3 108 479 .367 69.3 179 558 93.056
64.4 169 540 .538 69.4 241 621 .233
64.5 229 600 .708 69.5 304 684 .411
64.6 290 661 .879 69.6 366 746 .589
64.7 350 723 85.049 69.7 429 809 .767
64.8 412 784 .220 69.8 491 871 1 .945
64.9 473 845 .391 69.9 554 934 94.123
65.0 1.31533 1.31905 85.561 70.0 1.34616 1.34997 94.302
65.1 594 966 .733 70.1 679 1.35060 .481
65.2 655 1.32028 .904 70.2 742 123 .660
65.3 716 089 86.076 70.3 805 186 .839
65.4 777 150 .248 70.4 867 248 95.017
65.5 837 210 .419 70.5 930 311 .197
65.6 898 271 .591 70.6 993 375 .376
65.7 959 332 .763 70.7 1.35056 438 .556
65.8 1.32019 393 .935 70.8 119 501 .736
65.9 081 455 87.107 70.9 182 564 .916
66.0 1.32142 1.32516 87.280 71.0 1.35245 1.35627 96.096
66.1 203 577 .453 71.1 308 691 .276
66.2 264 638 .626 71.2 371 754 .456
66.3 325 699 .798 71.3 434 817 .636
66.4 385 759 .971 71.4 498 881 .817
66.5 446 820 88.142 71.5 561 944 .998
66.6 509 884 .318 71.6 625 1.36008 97.179
66.7 570 945 .492 71.7 688 072 .360
66.8 632 1.33007 .666 71.8 751 135 .541
66.9 693 068 .839 71.9 814 198 .722
67.0 1.32754 1.33129 89.012 72.0 1.35877 1.36261 97.904
67.1 816 192 .187 72.1 940 324 98.085
67.2 878 254 .361 72.2 1.36004 389 .268
67.3 939 315 .536 72.3 067 452 .449
67.4 1.33001 377 .711 72.4 131 516 .632
67.5 062 438 .885 72.5 194 579 .814
67.6 124 500 90.060 72.6 258 643 .997
67.7 186 562 .235 72.7 322 707 99.179
67.8 248 625 .411 72.8 385 771 .362
67.9 309 686 .585 72.9 450 836 .545
68.0 1.33371 1.33748 90.761 73.0 1.36514 1.36900 99.728
68.1 433 810 .937 73.1 578 964 .912
68.2 495 872 91.112 73.2 642 1.37028 100.095
68.3 557 935 .288 73.3 705 092 .278
68.4 619 997 .464 73.4 769 156 .462
68.5 681 1.34059 .641 73.5 833 220 .646
68.6 743 121 .817 73.6 896 283 .827
68.7 805 183 . 993 73.7 960 347 101.014
68.8 867 245 92.169 73.8 1.37024 411 .198
68.9 930 309 .347 73.9 088 476 .383
T a b l e XV—-continued
Percentage Apparent Percentage Apparent
of sucrose Apparent per 100 ml of sucrose Apparent specific - per 100 ml
(Brix) 20 °C 20 °C/20 °C (Brix) 20 °C 20 °C/20 °C
1 2 3 4 1 2 3 4
74.0 1.37153 1.37541 101.568 79.0 1.40409 1.40806 111.002

74.1 217 605 .753 79.1 475 872 .195
74.2 281 669 .937 79.2 541 938 .388
74.3 345 733 102.122 79.3 607 1.41005 .581
74.4 410 798 .308 79.4 674 072 .775
74.5 475 864 .493 79.5 740 138 .968
74.6 539 928 .679 79.6 806 204 112.161
74.7 604 993 .865 79.7 872 270 .354
74.8 668 1.38057 103.050 79.8 939 337 .549
74.9 733 122 .237 79.9 1.41005 404 .743
75.0 1.37797 1.38187 103.423 80.0 1.41072 1.41471 112.938

75.1 862 252 .609 80.1 138 537 113.131
75.2 926 316 .796 80.2 204 603 .326
75.3 991 381 .983 80.3 271 670 .521
75.4 1.38055 445 104.170 80.4 337 737 .715
75.5 119 1.38510 104.356 80.5 404 804 .911
75.6 184 575 .543 80.6 472 872 114.106
75.7 249 640 .731 80.7 537 937 .301
75.8 314 705 .919 80.8 604 1.42004 .497
75.9 379 770 105.106 80.9 671 072 .692
76.0 1.38444 1.38835 105.294 81.0 1.41737 1.42138 114.888

76.1 510 902 .482 81.1 804 205 115.084
76.2 575 967 .670 81.2 871 272 .280
76.3 640 1.39032 .859 81.3 938 339 .477
76.4 705 097 106.047 81.4 1.42005 406 .673
76.5 770 162 .236 81.5 072 474 .870
76.6 835 228 .424 81.6 139 541 116.067
76.7 900 293 .613 81.7 206 608 .264
76.8 965 358 ,802 81.8 273 675 .461
76.9 1.39030 423 .991 81.9 340 742 .658
77.0 1.39096 1.39489 107.181 82.0 1.42407 1.42810 116.856

77.1 161 554 .370 82.1 475 878 117.053
77.2 225 619 .560 82.2 543 946 .252
77.3 291 685 .750 82.3 610 1.43013 .449
77.4 356 750 .940 82.4 677 080 .647
77.5 422 816 108.130 82.5 744 148 .845
77.6 488 882 .320 82.6 811 214 118.044
77.7 554 949 .511 82.7 878 282 .243
77.8 619 1.40014 .701 82.8 946 350 .442
77.9 685 080 .892 82.9 1.43013 417 .641
78.0 1.39751 1.40146 109.084 83.0 1.43081 1.43486 118.840

78.1 816 211 .274 83.1 148 553 119.039
78.2 882 277 .466 83.2 216 621 .239
78.3 948 344 .657 83.3 283 688 .438
78.4 1.40013 409 .848 83.4 351 756 .638
78.5 079 475 110.041 83.5 419 824 .838
78.6 145 541 .232 83.6 488 894 120.039
78.7 211 607 .425 83.7 555 961 .238
78.8 277 674 .617 83.8 623 1.44029 .439
78.9 343 740 .809 83.9 691 097 .640
Percentage Apparent sucrose Percentage Apparent sucrose
of sucrose Apparent Specific per 100 ml of sucrose Apparent per 100 ml
by weight density at gravity at weight by weight density at gravity at weight in
(Brix) 20 °C in vacuo (Brix) 20 °C 20 °C/20 °C vacuo
20 °C/20 °C
l 2 3 4 1 2 3 4
84 . 0 1.43758 1.44165 120.841 89.0 1.47199 1.47616 131.096

.1 .43826 .44234 121.042 .1 .47269 .47686 .305
.2 .43894 .44302 .243 .2 .47339 .47756 .515
.3 .43962 .44370 .444 .3 .47409 .47826 .725
.4 1.44030 .44438 .646 .4 .47479 .47897 .935
.5 .44098 .44507 .847 .5 .47548 .47967 132.145
.6 .44166 .44575 122.049 .6 .47618 1.48037 .355
.7 .44234 .44643 .251 .7 .47688 .48107 .565
.8 .44303 .44712 .453 .8 .47758 .48177 .776
.9 .44371 .44780 .655 .9 .47828 .48247 .987
85 . 0 1.44439 1.44848 122.858 90.0 1.47898 1.48317 133.198
.1 .44507 .44917 123.061 .1 .47968 .48388 .409
.2 .44576 .44985 .263 .2 1.48039 .48458 .620
.3 .44644 1.45054 .466 .3 .48109 .48529 .832
.4 .44712 .45123 .670 .4 .48179 .48599 134.043
.5 .44781 .45191 .873 .5 .48249 .48669 .255
.6 .44849 .45260 124.076 .6 .48320 .48740 .467
.7 .44918 .45329 .280 .7 .48390 .48810 .680
.8 .44986 .45397 .484 .8 .48460 .48881 .892
.9 1.45055 .45466 .688 .9 .48531 .48951 135.104
86 . 0 1.45124 1.45535 124.892 91.0 1.48601 1.49022 135.317
.1 .45192 .45604 125.096 •1 .48672 .49093 .530
.2 .45261 .45673 .301 .2 .48742 .49164 .743
.3 .45330 .45741 .505 .3 .48813 .49234 .956
.4 .45398 .45810 .710 .4 .48883 .49305 136.170
.5 .45467 .45879 .915 .5 .48954 .49376 .383
.6 .45536 .45949 126.121 .6 1.49024 .49447 .597
.7 .45605 1.46018 .326 .7 .49095 .49518 .811
.8 .45674 .46087 .531 .8 .49166 .49588 137.025
.9 .45743 .46156 .737 .9 .49236 .49659 .239
87 . 0 1.45812 1.46225 126.943 92.0 1.49307 1.49730 137.454
.1 .45881 .46294 127.149 .1 .49378 .49801 .668
.2 .45950 .46364 .355 .2 .49449 .49872 .883
.3 1.46019 .46433 .562 .3 .49520 .49944 138.098
.4 .46088 .46502 .768 .4 .49591 1.50015 .313
.5 .46157 .46572 .975 .5 .49662 .50086 .529
.6 .46227 .46641 128.182 .6 .49733 .50157 .744
.7 .46296 .46710 .389 .7 .49804 .50228 .960
.8 .46365 .46780 .596 .8 .49875 .50299 139.176
.9 .46434 .46849 .803 .9 .49946 .50371 .392
88 0 1.46504 1.46919 129.011 93.0 1.50017 1.50442 139.608
1 .46573 .46989 .219 .1 .50088 .50513 .824
2 .46643 1.47058 .426 .2 .50159 .50585 140.041
3 .46712 .47128 .635 .3 .50230 .50656 .257
.4 .46782 .47198 .843 .4 .50302 .50728 .474
.5 .46851 .47267 130.051 .5 .50373 .50799 .691
6 .46921 .47337 .260 .6 .50444 .50871 .908
7 .46990 .47407 .468 .7 .50516 .50942 141.126
8 1.47060 .47477 .677 .8 .50587 1.51014 .343
9 .47130 .47547 .886 .9 .50659 .51086 .561
Table XVI—Weight p e r U n i t V o l u m e of S u g a r S o l u t i o n s at 20°C
Weight in air Weight in air

Brix Brix
lb/ft3 lb/gal ton/100 gal lb/ft3 lb/gal ton/100 gal
0 62.253 10.00 .4456 51 77.042 12.376 .5514

