Labortory Manual For South African Sugar Factories

QUT
Library
LABORATORY MANUAL
F OR
S OUTH AF RI C AN SUGAR F ACTORI ES
S OUTH AFRI CAN
SUGAR TECHNOLOGI STS' ASSOCI ATI ON
2 2 8 1 0 6 1 7 B
First published 1962 by the
SOUTH AFRICAN SUGAR TECHNOLOGISTS' ASSOCIATION
c/o S.A.S.A. EXPERIMENT STATION
MOUNT EDGECOMBE, NATAL
Text set in 10 Pt. Times Roman
Printed in the Republic of South Africa
by Hayne and Gibson Ltd.
50-60 Ordnance Road, Durban
P RE F AC E
One of the outstanding services rendered by the South African Sugar
Technologists' Association to our Sugar Industry has been its contribu-
tion to chemical control in our factories. This subject has formed an
integral part of our activities ever since the inception of our Association
in 1926 and the "Official Methods of the S.A. Sugar Technologists'
Association for Chemical Control" were published in 1927 as part of
the Proceedings of the first Annual Conference of the Association.
Revised editions were published in 1930 and 1931 in the Proceedings of
the fourth and fifth Annual Congresses. After a later major revision,
these methods, suitably augmented, appeared in a separate booklet under
the title "South African Sugar Technologists' Association Recommended
Methods of Chemical Control in which are included the Official Methods".
This publication became known as the "Recommended Methods" and
served the Industry well for more than 25 years. The need for further
revision and also the inclusion of additional useful methods has however
now been felt for some years and in fact "The Committee for Standardiza-
tion of Chemical Control" has remained most active throughout the
intervening years.
This first edition of the "Laboratory Manual for South African
Sugar Factories" is in fact the fifth publication of methods of chemical
control issued by the South African Sugar Technologists' Association
and it supersedes the "Recommended Methods of Chemical Control".
The loose cover now used will facilitate future alterations or additions
which can now be done by simply replacing or adding the necessary pages.
Members of the Chemical Control Committee have spent very many
hours over a period of years in endeavouring to give the Industry the
best. On behalf of the South African Sugar Technologists' Association
I wish to extend to the Committee and its members our most grateful
thanks.
The South African Sugar Industry is justly proud of the chemical
control practised in its factories, and there can be no doubt that this
manual will prove a great asset in the laboratories. I therefore have
pleasure in welcoming the "Laboratory Manual for South African Sugar
Factories" as a further worthwhile contribution by our Association to
the chemical control of the South African Sugar Industry.
J. L. DU TOIT
President
JUNE, 1962. S. Afr. Sugar Technologists' Association
C ONTE NTS
PAGE
Chapter I Definitions 1 - 1962
Chapter II The determination of factory weights
1. General 7 - 1962
2. Cane 7 - 1962
a. The weighbridge, tares . . . . . . 7 - 1962
b. S.A.R. trucks 8 - 1962
c. Tram trucks . . . . . . . . 8 - 1962
d. Wagons, lorries and trailers . . . . 8 - 1962
e. Chains 9 - 1962
f. Loading poles . . . . . . . . 9 - 1962
3. Imbibition water . . . . . . . . . . 9 - 1962
4. Mixed juice 9 - 1962
a. General 9 - 1962
b. Non-automatic scales . . . . . . 9 - 1962
c. Automatic scales . . . . . . . . 10 - 1962
5. Bagasse 11 - 1962
6. Final molasses . . . . . . . . . . 11 - 1962
7. Filter cake 11 - 1962
8. Sugar 11 - 1962
9. Burnt lime, Sulphur and Phosphoric acid . . 11 - 1962
Chapter III Calculations
1. General 1 2 - 1962
2. Calculation of quantities in stock .. .. 12 - 1962
3. Recording of decimal fractions .. .. .. 13 - 1962
4. Rules for rounding off . . .. . . . . 14 - 1962
5. Standardization of methods of calculation .. 14 - 1962
a. Weights 14 - 1962
b. Percentages and ratios . . . . . . 16 - 1962
c. Miscellaneous formulae . . . . . . 16 - 1962
6. Sugar Milling Research Institute monthly period
calculation sheet . . . . . . . . 18 - 1962
7. Sucrose balances . . .. . . . . .. 2 0 - 1962
Chapter IV Description and use of standard equipment
1. General 2 2 - 1962
2. Instruments . . . . . . . . . . 22 - 1962
a. Saccharimeters . . . . . . . . 22 - 1962
b. Light filters 22 - 1962
c. Illumination . . .. . . . . 22 - 1962
d. Saccharimeter tubes and cover glasses. . 22 - 1962
e. Quartz plates 23 - 1962
f. Thermometers for the Clerget analysis . . 23 - 1962
g. Brix hydrometers . . . . . . . . 23 - 1962
h. Hydrometer j ars .. .. .. .. 24 - 1962
j. Volumetric glassware . . . . . . 24 - 1962
k. Sugar flasks 24 - 1962
1. Pipettes 25 - 1962
m. Beaker flasks 26 - 1962
n. Bagasse digestion apparatus . . . . 26 - 1962
o. Counterpoise weights . . . . . . 26 - 1962
Laboratory Manual for S. Afr. Sugar Factories 1962 V
PAGE
Chapter V Sampl i ng
1. General 27 - 1962
2. Cane 28 - 1962
3. Bagasse 29 - 1962
4. First expressed juice . . . . . . . . 30 - 1962
6. Last expressed juice . . . . . . . . 33 - 1962
7. Sulphited mixed juice . . . . . . . . 33 - 1962
8. Clarified juice and filtered juice . . . . . . 33 - 1962
10. Syrup 33 - 1962
11. Massecuite (from pan) .. .. .. .. 35 - 1962
12. Massecuite (from crystallizer) . . . . . . 35 - 1962
13. Molasses 3 5 - 1962
14. Sugar 35 - 1962
Chapter VI Reagents
1. General 3 8 - 1962
2. Clarifying reagents . . . . . . . . 38 - 1962
a. Lead subacetate solution for general use 38 - 1962
b. Neutral lead acetate solution . . . . 38 - 1962
c. Dry subacetate of lead . . . . . . 38 - 1962
d. Alumina cream (aluminium hydroxide) 40 - 1962
3. Indicators 40 - 1962
a. Indicators for measurement of pH .. 40 - 1962
b. Neutral water for dilution of indicators 40 - 1962
c. Buffer solutions . . . . . . . . 40 - 1962
d. Indicator solutions made up in the
laboratory .. .. .. .. 40 - 1962
4. Standard acid and alkali solutions . . . . 41. - 1962
5. Iodimetry 42 - 1962
a. General 42 - 1962
b. Preparation of N/32 sodium thiosulphate
solution.. .. .. .. .. 4 2 - 1962
c. Standardization of N/32 sodium thiosul-
phate solution . . . . . . . . 42 - 1962
d. Preparation of iodine stock solution,
N/1.6 approx 4 3 - 1962
e. Preparation of N/32 iodine solution . . 43 - 1962
f. Standardization of N/32 iodine solution 43 - 1962
6. For the determination of sucrose . . . . 43 - 1962
a. Hydrochloric acid solution . . . . 43 1962
b. Sodium chloride solution. . .. .. 43 - 1962
7. For the determination of reducing sugars .. 43 - 1962
a. Preparation of standard invert sugar
solution . . . . . . 43 - 1962
b. Preparation of Fehling's solution,
Soxhlet's modification . . . . 44 - 1962
c. Standardization of Fehling's solution . . 44 - 1962
d. Preparation of Luff-Schoorl solution . . 44 - 1962
8. Juice preservative . . . . . . . . . . 45 - 1962
9. For the determination of calcium and mag-
nesium . . . . . . . . . . .. 45 - 1962
a. Ethylenediaminetetraacetic acid.. .. 45 - 1962
b. Standard calcium chloride solution . . 45 - 1962
c. Buffer solution (according to Saunier
and Lemaitre) . . . . . . . . 45 - 1962
d. Eriochrome black T . . . . . . 45 - 1962
e. Murexide . . . . . . . . 45 - 1962
f. Caustic soda solution . . . . . . 46 - 1962
g. Standardization of ethylenediaminetetra-
acetic acid solution . . . . . . 46 - 1962
VI 1962 Laboratory Manual for S. Afr. Sugar Factories
PAGE
10. For the determination of available phosphate .. 46 - 1962
a. Ammonium molybdate solution . . .. 46 - 1962
b. Reducing solution . . . . . . 46 - 1962
c. Standard phosphate solution . . . . 46 - 1962
d. Diluted standard phosphate solution . . 46 - 1962
11. For the determination of sulphur dioxide (modi-
fied Monier-Williams method) . . . . 46 - 1962