1 62.492 10.038 .4474 52 77.386 12.431 .5539
2 62.739 10.078 .4491 53 77.738 12.487 .5564
3 62.978 10.112 .4509 54 78.089 12.543 .5589
4 63.225 10.156 .4526 55 78.441 12.600 .5614
5 63.472 10.196 .4544 56 78.800 12.658 .5640
6 63.727 10.237 .4562 57 79.151 12.714 .5665
7 63.973 10.276 .4580 58 79.518 12.773 .5691
8 64.228 10.317 .4598 59 79.877 12.831 .5717
9 64.482 10.358 .4616 60 80.244 12.890 .5743
10 64.744 10.400 .4635 61 80.618 12.950 .5769
11 65.006 10.442 .4653 62 80.984 13.009 .5796
12 65.260 10.483 .4672 63 81.358 13.069 .5823
13 65.522 10.525 .4691 64 81.732 13.129 .5850
14 65.791 10.568 .4709 65 82.114 13.190 .5877
15 66.053 10.610 .4728 66 82.488 13.250 .5904
16 66.322 10.653 .4748 67 82.877 13.312 .5931
17 66.592 10.697 .4767 68 83.258 13.374 .5959
18 66.868 10.741 .4786 69 83.647 13.437 .5986
19 67.138 10.785 .4806 70 84.036 13.499 .6014
20 67.414 10.829 .4826 71 84.425 13.562 .6042
21 67.691 10.874 .4846 72 84.822 13.625 .6070
22 67.975 10.919 .4866 73 85.218 13.689 .6099
23 68.260 10.965 .4886 74 85.622 13.754 .6127
24 68.544 11.011 .4906 75 86.018 13.817 .6156
25 68.828 11.056 .4927 76 86.430 13.884 .6185
26 69.113 11.102 .4947 77 86.834 13.949 .6214
27 69.404 11.149 .4968 78 87.238 14.013 .6243
28 69.696 11.196 .4989 79 87.647 14.095 .6273
29 69.995 11.244 .5010 80 88.068 14.147 .6302
30 70.287 11.291 .5031 81 88.480 14.213 .6332
31 70.586 11.339 .5053 82 88.898 14.280 .6362
32 70.893 11.388 .5074 83 89.317 14.347 .6392
33 71.192 11.436 .5096 84 89.744 14.414 .6422
34 71.499 11.485 .5118 85 90.170 14.484 .6453
35 71.806 11.535 .5140 86 90.597 14.553 .6483
36 72.112 11.584 .5162 87 91.023 14.621 .6514
37 72.426 11.634 .5184 88 91.457 14.691 .6545
38 72.741 11.685 .5207 89 91.891 14.760 .6576
39 73.055 11.735 .5229 90 92.325 14.831 .6607
40 73.376 11.787 .5252 91 92.766 14.901 .6638
41 73.698 11.839 .5275 92 93.207 14.972 .6670
42 74.020 11.890 .5298 93 93.649 15.043 .6702
43 74.349 11.943 .5321 94 94.097 15.115 .6733
44 74.678 11.996 .5345 95 94.546 15.187 .6765
45 75.007 12.049 .5369 96 .6798
46 75.336 12.102 .5392 97 .6830
47 75.673 12.155 .5416 98 .6862
48 76.017 12.211 .5440 99 .6895
49 76.354 12.265 .5465 100 .6928
50 76.690 12.319 .5489
Table XVII—Degree of Supersaturation—All Values Being Prefixed by 1.
T a b l e XVIII—Crystal Content of M a s s e c u i t e s *
Purity drop
Mass. P
puritjT 15 16 17 18 19 20 22 23 24 25
21
90 60.0 61.5 63.0 64.3 65.5 66.7
89 57.7 59.3 60.7 62.1 63.3 64.5 65.6
88 55.6 57.1 58.6 60.0 61.3 62.5 63.6 64.7
87 53.6 55.2 56.7 58.1 59.4 60.6 61.8 62.9 63.9
86 51.7 53.3 54.8 56.3 57.6 58.8 60.0 61.1 62.1 63.2
85 50.0 51.6 53.1 54.5 55.9 57.1 58.3 59.4 60.5 61.5 62.5
84 48.4 50.0 51.5 52.9 54.3 55.6 56.8 57.9 59.0 60.0 61.0
83 46.9 48.5 50.0 51.4 52.8 54.1 55.3 56.4 57.5 58.5 59.5
82 45.5 47.1 48.6 50.0 51.4 52.6 53.8 55.0 56.1 57.1 58.1
81 44.1 45.8 47.2 48.6 50.0 51.3 52.5 53.7 54.8 55.8 56.8
80 42.9 44.4 45.9 47.4 48.7 50.0 51.2 52.4 53.5 54.5 55.6
79 41.7 43.2 44.7 46.2 47.5 48.8 50.0 51.2 52.3 53.3 54.3
78 40.5 42.1 43.6 45.0 46.3 47.6 48.8 50.0 51.1 52.2 53.2
77 39.5 41.0 42.5 43.9 45.2 46.5 47.7 48.9 50.0 51.1 52.1
76 38.5 40.0 41.5 42.9 44.2 45.5 46.7 47.8 48.9 50.0 51.0
75 37.5 39.0 40.5 41.9 43.2 44.4 45.7 46.8 47.9 49.0 50.0
74 36.6 38.1 39.5 40.9 42.2 43.5 44.7 45.8 46.9 48.0 49.0
73 35.7 37.2 3S.6 40.0 41.3 42.6 43.7 44.9 46.0 47.1 48.1
72 34.9 36.4 37.8 39.1 40.4 41.7 42.9 44.0 45.1 46.2 47.2
71 34.1 35.6 37.0 38.3 39.6 40.8 42.0 43.1 44.2 45.3 46.3
70 33.3 34.8 36.2 37.5 38.8 40.0 41.2 42.3 43.4 44.4 45.5
15 16 17 18 19 20 22 24 26 28 30
!
69 32.6 34.0 35.4 36.7 38.0 39.2 41.5 43.6 45.6 47.5 49.2
68 31.9 33.3 34.7 36.0 37.3 38.5 40.7 42.9 44.8 46.7 48.4
67 31.2 32.7 34.0 35.3 36.5 37.7 40.0 42.1 44.1 45.9 47.6
66 30.6 32.0 33.3 34.6 35.8 37.0 39.3 41.4 43.3 45.2 46.9
65 30.0 31.4 32.7 34.0 35.2 36.4 38.6 40.7 42.6 44.4 46.2
64 29.4 30.8 32.1 33.3 34.5 35.7 37.9 40.0 41.9 43.8 45.5
93 28.8 30.2 31.5 32.7 33.9 35.1 37.3 39.3 41.3 43.1 44.8
62 28.3 29.6 30.9 32.1 33.3 34.5 36.7 38.7 40.6 42.4 44.1
61 27.8 29.1 30.4 31.6 32.8 33.9 36.1 38.1 40.0 41.8 43.5
50 27.3 28.6 29.8 31.0 32.2 33.3 35.5 37.5 39.4 41.2 42.9
59 26.8 28.1 29.3 30.5 31.7 32.8 34.9 36.9 38.8 40.6 42.3
68 26.3 27.6 28.8 30.0 31.1 32.3 34.4 36.4 38.2 40.0 41.7
57 25.9 27.1 28.3 29.5 30.6 31.7 33.8 35.8 37.7 39.4 41.1
56 25.4 26.7 27.9 29.0 30.2 31.3 33.3 35.3 37.1 38.9 40.5
55 25.0 26.2 27.4 28.6 29.7 30.8 32.8 34.8 36.6 38.3 40.0
*With apparent purities t h e crystal content per cent Brix is derived. The use of
true purities gives crystal per cent dry substance. To obtain crystal per cent massecuite
multiply by Brix or dry substance per unit of massecuite.
Table X I X (a)—Stock Recovery.