a. Hydrogen peroxide solution . . . . 46 - 1962
b. Hydrochloric acid, concentrated. . .. 46 - 1962
c. Sodium hydroxide solution, N/50 . . 46 - 1962
d. Alkaline pyrogallol solution . . . . 46 - 1962
Laboratory Manual for S. Af r . Sugar Factories 1963 VI I
Chapter VII General methods of analysis
1. Temperature .. .. .. .. .. 47 - 1962
2. Filtration 47 - 1962
3. Brix 47 - 1962
4. Polarization, pol or apparent sucrose . . . . 48 - 1962
a. Horne's dry lead method . . . . 48 - 1962
b. Normal weight method . . . . . . 48 - 1962
5. Sucrose 4 9 - 1962
a. Using acid inversion (modified Jackson
and Gillis method IV) . . 49 - 1962
b. Using invertase . . . . . . . . 50 - 1962
c. The "chemical" method . . 51 - 1963
6. Reducing sugars . . . . . . . . 52 - 1963
a. The Lane and Eynon method . . 52 - 1963
b. The Luff-Schoorl method . . . . 5 3 - 1962
7. Sulphur dioxide 53 - 1962
a. The iodine-titration method .. 53 - 1962
b. The rapid method of determining avail-
able SO
s
in sugars 53 - 1962
c. The Monier-Williams method . . . . 54 1962
8. The conductivity of solutions of white sugars .. 55 - 1962
9. Calcium and magnesium (by a modification of
the Schwarzenbach method) . . . . . . 55 - 1962
10. Moisture 56 - 1962
11. pH 5 6- 1962
12. Titrated acidity or alkalinity . . . . . . 56 - 1962
13. Sulphated ash 5 6 - 1962
14. Test for traces of sugar in waters (Skarblom
test) 57 - 1962
Chapter VIM Analysis of products
1. Cane 58 - 1962
a. Sucrose % cane . . . . . . . . 58 - 1962
i. General factory method . . . . 58 - 1962
ii. Java ratio method . . . . 58 - 1962
iii. Test mill analysis . . . . . . 58 - 1962
b. Fibre % cane 59 - 1962
i. General factory method . . . . 59 - 1962
ii. Direct method 59 - 1962
iii. Indirect method . . . . . . 60 - 1962
2. Final bagasse . . . . . . . . . . 60 - 1962
a. Pol % bagasse . . . . . . . . 60 - 1962
b. Moisture % bagasse . . . . . . 60 - 1962
3. Bagacillo 61 - 1962
4. All juices other than mixed juice . . . . 61 - 1962
a. Brix 61 - 1962
b. Pol 61 - 1962
c. Reducing sugars . . . . . . 61 - 1962
d. Acidity or alkalinity . . . . . . 61 - 1962
VI I I 1963 Laboratory Manual for S. Afr. Sugar Factories
PAGE
e. Sulphur dioxide . . . . . . 61 - 1962
f. pH 62 - 1962
g. Calcium and magnesium . . . . . . 62 - 1962
a. Brix 62 - 1962
b. Pol 62 - 1962
c. Clerget sucrose by the Jackson and Gillis
method IV 62 - 1962
d. Clerget sucrose by the invertase method 64 - 1963
e. Reducing sugars . . . . . . 65 - 1962
f. Calcium and magnesium . . . . . . 65 - 1962
g. Available phosphate . . . . . . 65 - 1962
6. Syrup 66 - 1962
a. Brix 66 - 1962
b. Pol 66 - 1962
c. Reducing sugars . . . . . . 66 - 1962
d. Sulphur dioxide . . . . . . 66 - 1962
e. Hydrogen ion concentration (pH) 66 - 1962
a. Pol 66 - 1962
b. Moisture . . 66 - 1962
8. Massecuites . . . . . . . . 66 - 1962
a. Brix 67 - 1962
b. Pol 67 - 1962
c. Crystal content . . . . . . 67 - 1962
9. Molasses excluding final molasses and wash . . 67 - 1962
a. Brix 67 - 1962
b. Pol (for stocktaking) 67 - 1962
10. Final molasses . . . . . . . . . . 67 - 1962
a. Brix 67 - 1962
b. Dry substance . . . . . . . . 67 - 1962
c. Sucrose 68 - 1962
i. The Jackson and Gillis method IV 68 - 1962
ii. The chemical method, using in-
vertase .. .. .. .. 69 - 1963
d. Reducing sugars . . . . . . . . 70 - 1963
e. Total sugars . . . . . . . . 70 - 1963
f. Sulphated ash 70 - 1963
11. Sugars 70 - 1963
a. Pol 70 - 1963
b. Reducing sugars by the Luff-Schoorl
method 71 - 1963
c. Colour of white sugars . . . . 71 - 1963
d. Sulphur dioxide 72 - 1963
e. Moisture 72 - 1963
f. Sulphated ash 7 2- 1963
g. Conductometric ash (for mill white and
refined sugars) . . . . 72 - 1963
h. Grain size distribution . . . . 73 - 1962
TABLES
I Table adjusting the B.H.P. coefficient "f" according
to the purity of mixed juice .. .. .. . . Chapter III, 43
II Temperature corrections to readings of brix hydro-
meters (20C) IV, 2, g, v
III Schmitz's table for a normal weight of 26.000 g . . VII, 4, a
IV Table giving mg invert sugar required to reduce 10
and 25 ml of Fehling's solution in the presence of
different amounts of sucrose . . . . . . . . VII, 6, a, ii
Va Table giving the divisor, corrected for the brix of the
solution, of the formula to be used in the Jackson and
Gillis method IV VIII, 5, c, iii
Vb Temperature corrections for the divisors for the
Jackson and Gillis method for acid inversion . . VIII, 5, c, iii
VI Table to be used for the calculation of the result of the
Luff-Schoorl determination of reducing sugars . . VIII, 11, b
VII Recommended scheme of analysis of various factory
products . . . . . . . . . . . . . . VIII
FI G URES
1 Counterpoise weight . . . . . . . . . . Chapter IV, 2, o
2 Bagasse container . . . . . . . . . . V, 3, a, v
3 First expressed juice sampler .. . . . . . . V, 4, a, ii
4 Signalling device for first expressed juice sampler . . V, 4, b
5 Mixed juice sampler . . .. .. .. .. V, 5, c
6 Brix spindle reading . . . . . . . . . . VII, 3
7 Apparatus for determination of SO
2
by Monier-
Williams method . . . . . . . . . . VII, 7, c, ii
Laboratory Manual for S. Afr. Sugar Factories 1962 IX
CHAPTER I
DEFI NI TI ONS
ABSOLUTE J UICE: A hypothetical juice, the weight of which is equal
to the weight of cane minus the weight of fibre. It comprises all
the dissolved solids in the cane plus the total water in the cane.
AP P ARENT P URITY: See under Purity.
ASH: The residue remaining after burning off all organic matter.
BAGACILLO: Very small particles of bagasse separated either from
mixed juice or from the mass of the final bagasse for filtration or
other purposes.
BAGASSE: The residue obtained from crushing the cane in one or more
mills known respectively as first mill bagasse, second mill bagasse,
etc., and when referring to the residue from the last mill, last mill
bagasse, final bagasse, or simply bagasse.
BOI LI NG HOUSE OR FABRICATION DEP ARTMENT: That part of
the factory in which the processes of manufacture from mixed juice
to weighed sugar are carried out.
BOI LI NG HOUSE PERFORMANCE: The percentage ratio of crystal-
lized sucrose actually recovered in sugar to crystallizable sucrose
in mixed juice, as found by the method of calculation described in
chapter III, 5, 41.
BOILING HOUSE RECOVERY ( RECOVERY OF SUCROSE IN MIXED
J UI CE) : The percentage ratio of sucrose (or pol) actually recovered
in sugar to total sucrose (or pol) in mixed juice.
BRIX ( DEGREES) : Unit divisions of the scale of a hydrometer, which
when placed in a pure aqueous sucrose solution at 20C, indicates
the percentage by weight of solids in the solution. The reading
obtained in an impure sucrose solution is usually accepted as an
approximation of its percentage by weight of total soluble solids.
The term Brix is used in calculations as a measure of substance
e.g., tons Brix.
Refractometer Brix: The term used when a refractometer equipped
with a scale, based on the relationship between refractive indices
at 20C and the percentage by weight of total soluble solids of a
pure aqueous sucrose solution, is used instead of a hydrometer
to test the solids concentration of a sucrose-containing solution.
Laboratory Manual for S. Af r . Sugar Factories 1962 1
BRIX- FREE WATER: The water associated with the fibre in cane and
bagasse. In some respects this sorption water behaves in a manner
somewhat similar to water of hydration. It cannot be separated
from fibre by mechanical means but is driven off at raised tempera-
tures. It is not available for dissolving sucrose. The amount of
brix-free water is approximately 30% on bone dry matter (23% on
natural fibre) and for milling control purposes is calculated as
indicated in chapter III, 5, 33.