Total pol and recoverable pol in tons per 100 gallons of stock, when the apparent
purity of final molasses is 30.
Total
Brix pol(T) Apparent purity of product
of
pro— Recov.
duct pol(R) 45 50 55 60 65 70 75 80 85 90
64 1 T .169 .187 .206 .225 .243 .262 .281 .300 .318 .337
R .080 .107 .134 .160 .187 .214 .241 .267 .294 .321
66 T .175 .195 1 .214 .234 .253 .273 .292 .312 .331 .351
R .084 .111 .139 .167 .195 .223 .251 .278 .306 .334
68 T .182 .203 .223 .243 .263 .284 .304 .324 .345 .365
R .087 .116 .145 .174 .203 .232 .261 .290 .319 .347
70 T .190 .211 .232 .253 .274 .295 .316 .337 .358 .379
R .090 .120 .150 .180 .211 .241 .271 .301 .331 .360
72 T .197 .219 .240 .262 .284 .306 .328 .350 .372 .393
R .094 .124 .156 .187 .219 .250 .281 .312 .343 .375
74 T .204 .227 .249 .272 .295 .317 .340 .363 .385 .408
R .097 .130 .162 .194 .227 .259 .292 .324 .356 .389
76 T .212 .235 .259 .282 .306 .329 .353 .376 .400 .423
R .101 .134 .168 .202 .235 .269 .302 .336 .369 .403
78 T .219 .244 .268 .292 .317 .341 .365 .390 .414 .438
R .104 .139 .174 .209 .244 .278 .313 .348 .383 .417
80 T .227 .252 .277 .303 .328 .353 .378 .403 .429 .454
R .108 .144 .180 .216 .252 .288 .324 .360 .396 .432
82 T .235 .261 .287 .313 .339 .365 .391 .417 .443 .470
R .112 .149 .186 .224 .261 .298 .335 .373 .410 .447
84 T .243 .270 .297 .323 .351 .378 .405 .432 .459 .486
R .116 .154 .193 .231 .270 .308 .347 .385 .424 .462
86 T .251 .279 .307 .335 .362 .390 .418 .446 .474 .502
R .120 .159 .199 .239 .279 .319 .358 .398 .438 .478
88 T .259 .288 .317 .346 .374 .403 .432 .461 .490 .518
R .123 .165 .206 .247 .288 .329 .370 .411 .453 .494
90 T .268 .297 .327 .357 .387 .416 .446 .476 .505 .535
R .127 .170 .212 .255 .297 .340 .382 .425 .467 .509
92 T .276 .307 .338 .368 .399 .430 .460 .491 .522 .552
R .132 .175 .219 .263 .307 .351 .394 .438 .482 .526
94 T .285 .317 .348 .380 .411 .443 .475 .506 .538 .570
R .136 .181 .226 .271 .316 .362 .407 .452 .497 .543
96 T .294 .326 .359 .392 .424 .457 .490 .522 .555 .587
R .140 .186 .233 .280 .326 .373 .420 .466 .513 .559
98 T .303 .336 .370 .404 .437 .471 .504 .538 .572 .605
R .144 .192 .240 .288 .336 .384 .432 .480 .528 .577
100 T .312 .346 .381 .416 .450 .485 .520 .554 .589 .624
R .149 .198 .247 .297 .346 .396 .445 .495 .544 .594
The tons pol in residual molasses m a y be obtained by subtracting tons recoverable
pol from tons pol in stock.
T a b l e X I X (b)—Stock Recovery.
Total
of
Recov.
duct pol(R) 45 50 55 60 65 70 75 80 85 90
64 T .169 .187 .206 .225 .243 .262 .281 .300 .318 .337
R .058 .086 .115 .144 .173 .202 .230 .259 .288 .317
66 T .175 .195 .214 .234 .253 .273 .292 .312 .331 .351
R .060 .090 .120 .150 .180 .210 .240 .270 .300 .330
68 T .182 .203 .223 .243 .263 .284 .304 .324 .345 .365
R .062 .094 .125 .156 .187 .218 .249 .281 .312 .343
70 T .190 .211 .232 .253 .274 .295 .316 .337 .358 .379
R .065 .097 .130 .162 .194 .227 .259 .291 .324 .356
72 T .197 .219 .240 .262 .284 .306 .328 .350 .372 .393
R .067 .101 .135 .168 .202 .235 .269 .303 .336 .370
74 T .204 .227 .249 .272 .295 .317 .340 .363 .385 .408
R .070 .105 .140 .174 .209 .244 .279 .314 .349 .384
76 T .212 .235 .259 .282 .306 .329 .353 .376 .400 .423
R .072 .108 .145 .181 .217 .253 .289 .325 .362 .398
78 T .219 .244 .268 .292 .317 .341 .365 .390 .414 .438
R .075 .112 .150 .187 .225 .262 .300 .337 .375 .412
80 T .227 .252 .277 .303 .328 .353 .378 .403 .429 .454
R .077 .116 .155 .194 .233 .271 .310 .349 .388 .427
82 T .235 .261 .287 .313 .339 .365 .391 .417 .443 .470
R .080 .120 .160 .201 .241 .281 .321 .361 .401 .441
84 T .243 .270 .297 .323 .351 .378 .405 .432 .459 .486
R .083 .124 .166 .207 .249 .290 .332 .373 .415 .456
86 T .251 .279 .307 .335 .362 .390 .418 .446 .474 .502
R .086 .129 .173 .214 .257 .300 .343 .386 .429 .472
88 T .259 .288 .317 .346 .374 .403 .432 .461 .490 .518
R .089 .133 .177 .222 .266 .310 .354 .399 .443 .487
90 T .268 .297 .327 .357 .387 .416 .446 .476 .505 .535
R .091 .137 .183 .229 .274 .320 .366 .412 .457 .503
92 T .276 .307 .338 .368 .399 .430 .460 .491 .522 .552
R .093 .142 .189 .236 .283 .330 .378 .425 .472 .519
94 T .285 .317 .348 .380 .411 .443 .475 .506 .538 .570
R .098 .146 .195 .243 .292 .340 .389 .438 .487 .536
96 T .294 .326 .359 .392 .424 .457 .490 .522 .555 .587
R .100 .151 .201 .251 .301 .351 .402 .452 .501 .552
98 T .303 .336 .370 .404 .437 .471 .604 .538 .572 .605
R .103 .155 .207 .259 .310 .362 .414 .466 .517 .569
100 T .312 .346 .381 .416 .450 .485 .520 .554 .589 .624
R .107 .160 .213 .266 .320 .373 .426 .480 .533 .586
The tons pol in residual molasses m a y be obtained by subtracting tons recoverable
Table X I X (c)—Stock Recovery.

Total
of
Recov.
duct 1 pol(R) 45 50 55 60 65 70 75 80 85 90
64 T .169 .187 .206 .225 .243 .262 .281 .300 .318 .337
R .031 .062 .094 .125 .156 .167 .218 .250 .281 .312
T .195 .214 .234 .253 .273
66 .175 .292 .312 .331 .351
R .032 .065 .097 .129 .162 .194 .227 .259 .292 .235
68 T .182 .203 .223 .243 .263 .284 .304 .324 .345 .365
R .034 .068 .101 .135 .169 .202 .236 .270 .303 .338
70 T .190 I . 2 1 1 .232 .253 .274 .295 .316 .337 .358 .379
R .035 .070 .105 .140 .175 .210 .246 .280 .315 .351
72 T .197 .219 .240 .262 .284 .306 .328 .350 .372 .393
R .036 .073 .109 .145 .182 .218 .255 .291 .327 .364
74 T .204 .227 .249 .272 .295 .317 .340 .363 .385 .408
R .038 .076 .113 .151 .189 .227 .265 .302 .340 .378
76 T .212 .235 .259 .282 .306 .329 .353 .376 .400 .423
R .039 .078 .118 .157 .196 .235 .274 .314 .353 .393
78 T .219 .244 .268 .292 .317 .341 .365 .390 .414 .438
R .041 .081 .122 .163 .203 .244 .284 .325 .366 .406
80 T .227 .252 .277 .303 .328 .353 .378 .403 .429 .454
R .042 .084 .126 .168 .210 .252 .294 .336 .379 .420
82 T .235 .261 .287 .313 .339 .365 .391 .417 .443 .470
R .043 .087 .130 .173 .217 .260 .304 .347 .392 .435
84 T .243 .270 .296 .324 .351 .378 .405 .432 .459 .486
R .045 .090 .135 .180 .225 .269 .315 .359 .405 .450
86 T .251 .279 .307 .335 .362 .390 .418 .446 .474 .502
R .046 .093 .139 .186 .232 .279 .325 .371 .418 .465
88 T .259 .288 .317 .346 .374 .403 .432 .461 .490 .518
R .048 .096 .144 .192 .240 .288 .336 .384 .432 .480
90 T .268 .297 .327 .357 .387 .416 .446 .476 .505 .535
R .050 .099 .149 .199 .248 .298 .347 .397 .447 .495
92 T .276 .307 .338 .368 .399 .430 .460 .491 .522 .552
R .051 .102 .153 .205 .255 .307 .358 .408 .460 .511
94 T .285 .317 .348 .380 .411 .443 .475 .506 .538 .570
R .053 .105 .158 .211 .263 .316 .369 .421 .474 .527
96 T .294 .326 .359 .392 .424 .457 .490 .522 .555 .587
R .054 .109 .163 .217 .272 .326 .381 .435 .489 .544
98 T .303 .336 .370 .404 .437 .471 .504 .538 .572 .605
R .056 .112 .168 .224 .280 .336 .392 .448 .504 .560
100 T .312 .346 .381 .416 .450 .485 .520 .554 .589 .624
R .058 .115 .173 .231 .288 .346 .404 .462 .519 .577
The tons pol in residual molasses may be obtained by subtracting tons recoverable
T a b l e X X — F a c t o r s to be U s e d in Calculating W e i g h t per Gallon of M o l a s s e s .
Temp. °C Factor A Factor B Temp. °C Factor A Factor B

10 0.99975 1.0013 25 1.00013 1.0040
11 0.99978 1.0014 26 1.00015 1.0043
12 0.99980 1.0015 27 1.00018 1.0046
13 0.99983 1.0016 28 1.00020 1.0048
14 0.99985 1.0017 29 1.00023 1.0051
15 0.99988 1.0019 30 1.00025 1.0054
16 0.99990 1.0021 31 1.00028 1.0057
17 0.99993 1.0023 32 1.00030 1.0060
18 0.99995 1.0025 33 1.00033 1.0064
19 0.99998 1.0027 34 1.00035 1.0067
20 1.00000 1.0028 35 1.00038 1.0070
21 1.00003 1.0030 36 1.00040 1.0074
22 1.00005 1.0033 37 1.00043 1.0077
23 1.00008 1.0035 38 1.00045 1.0081
24 1.00010 1.0038 39 1.00048 1.0085
40 1.00050 1.0089
T a b l e X X I — W e i g h t s as D e c i m a l s of T o n .
lb ton lb ton lb ton lb ton
1 .00045 8 .00357 15 .0067 22 .0098

2 .00089 9 .00401 16 .0071 23 .0103
3 .00134 10 .0045 17 .0076 24 .0107
4 .00178 11 .0049 18 .0080 25 .0111
5 .00223 12 .0054 19 .0085 26 .0116
6 .00268 13 .0058 20 .0089 27 .0120
7 .00312 14 .0062 21 .0094 28 .0125
2 qr = . 025 ton, 3 qr = . 0375 ton and 4 qr = 1 cwt = . 05 ton.

Table XXII—Density* (g/ml) of Water at T e m p e r a t u r e s f r o m 0 to 102 °C.

According to M. Thiesen, Wiss. Abh. der Physikalisch-Technischen Reichsanstalt, 4,
No. 1; 1904.
Temp. °C Density Temp. °C Density Temp. °C Density

0 0.99987 35 0.99406 70 0.97781
1 0.99993 36 0.99371 71 0.97723
2 0.99997 37 0.99336 72 0.97666
3 0.99999 38 0.99299 73 0.97607
4 1.00000 39 0.99262 74 0.97548
5 0.99999 40 0.99225 75 0.97489
6 0.99997 41 0.99186 76 0.97428
7 0.99993 42 0.99147 77 0.97368
8 0.99988 43 0.99107 78 0.97307
9 0.99981 44 0.99066 79 0.97245
10 0.99973 45 0.99024 80 0.97183
11 0.99963 46 0.98982 81 0.97120
12 0.99952 47 0.98940 82 0.97057
13 0.99940 48 0.98896 83 0.96994
14 0.99927 49 0.98852 84 0.96930
15 0.99913 50 0.98807 85 0.96865
16 0.99897 51 0.98762 86 0.96800
17 0.99880 52 0.98715 87 0.96734
18 0.99862 53 0.98669 88 0.96668
19 0.99843 54 0.98621 89 0.96601
20 0.99823 55 0.98573 90 0.96534
21 0.99802 56 0.98524 91 0.96467
22 0.99780 57 0.98478 92 0.96399
23 0.99756 58 0.98425 93 0.96330
24 0.99732 59 0.98375 94 0.96261
25 0.99707 60 0.98324 95 0.96192
26 0.99681 61 0.98272 96 0.96122
27 0.99654 62 0.98220 97 0.96051
28 0.99626 63 0.98167 98 0.95981
29 0.99597 64 0.98113 99 0.95909
30 0.99567 65 0.98059 100 0.95838
31 0.99537 66 0.98005 101 0.95765
32 0.99505 67 0.97950 102 0.95693
33 0.99473 68 0.97894
34 0.99440 69 0.97838
1 imperial gallon of water at 62° F (16.7°C) weighs 10.0 lb.

1 cubic foot of water at 62° F (16.7° C) weighs 62.288 lb.
*The values in the above table, when divided by 0.099892, give the weight in pounds of 1 gallon of water
at the corresponding temperatures.
Table XXV
R e q u i r e m e n t s for A p p a r a t u s for U s e in the A n a l y s i s of Cane for
Payment Purposes
When apparatus is used for the analysis of cane for payment purposes it must
conform either to a specification from a recognised Standards authority or to the follow-
ing requirements.
Brix Hydrometers
The hydrometer must be of an approved shape, size and construction. The scale
shall correspond to one of the following ranges: 0 to 10, 10 to 20, 15 to 25, 20 to 30. It
shall be calibrated to read degrees Brix at 20 °C and the range shall be divided in inter-
vals of one tenth of one degree with full numbering at each unit graduation mark. The
graduation lines shall be fine, of uniform thickness and at right angles to the axis of
the hydrometer. The scale shall be firmly secured inside the stem and without twist.
The readings must conform to a tolerance of ± 0.1° Brix at any point of the scale.
The following inscriptions shall be clearly marked on the scale within the stem and
shall not encroach on the scale or numbering.
(a) The makers name
(b) Serial number
(c) Brix or per cent of sugar by weight
(d) Temp. 20 °C
P o l a r i m e t e r or S a c c h a r i m e t e r t u b e s
The tube must be straight. The length of the tube at 20 °C shall be within ± 0.03
per cent of the nominal lengths of 100 and 200 mm. The ends of the tube must be
parallel and ground flat in a plane at right angles to the axis of the tube and no detect-
able change in reading should be observed on rotating the tube.
Each end must project beyond the ferrule or threaded collar to a distance not
exceeding 1 mm, such t h a t a cover glass placed over the end of the tube does not touch
any other p a r t of the tube.
Cover g l a s s e s
Cover glasses for polarimeter or saccharimeter tubes must be made of clear optical
glass and free from strain. They must have plane parallel surfaces free from scratches.
The edges should be slightly bevelled to prevent chipping. A thickness of 1. 5 to 2 mm
is desirable for tubes of 200 mm length.
Polarimeters and Saccharimeters
These must be in a satisfactory condition mechanically and optically. The error at
any point of the scale must not exceed ± 0 . 1 scale degrees. It is recommended t h a t
they should be calibrated in terms of the International Sugar Scale corresponding to a
normal weight of 26. 000 grammes.
Thermometers
Thermometers are to be of mercury in glass, solid stem, or of an approved enclosed
scale type. All ranges up to a maximum of 110 °C to include zero. The maximum error
allowed is 1.0 °C. Total immersion thermometers are preferred. Inscriptions should
include the maker or vendors name or mark and the immersion for which the ther-
mometer is calibrated.
Refractometers
These must be in satisfactory condition mechanically and optically. The maximum
error at any point of the scale should be the equivalent of 0. 2 degrees Brix.
Balances
These should be within accepted tolerances for sensitivity and reproducibility
corresponding to the maximum capacity of the balance. Efficient damping is required
for rapid weighing.
Weights
Weights to lOOg should conform to Class B tolerances as specified by the National
Standards Laboratory Australia.
Weights of nominal values from lOOg to 1kg should conform to tolerances of 15
parts in 100,000.
Table XXV—continued
T o l e r a n c e s (B Class) for Apparatus for General U s e
in S u g a r Factory Laboratories
The tolerances shown in this Table have been compiled from specifications issued
by the British Standards Institution. They are recommended as being suitable for
apparatus for general use.
Flasks—One mark volumetric
Nominal capcity ml 5 10 25 50 100 200 250 500 1000 2000

Tolerance ± ml 0.04 0.04 0.06 0.10 0.15 0.30 0.30 0.50 0.80 1.20
(British Standard 1792:1960 endorsed as Australian Standard R.20-1961)
Sugar Flasks
Type 1—two graduation marks.
Type 2—single graduation mark for polarization of sugars.
Nominal capacity ml
Tolerance ± ml
(British Standard 675:1953)
Nominal Subdivision Tolerance on Delivery times

capacity ml ml capacity ± ml
min. max.
1 0.01 0.01 20 50
2 0.02 0.02 20 50
5 0.02 0.02 50 120
5 0.05 0.04 20 50
10 0.02 0.02 100 200
10 0.1 0.05 15 40
25 0.05 0.05 85 170
25 0.1 0.1 35 70
50 0.1 0.1 75 150
100 0.2 0.2 65 130
(British Standard 846:1962 endorsed as Australian Standard R. 10-1964)
Pipettes—One mark bulb
Nominal capacity ml 1 2 5 10 15 20 25 50 100

Tolerance ± ml .015 .02 .03 .04 .05 .06 .06 .08 .12
Delivery times (seconds)
minimum 5 5 10 10 15 20 20 20 30
maximum 15 15 25 25 30 40 40 50 60
(British Standard 1583:1961 endorsed as Australian Standard R. 16-1962)

T a b l e XXV—continued
Graduated P i p e t t e s
Type 1—for delivery from zero mark to graduation marks.
Type 2—for delivery down to jet.
Nominal capacity ml 1 2 5 10 25
Subdivisions ml .01 .02 .05 .10 .10
Tolerance ± ml .01 .02 .05 .10 .20
Delivery times, all sizes

Type 1 Minimum 15 s Maximum 30 s
Type 2 Minimum 10 s Maximum 25 s
(British Standard 700:1962, amendment No. 1 published 7/5/1963)
M e a s u r i n g Cylinders,—unstoppered
Nominal capacity ml
Tolerance ± ml
(British Standard 604:1952 endorsed as Australian Standard R.6-1953)
T h e r m o m e t e r s — M e r c u r y in glass type
Tolerance ± °C
British Graduation
Range °C Standard interval deg C Total Partial
immersion immersion
— 5 to + 1 0 0 593 0.1 0.2 0.4

— 20 to + 6 0 593 0.2 0.3 0.4
50 to 110 593 0.2 0.3 0.6
99 to 160 593 0.2 0.4 0.8
150 to 210 593 0.2 0.6 1.2
— 5 to + 1 0 5 1704 0.5 0.5 0.6
— 5 to + 1 0 5 593 1.0 0.3 0.6
— 5 to + 1 0 5 1704 1.0 1.0 1.0
— 5 to + 2 5 0 1704 1.0 1.0 1.0
— 5 to + 3 6 0 1704 1.0 2.0 3.0
95 to 205 593 1.0 0.5 1.0
Metric Weights
Nominal 5 3 2 1
value kg
Tolerance ± rag 250 150 100 50
10 0.05
Nominal value g 500 300 200 100 50 30 20 to to
0.1 0.001
Tolerance ± mg 25 15 10 5 2.5 1.5 1.0 0.5 0.2
For values not tabulated the tolerances are the same as those given for the next
larger tabulated value. The tolerances for burettes, graduated pipettes, graduated
cylinders, and thermometers apply to the whole of the graduated portion or to any
fraction of it.
Table XXVII—Temperature Conversion Table.

(Albert Sauveur.)
c F C F C F
— 17.8 0 32.0 16.7 62 143.6 51.1 124 255
-17.2 1 33.8 17.2 63 145.4 51.7 125 257
— 16.7 2 35.6 17.8 64 147.2 52.2 126 259
-16.1 3 37.4 18.3 65 149.0 52.8 127 261
— 15.6 4 39.2 18.9 66 150.8 53.3 128 262
— 15.0 5 41.0 19.4 67 152.6 53.9 129 264
-14.4 6 42.8 20.0 68 154.4 54.4 130 266
-13.9 7 44.6 20.6 69 156.2 55.0 131 268
— 13.3 8 46.4 21.1 70 158.0 55.6 132 270
-12.8 9 48.2 21.7 71 159.8 56.1 133 271
-12.2 10 50.0 22.2 72 161.6 56.7 134 273
— 11.7 11 51.8 22.8 73 163.4 57.2 135 275
-11.1 12 53.6 23.3 74 165.2 57.8 136 277
-10.6 13 55.4 23.9 75 167.0 58.3 137 279
-10.0 14 57.2 24.4 76 168.8 58.9 138 280
- 9.44 15 59.0 25.0 77 170.6 59.4 139 282
— 8.89 16 60.8 25.6 78 172.4 60.0 140 284
- 8.33 17 62.6 26.1 79 174.2 60.6 141 286
- 7.78 18 64.4 26.7 80 176.0 61.1 142 288
- 7.22 19 66.2 27.2 81 177.8 61.7 143 289
- 6.67 20 68.0 27.8 82 179.6 62.2 144 291
- 6.11 21 69.8 28.3 83 181.4 62.8 145 293
- 5.56 22 71.6 28.9 84 183.2 63.3 146 295
— 5.00 23 73.4 29.4 85 185.0 63.9 147 297
— 4.44 24 75.2 30.0 86 186.8 64.4 148 298
- 3.89 25 77.0 30.6 87 188.6 65.0 149 300
— 3.33 26 78.8 31.1 88 190.4 65.6 150 302
- 2.78 27 80.6 31.7 89 192.2 66.1 151 304
- 2.22 28 82.4 32.2 90 194.0 66.7 152 306
— 1.67 29 84.2 32.8 91 195.8 67.2 153 307
- 1.11 30 86.0 33.3 92 197.6 67.8 154 309
— 0.56 31 87.8 33.9 93 199.4 68.3 155 311
0.00 32 89.6 34.4 94 201.2 68.9 156 313
0.56 33 91.4 35.0 95 203.0 69.4 157 315
1.11 34 93.2 35.6 96 204.8 70.0 158 316
1.67 35 95.0 36.1 97 206.6 70.6 159 318
2.22 36 96.8 36.7 98 208.4 71.1 160 320
2.78 37 98.6 37.2 99 210.2 76.7 170 338
3.33 38 100.4 37.8 100 212.0 82.2 180 356
3.89 39 102.2 38.3 101 214 87.8 190 374
4.44 40 104.0 38.9 102 216 93.3 200 392
5.00 41 105.8 39.4 103 217 98.9 210 410
5.56 42 107.6 40.0 104 219 100 212 413
6.11 43 109.4 40.6 105 221 104 220 428
6.67 44 111.2 41.1 106 223 110 230 446
7.22 45 113.0 41.7 107 225 116 240 464
7.78 46 114.8 42.2 108 226 121 250 482
8.33 47 116.6 42.8 109 228 127 260 500
8.89 48 118.4 43.3 110 230 132 270 518
9.44 49 120.2 43.9 111 232 138 280 536
10.0 50 122.0 44.4 112 234 143 290 554
10.6 51 123.8 45.0 113 235 149 300 572
11.1 52 125.6 45.6 114 237 154 310 590
11.7 53 127.4 46.1 115 239 160 320 608
12.2 54 129.2 46.7 116 241 166 330 626
12.8 55 131.0 47.2 117 243 171 340 644
13.3 56 132.8 47.8 118 244 177 350 662
13.9 57 134.6 48.3 119 246 182 360 680
14.4 58 136.4 48.9 120 248 188 370 698
15.0 59 138.2 49.4 121 250 193 380 716
15.6 60 140.0 50.0 122 252 199 390 734
16.1 61 141.8 60.6 123 253 204 400 752
T a b l e XXVII—continued.
c F C F C F
210 410 770 282 540 1004 354 670 1238