CANE: The raw material from which sugar is recovered.
a. Extraneous matter: Consists of materials which become associated
with the cane after it has been reaped, but does not include those
comprised in the definition of 'field trash'.
b. Field trash: Consists of cane trash, tops, roots, dead sticks of cane,
mud, leafy material and other vegetable matter from the field in
which the cane was grown.
C. C. J . S .: A quantity used only for cane payment purposes and which
is calculated using the formula
Sucrose % first expressed juice from this cane
Tons of cane x
100
CLARI FI ED J UICE: The juice prepared for evaporation.
CUSH- CUSH: The material removable from mill juice by straining.
DI LUTI ON WATER: The portion of imbibition water or any other
weighed water present in mixed juice.
DRY SUBSTANCE: The material remaining after drying the product
to constant weight, or for a specified period. The weight of the
dry substance can also be found by deducting from the weight of
the product, the weight of moisture, as determined in a specified
manner.
EXTRACTION: The percentage ratio of sucrose in mixed juice to
sucrose in cane.
FACTORY: The premises on which sugar manufacturing operations
and their attendant activities are carried out.
FI BRE: The water insoluble matter of cane and bagasse from which
the approximate 23 % brix-free water (30 % on bone dry matter)
which it contains, has been removed by drying.
Where associated with brix-free water, fibre is often called
natural fibre.
In factory and milling control practice, the fibre content of
the final bagasse is calculated as indicated in chapter III, 5, 27.
FILTER CAKE: The residue removed from process by filtration
including any added filter aid.
2 1962 Laboratory Manual for S. Af r . Sugar Factories
FI LTER LIQUORS:
a. If filter presses are used
i. Filter juice: The clear filtrate from the presses. The filtrate
produced during the process of washing or sweetening off is
usually mixed with the filtrate obtained from juice and is
also termed filter juice. When fractional washing is applied,
the last runnings from one press are used for sweetening off
the next press and are ultimately mixed with filter juice.
b. If rotary vacuum filters are used
i. Cloudy filtrate: The filtrate produced during the initial stage
of the filtration process.
ii. Clear filtrate: The filtrate produced during the latter stage of
the filtration process, including the filtrate from the washing
process.
c. If the double carbonatation process is applied, the filter juices from
the first and second carbonatations are distinguished.
FI RST EXPRESSED J UICE: The juice expressed by the first two
rollers of the tandem.
GRAVI TY P URITY: See under Purity.
GRAVI TY SOLIDS: The weight of solids calculated from the brix
spindle determination.
IMBIBITION: The process in which water or juice is put on the bagasse
to mix with and dilute the juice present in the latter. The water
so used is termed imbibition water. General terms in use are:
a. Single imbibition,
b. double imbibition,
c. compound imbibition,
depending on the manner in which the water and/or juice is added.
INVERT SUGAR: A mixture of approximately fifty % glucose
(dextrose) and fifty % fructose (laevulose) obtained by the hydrolysis
of sucrose.
J AVA RATIO: The percentage ratio of sucrose (or pol) % cane to
sucrose (or pol) % first expressed juice. For distribution purposes,
the Java ratio is calculated as indicated in chapter III, 5, 36.
J ELLY ( STRI NGP ROOF) : A boiling which has been concentrated
without graining to such a consistency that it may be expected to
crystallize spontaneously on standing.
LAST EXPRESSED J UICE: The juice expressed by the last two rollers
of the tandem.
LAST MILL J UICE: The juice expressed by the last mill of the tandem.
MAGMA: A mixture of crystals and sugar liquor produced by mechani-
cal means.
M ASSECUI TE: The mixture of crystals and mother liquor discharged
from a vacuum pan. Massecuites are classified in order of descending
purity as first, second, etc., or A, B, etc., and jelly massecuite.
M I L L SETTI NGS:
a. Set opening: The set opening of a mill is the distance between the
circumferences escribed by the mean diameters of the top roller and
feed or discharge roller with the mill running empty.
The mean diameter of a grooved roller is equal to the diameter of the equiv-
alent (same volume and length) solid roller.
b. Work opening: The work opening is equal to the set opening plus
the increase in distance between the rollers resulting from the lift
during milling operations.
M I X ED J UI CE: The mixture of juices from the mills delivered via
ancillary mechanical equipment into the juice scales.
M OLASSES: The mother liquor separated from the massecuite by
mechanical means. It is distinguished by the same prefixes as the
massecuites from which it is separated.
Final molasses: The mother liquor separated from the final
massecuite by mechanical means. Final molasses is usually
discharged from the factory as such.
M UD S : The material removed from the bottom part of the subsiders.
The muds (or mud) contain most of the settled suspended solids.
NON- SUCROSE: Strictly, dry substance minus sucrose, often brix
minus sucrose.
NON- SUGAR: Brix minus pol.
NORM AL W EI GHT:
a. That weight of pure dry sucrose which, when dissolved in water
to a total volume of 100 ml at 20C and read at the same temperature
in a tube 200 mm long, gives a reading of 100 degrees on a sac-
charimeter scale. If the International Sugar Scale is used, the
normal weight of sucrose is 26.000 grams; if the Ventzke scale is
used, the normal weight is 26.026 grams, corresponding to a
reading of 100V.
b. The weight of sample equal to the normal weight of sucrose.
NUTS CH SAMP LE: A nutsch sample is any sample of molasses which
is separated from a massecuite at any time prior to curing the
massecuite in the factory centrifugals.
OV ERALL RECOV ERY : The percentage ratio of sucrose (or pol),
actually recovered in sugar to total sucrose (or pol) in cane.
P OL: The apparent sucrose content of any substance expressed as
a percentage by weight, and determined by the single or direct
polarization method. The term is used as if it were a real substance.
P OL- ASH RATI O: The ratio of pol to ash.
P OL EXTRACTION: The percentage ratio of the weight of pol in
mixed juice to the weight of pol in the corresponding weight of
cane.
P RIMARY J UICE: All the juice expressed before dilution begins.
P URI TY: The percentage ratio of sucrose (or pol) to the total soluble
solids (or brix) in a sugar product. The following terms are in
general use:
a. Apparent purity: The percentage ratio of pol to brix.
b. Gravity purity: The percentage ratio of sucrose to brix.
c. True purity: The percentage ratio of sucrose to total solids
determined by drying.
RECOVERY ON MIXED J UICE: See Boiling House Recovery.
REDUCI NG SUGARS: The reducing substances in cane and its
products determined as described in chapter VII and calculated as
invert sugar.
Note: The common practice of referring to reducing sugars as glucose is to
be discouraged.
REDUCI NG SUGAR ASH RATIO: The ratio of reducing sugars to
ash.
REDUCI NG SUGAR SUCROSE RATIO: The percentage ratio of
reducing sugars to sucrose or pol.
RESIDUAL J UICE: The juice left in intermediate or final bagasse.
SACCHARIMETER READING: Actual reading on the scale of a
saccharimeter.
SAFETY FACTOR: A number designed to indicate the probable
keeping quality of a fresh raw sugar. It is calculated by dividing
the percentage moisture in the sugar by one hundred minus the pol
of the sugar.
SECONDARY J UICE: The dilute juice which together with the primary
juice forms the mixed juice.
SUCROSE: The pure disaccharide, C
12
H
22
0
11
, also known as saccharose
or cane sugar.
SUGAR: The main product of a sugar factory consisting of crystals
of sucrose as removed from a massecuite and containing a smaller
or larger portion of natural impurities, depending on the type of
sugar.
SULP HATED ASH: The residue remaining after burning off all organic
matter in a sample, sulphuric acid being used as described in chapter
VII, 13.
Laboratory Manual for S. Afr. Sugar Factories 1962 5
UND I LUTED J UI CE: A hypothetical juice, whose weight is equal to
the weight of cane minus the combined weights of fibre and brix-
free water. For milling control purposes, the weight of undiluted
juice is calculated as indicated in chapter III, 5, 12.
W AS H: The diluted molasses thrown off by the centrifugals during
washing and/or steaming, and collected separately.
6 1962
Laboratory Manual for S. Afr. Sugar Factories
C H AP TE R I I
TH E D E TE RMI NATI ON OF F AC TORY
WE I G HTS
1. Gener al
All weighings shall be subject to the Weights and Measures Act and
Regulations and further to the rulings given by the Superintendent of
Assize or the Assizer concerned. The weighing of cane, imbibition water
and mixed juice shall be subject to the provisions of any Agreement
published in terms of the Sugar Act 1936, or any amendment thereof, or
any provisions as may be agreed upon by the South African Sugar
Association, and where necessary approved by the Assize Department.