216 420 788 288 550 1022 360 680 1256
221 430 806 293 560 1040 366 690 1274
227 440 824 299 570 1058 371 700 1292
232 450 842 304 580 1076 377 710 1310
238 460 860 310 590 1094 382 720 1328
243 470 878 316 600 1112 388 730 1346
249 480 896 321 610 1130 393 740 1364
254 490 914 327 620 1148 399 750 1382
260 500 932 332 630 1166 404 760 1400
266 510 950 338 640 1184 410 770 1418
271 520 968 343 650 1202 416 780 1436
277 530 986 349 660 1220 421 790 1454
NOTE.—The numbers in bold face type refer to the temperature either in degrees Centigrade or
Fahrenheit which it is desired to convert into the other scale. If converting from degrees Fahrenheit
to degrees Centigrade the equivalent temperature will be found in the left column, while if converting
from degrees Centigrade to degrees Fahrenheit, the answer will be found in the column on the right.
T a b l e XXVIII—Equivalents.
V o l u m e and Capacity Equivalents.
in» ft3 U K gal U S gal litres m«

1 0.0005787 0.00360 0.00433 0.01639 1.639 x I0-«
1,728 1 6.225 7.481 28.32 0.02832
277.42 0.1605 1 1.2 4.546 4.546 x 10~3
231 0.1337 0.833 1 3.785 3.785 x 10~ s
61.03 0.03531 0.22 0.2642 1 1 x 10-»
M a s s Equivalents.
kg oz lb Long ton Short ton Metric (tonne)
1 35.27 2.205 0.0009842 0.001102 0.001

0.02835 1 0.0625 0.0000279 0.00003125 0.00002835
0.4536 16 1 0.0004464 0.0005 0.0004536
1,016 35,840 2,240 1 1.12 1.016
907.2 32,000 2,000 0.8929 1 0.9072
1,000 35,274 2,205 0.9842 1.102 1
T a b l e XXVIII—continued.
D e n s i t y Equivalents.
g/ml lb/ft 3 lb/UK gal

1 62.43 10
0.01602 .1604
Linear M e a s u r e Equivalents.
km cm in ft yd mile
micro-
6
105 39,370 3,280.83 1,093.61 0.62137 metre
10- 1 0.3937 0.032808 0.010936 0.62 x 10~4
2.54 x 10- 5 2.54 0.0833 0.02778 0.158 x 10-4 3
3.048 x 10-* 30.48 12 1 0.3333 0.1894 x 10-
9.144 x 10-* 914.4 36 3 1 0.5682 x 10~ 3
10»
10*
25,400
304,801
914,402
Surface and Area Equivalents.
P r e s s u r e Equivalents.
Table XXVIII—continued.
Heat, E n e r g y a n d W o r k Equivalents.
H e a t F l o w Equivalents.
2
cal/sec cm cal/h cm 2 Btu/h ft 2
1 3,600 13,263
.0002778 1 3.684
.0000754 0.2714 1
Table XXX—Circles: Diameters, Areas, Circumferences.

Table XXXII—Capacities of Rectangular Tanks (UK gal) for Each Foot of Depth.
Tank width Tank length (ft in)

(ft in)
0-6 1—0 1-6 2—0 2—6 3—0 3-6 4—0 4—6 5-0 5—6 6-0 6—6 7—0
0—6 . 1.56 3.12 4.68 6.24 7.80 9.36 10.92 12.48 14.04 15.60 17.16 18.72 20.28 21.84
1—0 . 3.12 6.24 9.36 12.48 15.60 18.72 21.84 24.96 28.08 31.20 34.32 37.44 40.56 43.68
1-6 . 4.68 9.36 14.04 18.72 23.40 28.08 32.76 37.44 42.12 46.80 51.48 56.16 60.84 65.52
2—0 . 6.24 12.48 18.72 24.96 31.20 37.44 43.68 49.92 56.16 62.40 68.64 74.88 81.12 87.36
2-6 . 7.80 15.60 23.40 31.20 39.00 46.80 54.60 62.40 70.20 78.00 85.80 93.60 101.40 109.20
3—0 . 9.36 18.72 28.08 37.44 46.80 56.16 65.52 74.88 84.24 93.60 102.96 112.32 121.68 131.04
3—6 . 10.92 21.84 32.76 43.68 54.60 65.52 76.44 87.36 98.28 109.20 120.12 131.04 141.96 152.88
4—0 . 12.48 24.96 37.44 49.92 62.40 74.88 87.36 99.84 112.32 124.80 137.28 149.76 162.24 174.72
4—6 . 14.04 28.08 42.12 56.16 70.20 84.24 98.28 112.32 126.36 140.40 154.44 168.48 182.52 196.56
5—0 . 15.60 31.20 46.80 62.40 78.00 93.60 109.20 124.80 140.40 156.00 171.60 187.20 202.80 218.40
5—6 . 17.16 34.32 51.48 68.64 85.80 102.96 120.12 137.28 154.44 171.60 188.76 205.92 223.08 240.24
6-0 . 18.72 37.44 56.16 74.88 93.60 112.32 131.04 149.76 168.48 187.20 205.92 224.64 243.36 262.08
6—6 . 20.28 40.56 60.84 81.12 101.40 121.68 141.96 162.24 182.52 202.80 223.08 243.36 263.64 283.92
7—0 . 21.84 43.68 65.52 87.36 109.20 131.04 152.88 174.72 196.56 218.40 240.24 262.08 283.92 305.76
7—6 . 23.40 46.80 70.20 93.60 117.00 140.40 163.80 187.20 210.60 234.00 257.40 280.80 304.20 327.60
8-0 . 24.96 49.92 74.88 99.84 124.80 149.76 174.72 199.68 224.64 249.60 274.56 299.52 324.48 349.44
Table XXXIII—Capacity of Horizontal Cylindrical T a n k s at Varying Levels.

i = depth of liquid
d = diameter of vessel.
i/d fraction of i/d fraction of i/d fraction of i/d fraction of

total total total total
.01 .0017 .26 .2066 .51 .5127 .76 .8155
.02 .0048 .27 .2178 .52 .5255 .77 .8263
.03 .0087 .28 .2292 .53 .5382 .78 .8369
.04 .0134 .29 .2407 .54 .5509 .79 .8473
.05 .0187 .30 .2523 .55 .5636 .80 .8576
.06 .0245 .31 .2640 .56 .5762 .81 .8677
.07 .0308 .32 .2759 .57 .5888 .82 .8776
.08 .0375 .33 .2878 .58 .6014 .83 .8873
.09 .0446 .34 .2998 .59 .6140 .84 .8967
.10 .0520 .35 .3119 .60 .6265 .85 .9059
.11 .0598 .36 .3241 .61 .6389 .86 .9149
.12 .0680 .37 .3364 .62 .6513 .87 .9236
.13 .0764 .38 .3487 .63 .6636 .88 .9320
.14 .0851 .39 .3611 .64 .6759 .89 .9402
.15 .0941 .40 .3735 .65 .6881 .90 .9480
.16 .1033 .41 .3860 .66 .7002 .91 .9554
.17 .1127 .42 .3986 .67 .7122 .92 .9625
.18 .1224 .43 .4112 .68 .7241 .93 .9692
.19 .1323 .44 .4238 .69 .7360 .94 .9755
.20 .1424 .45 .4364 .70 .7477 .95 .9813
.21 .1527 .46 .4491 .71 .7593 .96 .9866
.22 .1631 .47 .4618 .72 .7708 .97 .9913
.23 .1737 .48 .4745 .73 .7822 .98 .9952
.24 .1845 .49 .4873 .74 .7934 .99 .9983
.25 .1955 .50 .5000 .75 .8045 1.00 1.0000
T a b l e X X X I V — A m o u n t of CaO in Milk of L i m e of Various D e n s i t i e s at 15 °C.

T a b l e X X X V — F u e l Value of B a g a s s e .
(a) G r o s s Calorific Value (B h ).
Formula B h = 8345 — 22.1 pol — 83.45 water Btu/lb.
Pol per cent bagasse

Moisture
per cent bagasse 1.0 1.5 2.0 2.5 3.0 3.5 4.0
38 5,152 5,141 5,130 5,119 5,108 5,097 5,085

39 5,068 5,057 5,046 5,035 5,024 5,013 5,002
40 4,985 4,974 4,963 4,952 4,941 4,930 4,919
41 4,901 4,890 4,879 4,868 4,857 4,846 4,835
42 4,818 4,807 4,796 4,785 4,774 4,763 4,752
43 4,735 4,723 4,712 4,701 4,690 4,679 4,668
44 4,651 4,640 4,629 4,618 4,607 4,596 4,585
45 4,568 4,557 4,546 4,535 4,523 4,512 4,501
46 4,484 4,473 4,462 4,451 4,440 4,429 4,418
47 4,401 4,390 4,379 4,367 4,357 4,346 4,334
48 4,317 4,306 4,295 4,284 4,273 4,262 4,251
49 4,234 4,223 4,212 4,201 4,190 4,179 4,168
50 4,150 4,139 4,128 4,117 4,106 4,095 4,084
51 4,067 4,056 4,045 4,034 4,023 4,012 4,001
52 3,984 3,972 3,961 3,950 3,939 3,928 3,917
53 3,900 3,889 3,878 3,867 3,856 3,845 3,834
54 3,817 3,806 3,795 3,783 3,772 3,761 3,750
55 3,733 3,722 3,711 3,700 3,689 3,678 3,667
Interpolations:
per cent moisture. .1 .2 .3 4 .5 .6 .7 .8 | .9
subtract 8 17 25 33 42 50 58 67 75
Approximate formula B h = Dry Substance x 82 Btu/lb.
(b) N e t Calorific Value (B 1 ).