2. Cane
a. The weighbridge, tares
i. The weighbridge shall be situated as near as possible to the
off-loading site in order to minimize any loss or gain in weight
after the cane has been weighed.
ii. Sequence numbered scale tickets, upon which the gross weight
of the vehicle shall be recorded by means of the stamping
device attached to the weighbridge, shall be used on all
weighbridges of the beam type.
iii. Special attention is drawn to regulation 53 (g) of the Weights
and Measures Act, which reads:
"Where any self-indicating weighing instrument approved in terms
of section twenty-three (1) of the Act after 1st September, 1957, is furnished
with a weight-recording or printing device, means must be provided to
prevent any recording or printing being effected while the pointer is
moving."
iv. The introduction of automatic self-recording weighbridges for
the weighing of cane, together with some automatic device to
ensure that the vehicle to be weighed is correctly placed on
the weighbridge platform, is strongly recommended.
v. The weight of the cane shall be obtained by subtracting the
gross tare from the gross weight of the vehicle and its contents.
vi. Gross tare means the weight of the vehicle (nett tare) plus
the weight of all loading poles or chains and all extraneous
matter, but not the weight of matter originally adhering to
the cane in the normal practice of harvesting, which means
that no deductions shall be made as tare for trash, tops,
roots, soil or mud.
b. S.A.R. trucks
i. S.A.R. trucks should be weighed uncoupled and separately,
especially where there exists any possibility of a downward or
upward thrust being created by the trucks preceding or
following the truck to be weighed. There should be at least
50 feet of straight level track on either side of the weighbridge.
If circumstances preclude the possibility of weighing S.A.R.
trucks uncoupled, then every precaution shall be taken to
ensure that the truck being weighed is free from interference
by the S.A.R. trucks preceding and following it.
ii. The nett tare weights which are stencilled on the side of the
S.A.R. trucks have been found, in certain cases, to be seriously
in error. The miller may re-tare each and every truck. Any
coal, lime, rocks or any other extraneous matter which may
be found at the bottom of the truck, shall be included in the
gross tare.
iii. Where unloaded S.A.R. trucks are not re-tared in the mill
yard, the nett tare, as stencilled on the side of the truck by
the Railway Administration, shall be accepted and no addition
shall be made thereto for the weight of any extraneous matter
remaining in the truck unless such weight has been determined
separately.
Caution: Portuguese rolling stock is marked with tares in kilograms
with or without the equivalent in pounds.
c. Tram trucks
i. Tram trucks should be weighed uncoupled and separately,
but where this is not possible every precaution shall be taken
to ensure that the tram truck being weighed is free from
interference from the tram trucks preceding or following it.
There should be at least 50 feet of straight level track on either
side of the weighbridge.
ii. The gross tare, which shall be distinctly marked on the side
of each truck, shall include the weight of the loading chains
attached to the truck; such gross tare weight shall be deter-
mined at the beginning of each season and as often as may be
deemed necessary due to repairs and other causes, to the
satisfaction of the miller and the supplier of the cane.
d. Wagons, lorries and trailers
i. The vehicles shall be weighed after unloading as often as is
agreed upon by the miller and the grower, but at least once
daily. The weight shall include side poles and chains used to
transport the cane from the field to the factory. This con-
stitutes the gross tare of the vehicle.
ii. Where cane is weighed in trailers which are too long to be
accommodated on the weighbridge platform, the following
procedure to determine the weight of cane shall be adopted:
The mechanical horse and trailer shall be weighed
coupled by first placing the horse dead centre on the weigh-
bridge platform (note weight recorded), then the load is drawn
across the scale platform until the trailer wheels reach dead
centre of the weighbridge platform (note weight recorded).
The sum of the two weights represents the total gross weight
of the consignment. Tare weights of the horse and trailer
are determined in the same way as described above, while
the nett weight of the consignment is the difference between
the two sets of weights so determined.
e. Chains
i. The tare for loading chains shall be included in the gross
weight of the vehicle and shall be determined either by taking
the average weight of a number of typical chains, or by sub-
stituting a similar number of chains for loading purposes
upon the empty vehicle to be re-weighed.
ii. Where cane is weighed in slings the bundle with sling attached
shall be completely disconnected from the crane. The weight
of the sling constitutes the tare weight and shall be determined
as under i above.
f. Loading poles
i. Loading poles should be approximately 8 ft 6 in. long and
3 in. butt end diameter. The weight of each pole should be
not less than 15 lb. nor greater than 30 lb.
ii. The average weight per pole shall be used in conj unction with
the total number of poles used per truck to determine the
tare for poles in each truck.
The average weight per pole shall be determined by
mutual agreement between the miller and the supplier of the
cane.
3. Imbibition water
The weight shall be determined by weighing. Any water that is used for
wash-down purposes which enters the mixed juice shall be determined
by weighing and included in the weight of imbibition water.
The provisions under 4, Mixed juice, below, concerning the operation
and checking of the scales ( non-automatic and automatic) shall also apply
to the weighing of imbibition water.
4. Mixed juice
a. General
The weight shall be determined by weighing.
b. Non-automatic scales
i. The nett weight of each tip shall be found by subtracting from
the weight of the full scale tank the weight of the emptied tank,
as determined after each weighing of a full tank.
ii. Sequence numbered tickets stamped with indelible numbers
shall be used for each scale tank weighed.
iii. An automatic device which records the filling or emptying
of each scale tank (such as the Bristol Recorder) shall be
fitted to each scale tank.
iv. An automatic counter for recording the number of loads
shall be fitted to each scale.
Automatic scales
i. Items iii and iv of paragraph 4, b, shall also apply to automatic
scales, but where the frequency of tips precludes the use of
the devices mentioned under 4, b, iii, then three automatic
counters shall be used on each scale for recording the number
of scale tanks weighed.
ii. Automatic weighing machines of the constant-load type
shall be adjusted by the District Assizer or by a person
authorized by him to perform such adjustment, and the weight
of any load of juice delivered by an adjusted weighing machine
shall be assumed to be equal to the capacity for which the
machine has been adjusted.
iii. Nevertheless it is strongly recommended that daily verification
be obtained of the accuracy of the assized weight of a load
in order to detect any deviations in the functioning of the
weighing machine. For this purpose ten consecutive loads of
juice, obtained under normal operating conditions, shall be
re-weighed over another assized or re-assized weighing
instrument.
iv. The arithmetical mean of the ten check weights shall be
determined, and if this mean weight differs by more than
0.5% either in excess or deficiency from the assized capacity,
the weighing machine shall be re-adjusted.
v. Automatic weighing machines of the variable-load type shall
be adjusted by the District Assizer or by a person authorized
by him to perform such adjustment.
vi. Nevertheless it is strongly recommended that daily verification
be obtained concerning the accuracy of the weight as indicated
by the recording mechanism of the weighing machine, using
the appropriate check weight.
vii. Re-weighing ten consecutive loads of juice as described in
4, c, iii and 4, c, iv above, provides an even better means of
verifying weighing machines of the variable-load type, where
a sufficiently accurate and sensitive secondary weighing
machine is available.
1962 Laboratory Manual for S. Af r . Sugar Factories
5. Bagasse
By inference, assuming the fundamental equation to be exact: weight of
cane + weight of imbibition water = weight of mixed j uice + weight of
bagasse.
Weight of bagasse is therefore: weight of cane plus weight of
imbibition water minus weight of mixed j uice.
6. Final molasses
By weighing.
7. Filter cake
Whether obtained from plate and frame or vacuum type filters, the
weight of the filter cake shall be determined by continuous or periodic
weighing of the contents of trucks into which the filter cake is discharged.
8. Sugar
By weighing on scales and in such manner as is approved by the
Government Assize Department. Where sugar is weighed in bags,
provision shall be made previously for the weight of the bags.
9. Burnt lime, Sulphur and Phosphoric acid
By weighing.
Laboratory Manual for S. Af r . Sugar Factori es 1962 11
C H AP TE R I I I
C ALC ULATI O NS
1. General
Control data are required for the purpose of factory control and as a
basis for cane payment. The former are recorded in daily, weekly,
monthly and annual reports.
Control data are usually calculated from quantities obtained by
direct weighing (infrequently by direct measuring) in conjunction with
figures obtained by direct analysis.
Quantities obtained by direct weighing are: tons* of cane, tons of
imbibition water, tons of mixed juice, tons of filter cake, tons of final
molasses and tons of sugar. The methods of weighing are described in
chapter II.
2. Calculation of quantities in st ock
For the purpose of correctly ascertaining sucrose, pol, brix, non-sucrose
and other balances, and certain efficiency data, account must be taken
of the materials currently being processed.
The estimation of the quantities in process is called stocktaking.
In stocktaking a list should be made of the estimated quantities of the
various products and their percentages of sucrose and brix. From these
data the total weights of sucrose and brix in stock and the average
purity of the products in stock are calculated. From the purity figures,
the fraction of sucrose in stock which shall be recovered as sugar is cal-
culated using the S.J.M. formula:
* Wherever the term tons is used it means tons of 2,000 lb. each.