Formula B 1 = 7783 — 22.1 pol — 88.27 water Btu/lb.
Moisture Pol per cent bagasse

per cent
bagasse 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5
38 4,407 4,396 4,385 4,373 4,362 4,351 4,340 4,329

39 4,318 4,307 4,296 4,285 4,274 4,263 4,252 4,241
40 4,230 4,219 4,208 4,197 4,186 4,175 4,164 4,153
41 4,142 4,131 4,120 4,109 4,098 4,087 4,076 4,064
42 4,054 4,043 4,031 4,020 4,009 3,998 3,987 3,976
43 3,965 3,954 3,943 3,932 3,921 3,910 3,899 3,888
44 3,877 3,866 3,855 3,844 3,833 3,822 3,811 3,800
45 3,789 3,778 3,767 3,756 3,745 3,734 3,723 3,712
46 3,701 3,690 3,679 3,668 3,657 3,646 3,635 3,624
47 3,612 3,601 3,590 3,579 3,568 3,557 3,646 3,535
48 3,524 3,513 3,502 3,491 3,480 3,469 3,458 3,448
49 3,436 3,425 3,414 3,403 3,392 3,381 3,370 3,358
50 3,347 3,336 3,325 3,314 3,303 3,292 3,281 3,270
51 3,259 3,248 3,237 3,226 3,215 3,204 3,193 3.182
52 3,171 3,160 3,149 3,138 3,127 3,116 3,105 3,094
53 3,083 3,072 3,061 3,050 3,039 3,028 3,017 3,006
54 2,994 2,983 2,972 2,961 2,950 2,939 2,928 2,917
55 2,906 2,895 2,884 2,873 2,862 2,851 2,840 2,829
Interpolat ions:
per cent moisture .1 .2 .3 4 .5 .6 .7 .8 .9
subtract 9 18 26 35 44 53 62 70 79
Table XXXVI—Boiling Point Elevation of Sugar Solutions and Cane

Juices (°F) at 760 mm Pressure.
Brix Purity
100 90 80 70 60 50 40
10 0.2 0.2 0.2 0.2 0.4 0.4 0.4

15 0.4 0.4 0.4 0.4 0.5 0.5 0.7
20 0.5 0.5 0.5 0.7 0.7 0.9 1.1
25 0.7 0.9 0.9 1.1 1.3 1.4 1.6
30 1.1 1.3 1.3 1.4 1.8 2.0 2.2
35 1.4 1.6 1.8 2.0 2.3 2.5 2.9
40 1.8 2.0 2.3 2.7 3.1 3.4 3.8
45 2.5 2.7 3.2 3.6 4.0 4.3 4.9
50 3.2 3.4 4.0 4.5 5.0 5.6 6.1
55 4.1 4.5 5.0 5.6 6.3 7.0 7.7
60 5.4 5.8 6.5 7.2 7.9 8.8 9.7
65 6.8 7.4 8.1 8.8 9.6 10.8 11.7
70 9.2 9.9 10.8 11.7 12.8 13.9 14.9
75 12.6 13.5 14.4 15.5 16.9 18.2 19.4
80 16.9 18.0 18.9 20.3 22.1 23.6 25.4
85 23.4 24.7 25.9 27.5 29.5 31.3 34.4
90 35.3 36.9 38.2 40.3 42.7 45.5
94 54.9
T a b l e XXXVII
Showing weights of pure sugar syrup filtered (between 2 and 7 minutes after appli-
cation of pressure) at various temperatures, under t h e standard conditions of the Rapid
Filterability Test, viz.
0.48 per cent filter aid on solids
9 . 0 pH obtained by buffer
(This table applies only to Celite 505 standardized in October 1966. When this batch is
exhausted, any further supply of filter aid will be accompanied by a table appropriate
to the new batch.)
T a b l e XXXVII—Continued
Wt. of nitrate Wt. of nitrate

Temp. °C (grammes) Temp. °C (grammes)
22.0 177 27.0 208

.1 178 .1 208
.2 179 .2 209
.3 179 .3 210
.4 180 .4 210
.5 180 .5 211
.6 181 .6 212
.7 182 .7 212
.8 182 .8 213
.9 183 .9 213
23.0 183 28.0 214
.1 184 .1 215
.2 185 .2 215
.3 185 .3 216
.4 186 .4 217
.5 186 .5 217
.6 187 .6 218
.7 188 .7 218
.8 188 .8 219
.9 189 .9 220
24.0 189 29.0 220
.1 190 .1 221
.2 191 .2 222
.3 191 .3 222
.4 192 .4 223
.5 192 .5 224
.6 193 .6 224
.7 194 .7 225
.8 194 .8 225
.9 195 .9 226
25.0 196 30.0 227
.1 196 .1 227
.2 197 .2 228
.3 197 .3 229
.4 198 .4 229
.5 199 .5 230
.6 199 .6 231
.7 200 .7 231
.8 200 .8 232
.9 201 .9 233
26.0 202 31.0 233
.1 202 .1 234
.2 203 .2 234
.3 204 .3 235
.4 204 .4 236
.5 205 .5 236
.6 205 .6 237
.7 206 .7 238
.8 207 .8 238
.9 207 .9 239
Table XXXVIII—International A t o m i c W e i g h t s , 1966
(Published by the C.R.C. Handbook of Chemistry and Physics.)
N O T E : The above atomic weights are based on the isotope CI2, whereas previous
tables were based on 0 = 16.000.
INDEX
First Aid, 181 dry, 88

safety precautions, 88
A solution, 88
Absolute juice, 1 specification, 88
Absorptiometer, 41 Bichromate filter, 27
Acid, definition of, 145 Birefringence, effect of, 21, 34
dissociation of, 144 Boiler efficiency, 166
normal solutions, 91 condensation loss, 169
Air in juice, 96 measurement, 168
Alkali, definition, 145 miscellaneous losses, 170
Alkalinity, 139, 178 sensible heat loss, 169
Alkalis, normal solutions, 91 unburnt gas loss, 170
Amici prisms, 15 Boiler water—
Analyser prism, 22 alkalinity, 84, 139, 178
Analysis of— analysis, 138, 178
bagasse, 102 reagents for, 84
boiler water, 138, 177 chemical dosage, 179
cane, 104 hardness, 141, 179
effluents, 130 phosphates, 140, 178
filter cake, (see mud) removal of oxygen, 176
gums, 126 sampling, 177
lime, 132 sugar in, 180
mud, 124 sulphates in, 142, 179
sugar, 116 sulphites in, 141, 178
water, 143 total dissolved solids, 142, 177, 179
Analytical methods— treatment, 139, 173
contents for, 94 prevention of scale, 174
for specific analyses, refer to the individual problems in sugar industry, 179
analysis involved, Boiler station, the, 166
Angular rotation, 23 Boiling house efficiency, 164
Apparent (analyses), 1 E.S.G., 165
Ash, 1 recovery, 153, 165
determination, 114 reduced, 165
Brix—
B definition, 1
Back roller juice, 1 determination—
Bagacillo, 1 by hydrometer, 95
pol added to filter cake by, 155 by pycnometer, 62
Bagasse—• by refractometer, 18, 95, 105
analysis, 102 for cane payment, 96
Brix, 153 indirect cane analysis, 105
moisture, 102 of mill products, 95
pol, 103 of sugar solution, 67
calorific value, 168 significance of, 97
definition, 1 temperature corrections in, 97
equivalent, 168 refractometer, 1
per cent cane, 154 Brix hydrometer—
preparation of sample, 81, 102 calibration, 75
samples, preservation, 81 dimensions, 67
sampling, 81 for cane payment, 96
wet disintegrator, 103 ranges, 67
Balance— requirement for cane p a y m e n t (table XXV)
analytical, 51 scale, 66, 67
constant load, 52 temperature of calibration, 67
for coarse weighing, 51, 57 temperature corrections, 67, table 1
requirement for cane payment (table XXV) tolerance, (table XXV)
sensitivity, 52 Buffer solutions—
setting up the, 53 reagents for, 85
testing, 55, 77 Bulk density, prepared cane, 1
weighing, 54 Burettes—
weights, 53 calibration, 71
Basic lead acetate— specification, (table XXV)
analysis, 88 tolerance, 71
244
c Clarifiability test, 133

Calcite, 21, 22 reagents, 85
Calculations in chemical control, 151 Clarified juice—
boiling house efficiency, 164 definition, 2
boiling house recovery, 153, 165 per cent cane, 156
c.c.s. formula, 2, 106 pH measurement, 149
clarified juice per cent cane, 156 phosphates, 129
coefficient of work, 165 turbidity measurement, 42
concentration and evaporation, 156 Cleansing solution, glassware, 69, 86
crystal content, 161 Clerget—
dilution, 155 divisors, 111
equivalent standard granulated, 161 method for sucrose, 108
evaporation coefficient, 156 Coal, calorific value, 168
expected purity of molasses, 161 Coefficient of supersaturation, 136
extraction, 153 Coefficient of work, 165
reduced extraction, 163 definition, 2
maceration per cent fibre, 155 upper limit, 165
materials balances, 151 Colorimetry, 42
overall recovery, 153 Colorimetric determination—
pol balance, 152 p H , 145
empirical system, 152 phosphates, 128
direct analysis, 153 starch, 123
recovery formulae, 157 Colour, in raw sugar, 124
S.J.M., 157 Commercial cane sugar—
Winter-Carp., 157 definition, 1
retention (rotary fiters), 156 formula, 2
taking stock, 159 Co mparator—
weekly report, 160 colour, 140
to date averages, 162 measurement of pol tubes, 77
Calibration of— measurement of p H , 146
Brix hydrometers, 75 Compression ratio (milling), 2
pol tubes, 75, 77 Concentration, definition, 136
thermometers, 75 Concentration and evaporation formulae, 156
volumetric glassware, 69, 77 Condensate, 2
burettes, 71 sugar in, 180
flasks, 70 Condensation loss, 169
measuring cylinders, 73 Continuous sampler, 79
pipettes, 72 Corrosion, in boilers, 139, 175
Calomel electrode, 147 Cover glasses, 77
Calorific values of fuels, 167 requirement for cane payment (table XXV)
Canada balsam, 21 strain, 37, 77
Cane— Crystal content, 2, 161
analysis, 104 Crystallizer drop, 2
direct, 104 Cutter-grinder, 105
whole stalk, 107 Cyclone purity of molasses, 2, 136
Brix by disintergrator method, 105 Cylinders, measuring, 73
C.C.S., 1, 106
definition, 1 D
fibre, 107 Definitions, 1
maturity, 19, 78 Densimetric methods of analysis, 58
moisture, 105 hydrometer, 65
pol in cane, 152 pycnometer, 60
pol by disintergrator method, 105 Density of a substance, 58
pol in open cells, 106 relative, 58
sample preparation, 105 Dextran, 3
sampling, 78 Dextrorotation, 23
Cane maturity, 78 Dichroic film, 20
by refractometer, 19 Diffraction grating, 41
Caustic cleaning solution— Dilution indicator, 3
determination of concentration, 133 Dilution, per cent clarified juice, 155
Caustic embrittlement, 175, 179 per cent fibre, 155
CCS — per cent mixed juice, 155
definition, 1 per cent undiluted juice, 3, 155
formula, 2 Dilution water, 3, 155
Cell- Disintegrator, wet, 103, 104
Faraday, 30, 33 Dispersion—
saturation, 137 prism, 10
Chemical control, calculations, 151 rotatory, 24, 26
Chemical dosage of boilers, 179 Dissociation constant of water, 144
INDEX 245
Dosage of chemicals to boilers, 179 specification, (table XXV)