12 1962 Laboratory Manual for S. Afr. Sugar Factories
where x = recovery of sucrose % sucrose in the primary
product
S = expected purity of the sugar to be produced
J = purity of the primary product
M = expected purity of the final molasses to be pro-
duced which in Natal is taken as equal to the
average purity of the final molasses produced
in the preceding week.
x = 100 x
S ( JM)
J (SM)
The use of the formula is illustrated by calculation of the percentage of
sucrose which should be recovered from the total stock in process at the end
of the week.
Let total tons brix in stock = 2000
and sucrose in stock = 1500
then average purity of stock =
If the expected purity of sugar to be produced = 99
and if the purity of final molasses for the preceding week = 39.7
then from S.J.M. formula
x = 100 x = 78.6
i.e. 78.6% of the sucrose in stock should be recovered in sugar while the
balance (21.4%) should be retained in the final molasses.
Subsequent calculations yield:
a. tons of sucrose in stock expected to go into sugar
b. tons of sucrose in stock expected to go into final molasses.
The former quantity should be added to tons of sucrose in sugar made
yielding tons of sucrose in sugar made and estimated. The latter quantity
should be added to tons of sucrose in final molasses made yielding tons
of sucrose in final molasses made and estimated.
From tons of sucrose in sugar made and estimated, tons of sugar
made and estimated can be computed. From tons of sucrose in final
molasses made and estimated, tons of final molasses made and estimated
can be computed.
As well as making a sucrose balance, other balances, e.g. brix and
non-sucrose balances, may be made using the above-mentioned data.
3. Recording of decimal fractions
A note of caution is given to chemists that decimal fractions should be
used with discretion. If random errors alone were considered, then the
average of a large number of analyses could be carried to more places
of decimals than the result of a single test; but there are constant errors
such as errors in apparatus which cannot be reduced in this way. Con-
sideration of all types of errors shows that the average of a series of pol
or sucrose percentages in sugars or juices should not be reported to more
than the second decimal place. The reading of a brix spindle should be
recorded to the nearest 0.05 brix and the temperature correction to
the nearest second decimal place. The second place of the resultant
figure should be discarded and the brix of all products should be recorded
to the nearest first decimal place. The calculated average, however,
should be recorded to the nearest second place. To record decimal
places in the case of the weight of filter cake, which is not continuously
and carefully weighed, is wrong and misleading. Alternatively, if sugar
or cane is weighed precisely to the third or fourth decimal of a ton,
then the third or fourth decimal must always be recorded even when
the figure is 0.
x 100 = 75.
In the fundamental equation:
weight of cane + weight of imbibition water = weight of mixed j uice
+ weight of bagasse,
the weight of cane, imbibition water, mixed juice and bagasse are all
reported to the third decimal place in tons. Where the weight of the cane
is recorded to the nearest pound, this weight should be reported to the
nearest 0.0005 tons, in which case the fundamental equation should be
carried to the fourth decimal place. (Note: While the weight of bagasse
cannot be assumed to be accurate, the third decimal place should neverthe-
less be recorded, in order to make the fundamental equation balance.)
The corresponding weights of sucrose in mixed juice and bagasse should
be recorded to the third decimal place in tons, and their sum, which
is the weight of sucrose in cane, to the third decimal place.
4. Rul es for roundi ng off
Wherever a decimal place to be discarded is represented by a number less
than five, the preceding digit (that is the last to be recorded) shall remain
as it stands; but where the number to be discarded is greater than five,
one shall be added to the preceding digit. Where the number to be
discarded is exactly five, the preceding digit shall be unaltered if it is
an even number, but if it is an odd number one shall be added to it.
5. Standardization of met hods of cal cul ati on
The calculations in this section are given with a view to standardization
of methods. The formulae do not include all the calculations which the
chemist may be required to make in his capacity as statistician. Others
will be found in subsequent chapters of this manual.
In the following formulae, numbers in square brackets [ ] refer to
the number of decimal places to which calculations should be made,
numbers in round brackets ( ) refer to the calculations hereunder.
The letter w signifies a quantity obtained by direct weighing or direct
measurement and x denotes a value obtained by direct analysis.
a. Weights
1 . TONS OF B RI X IN CANE [3]
Tons of brix in mixed juice (9) + tons of brix in bagasse (5).
2. TONS OF SUCROSE IN CANE [3]
Tons of sucrose in mixed juice (10) + tons of sucrose in bagasse (6).
3 . TONS OF FI B RE IN CANE [3]
Is equal to tons of fibre in bagasse (7).
4. TONS OF B AGASSE [3]
Tons of cane w + tons of imbibition water w tons of mixed juice w.
5 . TONS OF B RI X IN B AGASSE [3]
Tons of bagasse (4) x brix % bagasse (26)
100
6 . TONS OF SUCROSE IN B AGASSE [3]
Tons of bagasse {4) x sucrose (pol) % bagasse x
l00
7 . TONS OF FI B RE IN B AGASSE [3]
Tons of bagasse {4) x fibre % bagasse {27)
100
8 . TONS OF MOI STURE IN B AGASSE [3]
Tons of bagasse (4) x moisture % bagasse x
100
9 . TONS OF B RI X IN MI X ED J UI CE [3]
Tons of mixed juice w x brix % mixed juice x
100
10. TONS OF SUCROSE IN MI X ED J UI CE [3]
Tons of mixed juice w x sucrose % mixed juice x
100
11. TONS OF AB SOLUTE J UI CE [3]
Tons of cane w tons of fibre in cane (3).
12. TONS OF UND I LUTED J UI CE [3]
Tons of brix in cane (1) X 100
Brix % first expressed juice x
13. TONS OF SUCROSE IN FI LTER CAK E [3]
Tons of filter cake w x sucrose (pol) % filter cake x
Too
*14. TONS OF SUCROSE IN SUGAR [3]
Tons of sugar w x sucrose (pol) % sugar x
100
* These are general formulae; if quantities in stock are to be taken into account
the procedure mentioned under 2 above should be followed.
Laboratory Manual for S. Af r . Sugar Factories
1962 15
*15. TONS OF MOI STURE IN SUGAR [3]
*16. TONS OF B RI X ( SOLI D S) I N SUGAR [3]
Tons of sugar w tons of moisture in sugar (15).
*17. TONS OF SUCROSE IN FI NAL MOLASSES [3]
Tons of final molasses w x sucrose % final molasses x
100
*18. TONS OF B RI X IN FI NAL MOLASSES [3]
Tons of final molasses w x brix % final molasses x
l00
*19. TONS OF UND ETERM I NED LOSS OF SUCROSE [3]
Tons of sucrose in mixed juice (10) tons of sucrose in filter cake (13)
tons of sucrose in final molasses (17) tons of sucrose in sugar (14).
b. Percentages and ratios
20. SUCROSE % CANE [2]
Tons of sucrose in cane (2) X 100
Tons of cane w
21. SUCROSE % CANE ( AP P ROXI MATE CALCULATI ON) [1]
sucrose (pol) % first expressed juice x x an assumed Java ratio
100
22. FI B RE % CANE [2]
Tons of fibre in bagasse (7) X 100
Tons of cane w
23. B AGASSE % CANE [2]
Tons of bagasse (4) X 100
Tons of cane w
24. I M B I B I TI ON % CANE [1]
Tons of imbibition water w X 100
Tons of cane w
25. I M B I B I T I O N % F I B RE [0]
Tons of imbibition water w X 100
Tons of fibre in cane (3)
26. B RI X ( SOLUB LE SOLI D S) % B AGASSE [2]
Sucrose (pol) % bagasse x X 100
Purity of last expressed juice x
27. FI B RE % B AGASSE [2]
Dry substance % bagasse x brix % bagasse (26).
28. B RI X % AB SOLUTE J UI CE [2]
Tons of brix in cane (1) X 100
Tons of absolute juice (11)
29. D I LUTI ON % AB SOLUTE J UI CE EX TRACTED [2]
Brix % absolute juice (28) brix % mixed juice x X 100
Brix % mixed juice x
30. AB SOLUTE J UI CE LOST IN B AGASSE % FI B RE [0]
Brix % bagasse (26)
Brix % absolute juice (28) x fibre % bagasse (27)
31. RED UCI NG SUGAR/ SUCROSE RATIO [2]
Reducing sugar % product x
X 100
Sucrose (pol) % product x
32. RED UCI NG SUGAR/ ASH RATIO [2]
Reducing sugar % product x
Sulphated ash % product x
c. Miscellaneous formulae
33. B RI X- FREE WATER % FIBRE [0]
Tons of absolute juice (11) tons of undiluted juice (12) X 100
Tons of fibre in bagasse (7)
X 10,000
34. POUNDS OF FIBRE PER CUBIC FOOT ESCRIBED VOLUME [0]
Calculated weekly for the discharge opening of each mill unit.