Double refraction, 21 standardization, 70
Dry substance— sugar polarization, 117
definition, 3 tolerance, 71
determination, 100 Flue gas—
Josse method, 101 composition, 171
sand method, 100 heat losses in, 171
Drying oven, Spencer type, 102 temperature, 171
volume, 171
E Formula—
c.c.s., 2
E.D.T.A., 85 crystal content, 161
Effets, overall evaporation coefficient of, 156 expected purity of molasses, 161
Effluents, sugar detection in, 130 gross calorific value of bagasse, 168
Electrode— lost undiluted juice per cent fibre, 164
calomel, 147 net calorific value of bagasse, 168
glass, 148 recovery, 157
hydrogen, 146 S.J.M., 157
Electrolytes, 144 Winter-carp, 158
Electrolytic dissociation theory, 144 reduced extraction, 163
Equivalent bagasse, 168 Fuel—•
Equivalent Standard Granulated (E.S.G.), bagasse moisture influence, 173
161 calorific value, 167
Escribed volume, 3 equivalent bagasse, 168
Evaporation coefficient of effets, overall, 156 used, 167
Evaporation formula, 156 weight of fuel, 167
Expected purity of molasses, 161
Extraction— G
calculation, 153 Glass electrode, 148
definition, 3 Glassware—-
pol, 3, 153 calibration, 69, 77
reduced, 6, 163 cleansing solution, 69, 86
Extraneous matter, 3 volumetric, 69
specifications, 69
F tolerances, (table XXV)
Fans— Grain size, raw sugar, 121
boiler, 171 Gravity solids, 4
forced draught, 172 purity, 4
horse power required, 172 Grist, raw sugar, 121
induced draught, 171 Gums, 4
performance, 172 analysis, 126
Faraday effect, 23 reagents for, 93
Faraday cell, 30, 33
Fehling's solutions— H
reagents, 90 Half shadow angle, 25
standardization, 90 Hand refractometer, 18
Fibre— Hardness analysis, boiler water, 141, 179
definition, 3 Heat-
determination— in steam, 166
prepared cane method, 107 losses, 168
whole stalk method, 107 condensation, 169
in bagasse, 153 in flue gas, 171
in cane, 78, 107 sensible heat, 169, 171
in mud, 126 unburnt gas, 170
Filling ratio, 3 required, by factory, 170
Filter— Herles' reagent, 87
retention, 156 Hydrochloric acid—
washing water, 155 for sucrose inversion, 92
Filterability— normal solution, 91
definition, 3 Hydrogen electrode, 146
reagents for, 85 Hydrogen ion concentration (see pH), 144
test, 119 Hydrometer, 65
Filter cake (see Mud), 3, 125 Brix, 66, 67
sampling, 82 requirement for cane payment (table XXV)
Filtrate, 3 for total dissolved solids in boiler water,
Final molasses (see molasses) 142, 179
First aid, 181 scale, 65
First expressed juice, 3 testing of, 75
Flasks, 69, 70 Hygroscopic water, 4, 104, 105
246 INDEX
I I Light-
Imbibition, 4 amplitude of wave, 8
Impurities, 4 dispersion, 10, 15, 18, 24, 27
Indicators, 86, 145 double refraction, 21, 34
pH range, 86 filter, 27, 29, 31, 32
preparation, 86 frequency, 9
Insoluble solids— linearly polarised, 9, 20
in clarifier feed, 124 monochromatic, 17, 24, 26, 41
in mud, 124 nature of, 8
International sugar scale, 24, 35 plane polarized, 9, 22
ICUMSA definition, 35 refraction, 9
Interference filter, 32, 33 source, 10, 26
Inversion of sucrose— spectrum, 8, 10
by hydrochloric acid, 108, 110 wavelengths, 8
by invertase, 108 Lime—
Walker method, 110 addition, 149
U.S. Customs method, 111 automatic to juice, 149
Invertase, 108, 110, 112 analysis—
Invert sugar, 4 available CaO, 132
standard solution, 90 neutralizing value, 132
Ions, 144 pH control, 149
quality, 132
Lime sucrose reagent, 85
J Lippich polarizer, 25
Jackson-Gillis modification IV, 110 Litre, 68
divisors, 111 Losses—
method, 110 heat, 169
reagents, 92 miscellaneous, 170
J a v a ratio, 4 pol, 152
Juice— undetermined, 152
absolute, 1 Lost undiluted juice per cent fibre, 164
air bubbles in, 96
back roller, 1 M
Brix, 1, 95 Maceration—-
clarified, 2 definition, 4
per cent cane, 156 per cent fibre, 155
p H , 149 Magma, 4
extraction, 3 Magnification, 45
first expressed, 3 Massecuite—
gums in, 127 composition formula, 160
last expressed, 4 crystal content, 161
lost undiluted, per cent fibre, 164 definition, 4
mixed, 4 purity, 4
p H , 149 sampling, 80
phosphate, 129 Materials balances—
pol, 97 pol balance, 152
preservation, 89 quantitative data, 151
primary, 5 stock, 152, 159
residual, 6, 104 Maturity testing, 19, 78
sampling, 79 Meniscus—
suspended matter in, 96 correction, 96
temperature, 96 setting of, 69, 70, 71
undiluted, 6 Metrology laboratory, 75
lost in bagasse, 164 N.A.T.A. registration, 75
Microscope, 8, 42
construction, 43
L micrometer eyepiece, 47
Laboratory reagents, 83 micrometer stage, 47
Laevorotation, 23 projection type, 48
Last expressed juice, 4 table of magnifications, 45
Lead acetate— Millilitre, 68
basic, 88 Milling—
neutral, 89 efficiency, 163
powder, 88 extraction, 3, 153
solution, 88 loss, 4
specifications, 88 lost undiluted juice in bagasse, 164
Lead compounds, 88 performance criteria, 163
safety precautions, 88 reduced extraction, 6, 163
Lenses, 45 Mixed juice, 4
INDEX 247
Moisture— P
bagasse, 102 Pellet's continuous tube, 37
cane, 105 pH—
filter cake, (see mud) brom. thymol blue disc, 146
mud, 126 buffer solutions, 85, 149
raw sugar, 119 clarified juice, 149
Spencer-type oven for, 102 colour comparator, 146
Molasses— control, 149
analysis— definition, 144
Brix, 95 determination, 144, 149
pol, 100 indicators, 86, 145
reducing sugars, 112 measurement, 145
sucrose, 112 colorimetric method, 145
total sugars, 112 electrometric method, 146
calorific value, 168 meters, 149
cyclone purity, 2, 136 recorder, 149
definition, 4 sugar mill products, 149
expected purity ,161 temperature compensation, 149
in stock, 158 test papers, 145
measuring device, 159 value of boiler water, 178
sampling, 80 Phosphates—
supersaturation coefficient, 136 analysis, 87, 94, 128
Monochromatic light, 17, 24, 26, 41 reagents for, 87
Mud- colour comparator, 140
analysis, 124 determination in—
fibre, 126 boiler water, 140, 178
insoluble solids, 124 juice, 129
moisture, 126 raw sugar, 128
pol, 126 syrup, 129
soluble solids, 125 soluble and insoluble, 129
solids, 4 Photomicrography, 49
Photomultiplier, 31, 34
N Pipettes—
N.A.T.A. registrations, 75 calibration, 72
Net titre, 5 delivery time, 72
Nicol prism, 21 graduated, 73
Non sucrose, 5 specification, (table XXV)
Non sugars, 5 tolerance, 73
Normal quartz plate, 35 Pneumercator, 159
Normal solutions, 91 Poisons, 83
Pol-
Normal sugar solution, 35 added to filter cake by bagacillo, 155
definition, 36 balance—
formula for calculation of wavelengths, 37
rotation of, 35 empirical system, 152
Normal weight, 5, 36 direct analysis, 153
No-void volume, 5 definition, 5
determination—
bagasse, 103
o cane, 105
Oil- juice, 97
calorific value, 168 molasses, 100
Optical activity, 9, 23 mud, 126
quartz, 23 pan products, 100
sugar solutions, 23 sugar, 116
Optical instruments, 8 temperature corrections, 38, 99, 118
care of, 49 extraction, 3, 153
microscope, 42 indirect cane analysis, 105
projection type, 48 in open cells, 106
polarimeter, 24 losses, 152
refractometer, 11 methods of analysis—
saccharimeter, 24, 26 dry lead, 97
spectrophotometer, 40 Herles', 99
Optic axis, 21, 23 normal weight, 98
Other organic matter, 5 reagents for, 87
Oven— Polarimeter—
Spencer type, 102 automatic, 8, 24, 29
Overall evaporation coefficient of effets, 156 construction of, 24, 30
Overall recovery, 153 photo electric, 30
Oxygen, in boiler water, 175 requirement for cane payment (table XXV)
248 INDEX
standardization, 35 net titre, 5

sugar, 26 other organic matter, 5
Polarimeter tubes, 37, 75 sampling, 80
calibration, 75, 77 temperature corrections for pol, 39, 118
requirement for cane p a y m e n t (table XXV) tons E S G , 161
Polarimetry, 23 Reabsorption factor, 6
Polariscope (see Polarimeter and sacchari- Reagents for—
meter) boiler water analysis, 84
Polarized light, 20 buffer solutions, 85
by dichroic film, 20 clarifiability test, 85
extraordinary ray, 21 filterabihty, 85
linearly, 20, 23 glass cleaning solution, 86
ordinary ray, 21 indicators, 86
Polarizer prism, 21 phosphate analysis, 87
Prepared cane analysis, 104 pol determination, 87
Preservation of samples— preservatives, 89
for analysis, 81, 89 reducing sugar analysis, 90
for storage conditions, 89 standard acids and alkalis, 91
Preservatives, 89 starch analysis, 92
reagents for, 89 sucrose analysis, 92
Pressure filter, 120 sugar detection, 92
purity of molasses, 136 water analysis, 93
Primary juice 5 Recovery—
Primary mud, 5 boiling house, 153
Prisms— E S G , 161
amici, 15 formula, 157
analyser, 22 overall, 153
calcite, 21 pol in stock, 159
dispersion, 10, 15 reduced overall, 165
Nicol 21 Reduced extraction, 6, 163
polarizer, 21, 25 Reducing sugars—
refractometer, 14, 17 definition, 6
Purity— determination, 113
apparent, 1, 5 molasses, 112
gravity, 5 reagents for, 90
true, 5 total, 112
Pycnometer, 60 Reducing sugar ash ratio, 6, 114
constant, 63 Refractive index, 9
temperature effects, 63 angle of incidence, 9, 11
determination— angle of refraction, 9
Brix 62 impure sugar solutions, 18
specific gravity, 62 measurement, 11, 19
volume, 60 temperature effect, 10, 18
Refractometer, 8, 11
Q Abbe, 14
adjustment, 16
Quartz plates, 35 automatic, 8, 19
compensator, 27 critical angle, 11, 19
for Bendix polanmeter, 35 dipping or immersion, 17
normal, 35 dry substance determination by, 18
specification (table XXV) hand, 18
standardization of polarimeters by, 35 high accuracy, 17
strain, 77 requirement for cane p a y m e n t (table XX 1
testing, 35, 77 scale, 18
Quartz wedge compensation, 26 testing of, 77
Refractometer Brix, 1, 6, 18
R Relative density, 58
Raw sugar— Remelt, 6
analysis, 116 Residual juice, 6
ash, 115 Retention, rotary filter, 156
colour, 124 Rotatory dispersion, 24, 26
moisture, 119
phosphates, 128 S
polarization, 116 Saccharimeter, 8, 24, 26
reducing sugars, 113 automatic, 30
starch, 123 calibration of scale, 28, 77
dilution indicator, 3 construction, 27
filterability test, 119 definition, 26
gram characteristics, 121 effect of illumination, 29
INDEX 249
examination, 77 trace sugars, 130

influence of temperature, 39 turbidity measurement, 42
International sugar scale, 24, 35 Spencer-type drying oven, 102
light filter, 27, 29, 31, 32 Standard invert sugar solution, 90
quartz wedge compensation, 27 Standardization—
requirement for cane payment (table XXV) acids and alkalis, 91
scale, zero adjustment, 29 Fehling's solution, 90
standardization, 35 normal solutions, 91
tolerance, 77 polarimeters, 35
Sample— quartz plates, 77
container, 79, 82 refractometers, 18
identification, 79 soap solution, 141
preservation, 82, 89 weights, 56, 77
Sampler— Starch-
automatic, 79 indicator solution, 84
care of, 82 in raw sugar, 123
continuous, 79 reagents for analysis, 92, 123
pitot tube type, 80 standard solution, 92, 123
Sampling— Steam—
bagasse, 81 dry saturated, 167
boiler water, 177 heat required, 166
cane, 78, 107 produced, 166
prepared, 78 superheated, 166
filter cake, 82 Stock—
juice, 79 bulk sugar in, 160
massecuite, 80 materials balance, 152
molasses, 80 molasses in, 158
raw sugar, 80 taking, 159
syrup, 80 Strain, in glass, 23, 34
Saturation-definition, 136 Sucrose—
Saturation cell, 137
Scale on boiler heating surfaces, 174 analysis, 92, 108, 112
Schmitz's table for pol, formula, 99 reagents, 92
Seed, 6 definition, 6
in high purity material, 108
Sensible heat loss, 169 in low purity material, 112
Set opening, 6 methods—
Settling test, C.S.R. laboratory, 133 chemical, 112
Sieves— Clerget, 108, 110
British standard, 122 invertase, 108
Tyler, 122 Jackson and Gillis modification IV, 110
S.J.M. formula, 157 normal weight, 5, 36
Sodium D line, 10 recoverable, 157
Solids- solubility, definition, 136
dissolved, in boiling water, 142, 179 Sugar analysis—
in mud, 124 ash, 115
insoluble, 124 filterability, 119
soluble, 125 grain size, 121
soluble, 1 moisture, 119
suspended- phosphate, 128
definition, 6 polarization, 116
in juices, 96 reducing sugars, 113
total dissolved—boiler water, 142 starch, 123
Solubility coefficient, 136 total colour attenuation, 124
Specific gravity— Sugar, definition, 6
bottle, 60 Sugars—
definition, 58
determination, 59 by refractometer, 18
by hydrometer, 65 detection of, in effluents, 130
by pycnometer, 60, 62 in boiler water, 180
sugar solutions, 59 influence of temperature on rotation, 38
Specific rotation, 23 99, 118
Spectrophotometer, 8, 40 optical rotation of, 23
optical system, 41 reducing, 6, 113
use of— specific gravities of, 59
total, 112
colour, total, 124 Sugar detection—
gums, 126 methods, 130
phosphate determination, 128, 140 reagents, 92
starch determination, 123 Supercel, 87
250 INDEX
Supersaturation— Undiluted juice, 6

coefficient, 136 dilution per cent, 155
determination, 136 lost in bagasse per cent fibre, 164
Suspended solids, 6
in juice, 96 V
Syrup— Verdet constant, 23
definition, 6 Volumetric coefficient, 6
phosphate determination in, 129 Volumetric equipment, 68
sampling, 80
units of volume, 68
T Volumetric glassware, 69
Tar, calorific value, 168 calibration, 77
Temperature e f f e c t s - meniscus setting, 69, 70, 71
boiler feed water analysis, 142, 177 specifications, 69
pH determination, 145 standard temperature, 69, 70
pol reading, 38, 99, 118 W
refractive index, 10
sugar solutions, 38, 99, 118 Water—
Thermometer, 73 analysis—
calibration, 75 chlorides, 143
emergent column error, 74 reagents, 93
requirement for cane payment (table XXV) dilution, 3
To date, averages, 162 dissociation constant, 144
Tolerances for laboratory apparatus (see hygroscopic, 4
table XXV) Weighing—
Total dissolved solids—boiler water, 142, 179 by substitution, 52
Total sugars— coarse, 57
by refractometer, 18 general precautions in, 54
definition, 6 method of, 54
estimation of, 112
Toxic materials, 83 Weighted average for " t o d a t e " figures, 162
True purity, 5 Weights—
Turbidimeter, 8 requirement for cane p a y m e n t (table XXV)
Turbidity, 6 standardization, 77
Turbidity measurement, clarified juice, 42
tolerances (table XXV)
U Winter-Carp formula, 158
Unburnt gas loss, 170 Wood, calorific value, 168
Undetermined loss, 152 Work opening, 7
Work ratio, 7

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BUREAU OF SUGAR EXPERIMENT STATIONS QUT j

Wholly set up and printed in Australia by

W h e r e v e r possible, descriptions and illustrations of apparatus cover t h e most modern

The Bureau of Sugar Experiment Stations wishes to acknowledge t h e assistance given

Bureau of Sugar Experiment Stations, Brisbane.

milling and refining operations were conducted at a prescribed

Gravity Purity—See Purity.

Non-Sucrose—The difference between dry substance and sucrose.

The term purity alone generally signifies apparent purity.

Fig. 1—Illustrating the principle of a light wave.

Fig. 1 represents a wave in which the vibration is at right angles to the

Fig. 2—Illustrating the law of refraction.

Fig. 3—Illustrating the measurement of critical angle,

Fig. 4—The essential parts of an Abbe refractometer.

Fig. 5—The principle of the Abbe refractometer.

Fig. 6—Abbe refractometer by Carl Zeiss, W. Germany.

Fig. 7—High accuracy refractometer by Bellingham and Stanley, London.

Fig. 8—High accuracy immersion refractometer with temperature controlled prisms by

With high accuracy refractometers the scale is not calibrated in refrac-

Fig. 9—Hand refractometer by Atago Optical Works, Japan.

Fig. 10—Typical field of a hand refractometer.

Fig. 11—Illustrating double refraction of light in calc spar.

Fig. 12—Illustrating the principle of the Nicol prism.

II. Crossed Nicols.

W h e n linearly polarized light passes t h r o u g h a birefringent crystal, it

Sucrose +66.54 Laevulose —92.5

In any method of polarimetry, the solution is placed in a cell of known

Fig. 14—Showing the essential parts of the simple polariscope.

The three-field alternative has an even greater sensitivity but, if the

intensity. The reduction of intensity affects the posit-

Fig. 1 7—Showing the construction of single wedge quartz compensation.

Fig. 18—Illustrating the parts of a saccharimeter.

plate. The sugar solution under examination is contained in the cell g; h is a

Fig. 19—Illustrating a Schmidt and Haensch saccharimeter.

of 10 °S subdivided into 100 divisions is also provided whereby the reading

The polarimeter is balanced in one of three ways, corresponding to the

Fig. 22—Schematic layout of Hilger M560 automatic polarimeter.

mechanical digitizer disc; this consists of a number of miniature commutator

Fig. 23—Diagram of Zeiss OLD digital polarimeter.

Fig. 24—Diagram of Bendix-NPL automatic polarimeter Type 700.

would change if the instrument were turned around on a table. It is therefore

about the direction given by the polarizer. A modulation frequency of 380 Hz

The International Sugar Scale

Fig. 25—Polarimeter tubes, a

colorimeters, or, more correctly, photoelectric absorptiometers. These instru-

Fig. 26—The Spectronic 20, Bausch and Lomb

operation of the instrument is as follows:—White light emanating from the

Fig. 27—Schematic optical diagram of Spectronic 20.

ACTUAL PATH OF LIGHT.

RAY PATH OF VIRTUAL IMAGE.

i Fig. 28—The essential parts of a microscope.

uses for w h i c h a fairly h i g h d e g r e e of m a g n i f i c a t i o n is r e q u i r e d . H e n c e , w h i l s t

The Structure and Operation of the Microscope

Objective focal Objective or initial |

An objective is always designed to be used with a certain tube length,

ing a coverslip over t h e whole. F o r pan-stage observations w i t h v e r y low

gives the magnification of the particular optical set-up of the microscope.

Fig. 29—A projection microscope of medium cost (Maruzen).

of nearly 7 in diameter. The standard lens supplied (x 10) is of sufficient

The Care of Optical Instruments

be experienced when an attempt is made to remove them. In some sacchari-

Fig. 30—-A modern single pan constant load balance (Sartorius).

Fig. 31—Diagrammatic representation of a single pan constant load balance (Sartorius).