The escribed volume is equal to n n D L K cu. ft
where n = the total number of revolutions of the top roller for the week
D = the corrected mean diameter of the top roller, in ft
L = the length of the top roller, in ft
K = the average work opening, in ft.
K is found from the set opening and the average lift of the top roller
using the formula: K = S + 0.8H where S is the set-opening in ft and
H is the average lift of the top roller in ft (generally 3 0% of the total
possible lift).
Pounds of fibre equals tons of fibre for the week x 2,000.
Hence Pounds fibre per cu. ft escribed volume
37. EXTRACTI ON [2]
Tons of sucrose in mixed juice (10)
Tons of sucrose in cane (2)
x 100
40. EX P ECTED P URI TY OF FI NAL MOLASSES ( D OUWES D EK K ER
F O R M U L A )
Expected (true) purity = 35.886 0.08088 R + 0.26047 A
where R = reducing sugars % non-sucrose
A = ash % non-sucrose.
41. BOILING HOUSE PERFORMANCE [2]
Laboratory Manual for S. Af r. Sugar Factories
in which sum of tons C.C.J.S. is equal to the sum of the quantities
x 100
1962 17
Tons of sucrose in sugar (14)
Tons of sucrose in mixed juice (10)
x 100
39. O V E R A L L RECOVERY [2]
Pounds of fibre for the week
Escribed volume for the week
35. J AVA RATIO [2]
Sucrose % cane (20)
Pol % first expressed juice x
x 100
36. J AVA RATIO FOR DISTRIBUTION PURPOSES [4]
Tons of sucrose in cane for a certain period
Sum of tons C.C.J.S.
x 100
Tons of cane x
Sucrose % first expressed juice from this cane
100
for each consignment.
x 100
38. BOILING HOUSE RECOVERY [2]
4 2 . C R Y S T A L L I Z A B L E S UC R OS E [3]
Crystallizable sucrose is calculated using the S.J.M. formula in the form
Percentage crystallizable sucrose = S
where S is the percentage sucrose in the product
B is the percentage brix in the product
P is the purity of final molasses (either the expected or actual
purity may be employed).
Note: Under particular conditions
e.g. when P = 28.57 this formula is known as the Winter formula
or when P = 30.0 Carp formula.
4 3 . B . H . P . COEFFI CI ENT ( f)
The B.H.P. coefficient which is equal to the term in the
formula for calculating percentage crystallizable sucrose in a product
is dependent on the purity of the mixed juice. The values reported in
Table I have been adjusted to Natal conditions.
6. Sugar Milling Research Institute monthly period calculation sheet
The calculation sheet used by the Sugar Milling Research Institute for
the " to date" and "period" figures for Boiling house performance and
Lost absolute juice together with Purity of last expressed juice, Brix-free
water and Imbibition efficiency which are used as checks on the accuracy
of some of the factory data, follows. A typical worked example is included.
Boiling House Performance Calculation
1. Tons Brix in mixed juice (To Date) 99888.308
2. Tons Sucrose in mixed juice (To Date) 85241.711
3. Tons Non-Sucrose in mixed juice (To Date) 14646.597
4. f (to three decimal places, according to purity
of M.J.) 0.492
(-)
( x )
_5. Tons Non-Crystallizable Sucrose in mixed juice (To Date) 7206.126
100.00
44. C R U S H I N G T I M E ANAL Y S I S
a. Hours available for crushing [1]
is a minimum weekly time of 144 hours.
b. Overall efficiency [2]
Hours of actual crushing [1]
Hours available for crushing (44, x)
c. Hours of stoppage percentage [2]
Hours ot stoppage LI J
Hours available for crushing (44, x)
It should be recorded as follows:
i. H.S.P. due to mechanical failures in the
mills
ii. H.S.P. due to mechanical failures in the
boiling house
iii. H.S.P. due to other causes inside the
factory (jams, etc.)
iv. H.S.P. due to shortage of cane
v. H.S.P. due to other causes outside the
factory
Overall efficiency
85241.711
7206.126
78035.585
75720.955
75012.993
707.962
90.84
37.60
53.24
70.62
75012.993
499.963
74513.030
95.49%
To-Date
651078.770
102672.132
548406.638
242432.185
130066.889
112365.296
102672.132
9693.164
99888.308
109581.472
548406.638
19.98
9693.164
19.98
48514.334
102672.132
47.25
74513.030
62349.459
12163.571
78035.585
65336.107
12699.478
95.78%
Period
106151.520
17326.585
88824.935
41805.640
22882.386
18923.254
17326.585
1596.669
16267.461
17864.130
88824.935
20.11
1596.669
20.11
7939.677
17326.585
45.82
Lost Absolute Juice Calculation
Tons of Cane crushed
Tons of Fibre in Cane
Tons of Absolute Juice
Tons of Bagasse
Tons of Moisture in Bagasse
Tons of Dry Matter in Bagasse
Tons of Fibre in Bagasse
Tons of Brix in Bagasse
Tons of Brix in Mixed Juice
Tons of Brix in Cane
( x 1OO)
Brix % Absolute Juice
Brix % Absolute Juice
( x 1OO)
Tons of Absolute Juice in Bagasse
Tons of Fibre in Bagasse
( x 1OO)
LOST ABSOLUTE JUICE % FIBRE
2. Tons Sucrose in mixed juice (To Date)
5. Tons Non-Crystallizable Sucrose in mixed juice (To Date)
6. Tons Crystallizable Sucrose in mixed juice . . (To Date)
7. Tons Solids in Sugar made and estimated . . (To Date)
8. Tons Sucrose in Sugar made and estimated . . (To Date)
9. Tons Non-Sucrose in Sugar made and estimated (To Date)
10. Brix % final molasses (To Date)
11.. Sucrose % final molasses (To Date)
12. Non-Sucrose % final molasses (To Date)
13. Sucrose % Non-Sucrose in final molasses
100x11/12 (To Date)
8. Tons Sucrose in Sugar made and estimated . . (To Date)
14. Tons Non-Crystallizable Sucrose in sugar made
and estimated 9 x 13/100 (To Date)
15. Tons Crystallizable Sucrose in Sugar made and
estimated (To Date)
16. BOILING HOUSE PERFORMANCE 10 0 X 15 / 6 . . (To Date)
15.. Tons Crystallizable Sucrose in Sugar made and
estimated (To Date)
17. Ditto to-date quantity of the previous report . .
18. Tons Crystallizable Sucrose in sugar made and
estimated (Period)
6. Tons Crystallizable Sucrose in mixed juice . . (To Date)
19. Ditto to-date quantity of the previous report . .
20. Tons Crystallizable Sucrose in mixed juice . . (Period)
21. BOILING HOUSE PERFORMANCE 10 0 X 18 / 20 . . (Period)
Purity of Last Expressed Juice Calculation
Tons of Sucrose in Bagasse
( x 1OO)
Weighted Mean of
PURITY OF LAST EXPRESSED JUICE
Brix-free Water % Fibre Calculation
Tons of Brix in Cane
Brix % First Expressed Juice
(x 1OO)
Tons of Undiluted Juice
Tons of Undiluted Juice
Tons of Brix-Free Water
Tons of Fibre
(x 100)
BRIX-FREE WATER % FIBRE
Imbibition Efficiency Calculation
Tons of Fibre
Tons of Bagasse
(x 1OO)
Fibre % Bagasse
Brix of Last Expressed Juice
Purity of Last Expressed Juice
(x 100)
Sucrose % Last Expressed Juice
Fibre % Bagasse
(100 Fibre % Bagasse)
Sucrose % Last Expressed Juice
(x 100)
Sucrose % Bagasse (Calculated)
Sucrose % Bagasse (Analysis)
(x 100)
IMBIBITION EFFICIENCY
Period
1230.614
1596.669
77.07
To-Date
7267.915
9693.164
74.98
Period
17864.130
21.32
83790.478
To-Date
109581.472
21.00
521816.533
88824.935
83790.478
5034.457
17326.585
29.06
548406.638
521816.533
26590.105
102672.132
25.90
Period
17326.585
41805.640
41.45
To- Date
102672.132
252432.185
40.67
4.26
77.07
3.28
3.41
74.98
2.56
100.00
41.45
58.55
3.28
1.92
2.94
65.31%
100.00
40.67
59.33
2.56
1.52
2.88
52.78%
7. Sucrose bal ances
The sucrose balance offers a convenient means of detailing losses of
sucrose in process of manufacture. The use of two such balances is
recommended:
a. balance as sucrose % sucrose in cane
b. balance as sucrose % sucrose in mixed juice.
These balances should be drawn up as follows:
Product
Final Bagasse
Filter Cake
Final Molasses
made and
estimated
Sugar made and
estimated
Undetermined
Mixed Juice
Cane
Weight of sucrose
in product
Sucrose Balances
Sucrose %
sucrose in
cane
100.00
Sucrose % sucrose
in mixed juice
100.00
C H AP TE R I V
DE S CRI P TI ON AND USE OF S TAND ARD
E Q U I PME NT
1. General
a. Standardized equipment shall be used for the determination of
sucrose in cane.
b. All volumetric glassware, brix hydrometers and saccharimeter tubes
shall be standardized at 20C. This apparatus, together with the
thermometer used in the estimation of sucrose by the Jackson and
Gillis method or by the direct polarization method, must have been
tested by the Sugar Milling Research Institute and provided with
a Certificate of Accuracy.
2. I nst r ument s
a. Saccharimeters: It is recommended that saccharimeters be equipped,
wherever possible, with the International Sugar Scale (S), corres-
ponding to a normal weight of 26.000 grams.
For saccharimeters still equipped with the Ventzke scale (V) a
normal weight of 26.026 grams shall be used.
All saccharimeters must be marked with either a large S or a
V indicating whether an International Sugar Scale or a Ventzke
Scale is fitted.
b. Light filters: When saccharimeters are provided with light filters in
the form of dichromate cells, these cells shall be filled with a solution
containing 9/L grams of potassium dichromate per 100 ml, where L
is the length of the cell in centimetres.
c. Illumination: The source of illumination shall be fixed relative to
the saccharimeter and therefore saccharimeters which have the
lamp attached by a metal arm to the instrument are recommended.
For the same reason, screw-type and not bayonet-type globe fittings
are approved.
d. Saccharimeter tubes and cover glasses
i. Tubes of three different lengths are required, 100 mm, 200 mm
and 400 mm. Tubes with a side opening are recommended
as most suitable for all types of routine analyses. If solutions
in tubes with side openings are not to be read immediately,
closure of the opening should be effected to prevent
evaporation.
ii. Saccharimeter tubes and cover glasses shall satisfy the require-
ments given in Polarimetry, Saccharimetry and the Sugars
(N.B.S., U.S. Department of Commerce, Circular C440),
Washington, United States Government Printing Office,
pages 102-106. They shall be covered by a certificate of
accuracy issued by the Sugar Milling Research Institute.
e. Quartz plates: Every factory shall have at least two quartz plates.
The value of one shall be near 100S and the value of the other
between 10S and 15S. Quartz plates shall be procured from
a reputable firm and their value shall be checked once a year by
the Sugar Milling Research Institute. When warranted, a certificate
of accuracy shall be provided after checking.
f. Thermometers for the Clerget analysis
i . THE 0 - 10 0 OR 110 C THERMOMETER
This thermometer shall be graduated in single degrees
(tolerance 0.5C) and shall not exceed 10 mm in diameter
so as to ensure the unimpeded flow of the hydrochloric acid
which is added to the solution at 65C. Its length shall be
such that the 65C mark is visible above the top of the
inversion flask.
ii. THE " I NV E RS I ON" TY P E THERMOMETER
This thermometer should have a range from 10C to 35C
and shall be graduated in l/10th degrees (tolerance 0.2C).
Thermometers of this type are used for measuring the
temperatures of the solutions to be polarized in the inversion
method of analysis.
All thermometers selected for the Clerget inversion
analysis shall be kept and used only for that purpose.
g. Brix hydrometers
i. The graduation of the brix hydrometers shall be based on
Plato's table giving the relationship between the concentration
of pure sucrose solutions and the density at 20
0
/4
0
C.
ii. A set of six hydrometers covering the following ranges is
recommended:
No. 0 from 0bx to 5 bx; graduation interval 0.05bx
No. 1 from 2bx to 13.5bx; graduation interval optional but
not greater than 0.1 bx
No. 2 from 13bx to 21 bx; graduation interval optional but
No. 3 from 19bx to 27 bx; graduation interval optional but
Laboratory Manual for S. Af r. Sugar Factories 1962 23
No. 4 from 26bx to 48 bx; graduation interval 0.1 bx
No. 5 from 46bx to 68 bx; graduation interval 0.1 bx
iii. The length of the brix scale shall be approximately:
No. 0 220 mm; No. 2 250 mm; No. 4 320 mm;
No. 1 270 mm; No. 3 250 mm; No. 5 320 mm.
iv. The stems of the instruments shall be flattened at two opposite
sides, the graduation being printed on both sides of the paper
scale. The ratio between the axes of the elliptical section of the
stem shall be approximately 2: 1. The distance between the
top of the instrument and the highest graduation mark shall
be 20-60 mm, between the lowest graduation mark and the
top conical part of the bulb 10-30 mm.
v. The thermometer shall be located within the bulb of the
instrument. The thermometer scale shall cover the range
from 10C-35C. The scale on the left of the capillary shall
be graduated in C (graduation interval 0.5C, tolerance
1C) while the scale on the right shall indicate the brix
corrections. If desired the positive corrections may be in
black and the negative corrections in red. The corrections are
given in Table II.
vi. The instruments shall be made of a boro silicate glass. The
error of the instruments at any point on the scale shall be less
than 0.1 bx and the difference between any two readings
shall be correct to within 0.1 bx.
h. Hydrometer jars: These may be of glass or metal and should be
made without a lip. Glass j ars only are recommended for mixed
juice. Hydrometer j ars attached to troughs to catch overflows are
not recommended. Jars shall be constructed so that they always
stand vertically.
Dimensions:
Overall length: 610 mm
Inside diameter: 73 mm.
j . Volumetric glassware
i. The unit of volume adopted is the litre (1) and is defined
as the volume occupied by one kilogram of pure water at its
temperature of maximum density (4C) under normal atmos-
pheric pressure. The millilitre is 1/1000th part of the litre.
ii. In general, the requirements for volumetric glassware shall
be those of the U.S. Bureau of Standards (Treadwell & Hall,
Analytical Chemistry, New York, John Wiley & Sons, Inc.,
7th edition, Vol. II, p. 448 et seq.).
k. Sugar flasks: The following types of flasks are recommended for
the analysis of sugars and sugar products:
i. 100- 110 ML DILUTION FLASK : The total height shall
be 210 mm. The 100 ml mark shall be at least 10 mm above
the top of the conical portion, and the 110 ml mark at least
60 mm below the top of the flask. The error in volume shall
not be greater than 0.2 ml at the 100 and 110 ml marks, but
the difference between the two volumes shall be correct to
within 0.1 ml.
ii. 100 ML K OHLRAUSCH FLASK FOR THE DETERMINA-
T I O N O F SUCR O SE I N J UI CE
Internal diameter of narrow part of
neck:
Internal diameter of wide part of neck:
Length of cylindrical portion of narrow
part of neck:
Overall height:
Diameter of base to be at least:
Length of tube of uniform bore above
and below graduation mark to be at
least:
Tolerance:
9 mm to 12 mm
23 mm to 27 mm
30 mm to 40 mm
150 mm to 160 mm
34 mm
5 mm
0.05 ml.
iii. 200 ML K OHLRAUSCH FLASK FOR THE DETERMINA-
T I O N O F PO L I N F I LTER CAK E
Internal diameter of narrow part of
neck:
Internal diameter of wide part of neck:
Length of cylindrical portion of narrow
part of neck:
Overall height:
Diameter of base to be at least:
Length of tube of uniform bore above
and below graduation mark to be at
least:
Tolerance:
10 mm to 14 mm
28 mm to 32 mm
35 mm to 45 mm
180 mm to 190 mm
40 mm
6 mm
0.2 ml.
iv. 100 ML P OLARIZ ATION FLASKsType 2 sugar flasks
which conform in respect of materials, workmanship and
dimensions to B.S. 675: 1953 are recommended for the
polarization of raw sugars.
1. Pipettes: For the Clerget sucrose determination the following
pipettes are recommended:
i. 50 ml certificated pipette of the standard type with one mark.
Tolerance 0.04 ml.
For the discharge of pipettes, hold in a vertical position
with the tip of the pipette touching the wall of the vessel.
Laboratory Manual for S. Afr. Sugar Factori es
When the continuous discharge has ceased, the tip is held
in contact with the side of the vessel for 15 seconds draining
time, after which the vessel is removed taking with it any drop
adhering to the outside of the pipette.
ii. 10 ml automatic pipette for addition of sodium chloride and
hydrochloric acid solutions.
m. Beaker flasks: Beaker flasks for the Clerget sucrose determination
should be made of heavy glass and have a wide neck to facilitate
cleaning. For direct polarizations similar metal or plastic beaker
flasks may be used.
n. Bagasse digestion apparatus: A brass or copper digester of
cylindrical form, 200 mm inside diameter and 254 mm high, having
a 3 mm thick machined flange 25 mm wide to form an airtight j oint
with the cover. The flange should carry four hinged bolts with
wing nuts for securing the cover. The cover should be 3 mm thick,
having in the centre a hole 38 mm in diameter, encircled with a
collar 13 mm in height and very slightly tapered to hold a rubber
stopper through which passes the lower end of an efficient reflux
condenser. Where the double lid type of condenser is used, the
collar need not be tapered and can be of convenient height to
receive the incoming cold condenser water. Between the centre and
the periphery, a hole shall be provided to take a rubber stopper
holding a thermometer, the bulb of which shall be in the vapour
space.
o. Counterpoise weights: The counterpoise or tare weights which may
be used for the weighing out of the requisite amounts of bagasse
and water for the determination of sucrose in bagasse, moisture
in bagasse, or any other weighing such as molasses, syrup, etc., shall
be constructed in brass, cylindrical in shape, in varying sizes to
suit the analysis undertaken. The top of such a counterpoise
weight shall be so constructed that it may be screwed into the main
body of the counterpoise weight, the centre of which shall be
provided with a cavity to accommodate any lead shot needed to
adjust the mass of such counterpoise weight (Figure 1).
26 1962
C H AP TE R V
S AMP LI NG
1. Gener al
a. Samples are taken in the sugar industry either from distinct quantities
of material like a tank of syrup, a lorry load of cane, a bag of
sugar, or from material which is moving past a sampling point.
Examples of the latter are the sampling of j uice from a gutter,
syrup from a continuously running sampling cock, etc. If the
distinct quantity of material to be sampled were truly homogeneous,
the composition of the sample would be identical to that of the
material and the size of the sample would be decided only by the
amount required for the actual analysis. In practice this is rarely,
if ever, the case. Hence the sample should be composited from a
large number of primary samples taken at various spots in the mass
to be sampled. The larger the number of these primary samples,
the closer the composition of the composite sample will be to the
average composition of the sampled material. If the weight of the
composite sample becomes excessive due to a very large number of
primary samples being used in compositing, the composite sample,
after thorough mixing, should be sub-sampled. To do this, various
suitable methods are available. Where moving material is being
sampled, sampling is either continuous or semi-continuous. We
speak of continuous sampling when the sample is withdrawn
uninterruptedly and of semi-continuous sampling when the samples
are taken at, usually pre-determined, time intervals. Sampling
sugar by taking a primary sample from each or every fifth bag
which is filled, is semi-continuous. Sampling of final bagasse by
taking a primary sample once every quarter of an hour can also
be called semi-continuous, but due to the relatively large time
interval between two primary samples, one could also speak of
snap samples being taken.
The particular method of sampling to be employed in each
separate case should be decided on very carefully. It should be
remembered that the aim is to produce a sample, the composition
of which is as similar to that of the mass of the material which is
being sampled as is required by the use of the analytical data
determined on the sample. For this reason where great accuracy is
not required, catch samples taken at fairly large time intervals will
often be adequate, particularly when the variability in the compo-
sition of the material to be sampled is relatively small.
However where great accuracy is required, continuous
sampling should be employed and care should be taken that the
ratio between the weight of the fraction of the sample
extracted in each unit of time and the weight of the material it
represents, is constant.
It is sometimes better to take a number of catch samples than
a continuous sample, for example if it is desirable to get some
information on the variability of the composition of the sampled
material. Catch samples are also taken when it is feared that a
continuous sample will deteriorate during the sampling period.
b. In order to obtain correct results, cleanliness of sample receptacles
and strict periodic supervision of the sampling are essential. With
regard to the state of cleanliness, seamless stainless steel or copper
buckets with seamless rounded bottoms shall be used because such
vessels are readily kept clean. Sample buckets should be provided
in duplicate sets so that when one set is in use the other may be
cleaned.
c. With regard to supervision, it is essential that a record of all
sampling devices be kept in each laboratory, that all sampling
devices and receptacles be inspected at least once in twenty-four
hours, and that the results and time of the inspection be logged and
kept as a permanent record of sampling conditions throughout the
season.
d. A summary of the sampling procedures recommended for taking
the routine samples has been included in Table VII.
2. Cane
a. The very nature of cane makes representative sampling a precarious
undertaking and special care is required to achieve some measure
of accuracy.
To sample a field of cane for the purpose of studying changes
in its sucrose content as an indication of the ripening process,
or for other purposes, in each sampling operation one stalk should
be taken from a large number of marked stools randomly distributed
over the field. If a second sample has to be taken, it too should
consist of one stalk from each of the marked stools used for the
first sampling operation.
b. If a fairly large sample has to be sub-sampled to obtain a quantity
sufficiently small to be crushed conveniently in a laboratory mill,
the following procedure should be used. Sticks are arranged in
descending order of length with tops all one way. Each stick is
then cut into three (approximately equal) lengths and replaced in
position. Sub-sampling is done by taking the top sections from the
first, fourth, seventh, etc., the middle sections from the second,
fifth, eighth, etc., and the butt sections from the third, sixth, ninth,
etc. This gives one sub-sample. Two more sub-samples may be
obtained by taking alternate lengths from each section.
3. Bagas s e
a. Since representative sampling and sub-sampling of bagasse are
matters of considerable difficulty, routine sampling of bagasse for
pol and moisture determinations shall be done at all factories in
the following manner:
i. Regardless of chokes or other irregularities of crushing, a
sample of bagasse shall be taken at least every quarter of an
hour throughout the width across the discharge of the mill as
the bagasse emerges from the last two rollers of the milling
train.
ii. The sample shall be taken by using a small trough-shaped
sampler, the length of which shall be the same as the width
across the discharge of the last mill chute. A simple but
effective sampler comprises a length of galvanized iron
guttering 5 inches wide and 3 inches deep, closed at one end
and strengthened by two supports which also serve as handles,
iii. The sampler should be constructed to hold, when full,
approximately 3 to 7 lb. of final bagasse. When sampling is
carried out the sampler is held across and below the falling
bagasse and as a precaution against the sampler being dis-
lodged during sampling by the weight of material above it,
protective guide lugs to support each end of the sampler
should be welded to the side of the mill discharge chute.
iv. The quarter hourly samples shall be placed in a closed
container which has a capacity of approximately 30 lb. of
final bagasse.
v. Such a container shall be constructed in accordance with the
diagram shown in Figure 2.
FIGURE 2
BAGASSE CONTAI NER
vi. At the end of each hour the sub-samples so collected shall be
thoroughly mixed, coned and quartered. Two opposite
quarters shall be rejected, the remaining two quarters shall
be intimately mixed. This whole operation must be done as
thoroughly and quickly as possible to avoid selective sub-
sampling and loss of moisture.
vii. This constitutes the hourly sample for analysis from which
520 g for the pol test and 100 g for the moisture test are drawn
at random.
4. First expressed juice
a. Sampling procedure
i. The sampler is continuous and automatic. The fundamental
purpose of this device is to give a continuous sample of the
juice as it flows from all points along the whole width of the
first two rollers of the crushing train. The sampler is designed
to make it possible to adjust the rate of delivery in accordance
with the size of sample required.
ii. Figure 3 is a diagram of the first expressed j uice sampler
which shall be used. In the diagram the size of the sampler
relative to that of the mill has been enlarged. A convenient
length for each rotating sampling pipe is about six inches.
The sampler receiving tank shall be made of stainless steel,
copper or heavily enamelled metal, while the rotating dippers
shall be made of stainless steel or copper. Exception will be
made in the case of a mill operating a 2-roller crusher where
a dipper sampler in the juice gutter shall be permitted.
iii. Cleanliness of the apparatus is maintained by the installation
of a steaming system. Great care shall be taken that cleaning
operations are not carried out while sampling is in progress,
otherwise dilution of the sample, due to condensation of
steam, will take place.
iv. The rate of flow and the size of the receiving container shall
be proportioned so that the container is not more than
filled during the period of taking the sample. At the end of
the sampling period the contents of the container shall be
well mixed before a sub-sample is taken to the laboratory.
b. Signalling devices
In order to indicate to the sample taker the time when the
beginning and end of any consignment of cane has reached the
first pair of rollers, an automatic signalling device shall be installed.
Figure 4 is a diagram of the signalling device which shall be used.
The details governing the time of switching the bulbs on and off
will vary according to the conditions obtaining, being dependent
largely on the length of the main cane carrier.
SHAFT WITH CONTACT DRUM FOR A.C. ONLY 220V.
5. Mixed juice
a. Mixed juice shall be sampled after it has been weighed and at the
point of weighing.
b. The sample shall be proportionally representative of the weight of
juice and of the juice at every depth in the scale tank.
c. Figure 5 is a diagram of the automatic j uice sampler recommended
for sampling cold juice. It has the following constructional details.
i. A copper tube of 25 to 32 mm diameter is placed so that one
end of it is in the outflow during the discharge of the j uice
from the scale tank.
ii. This tube is inserted in the stream of juice to a depth such
that sufficient j uice is collected to provide an aliquot sample
per scale tank.
iii. Care should be taken to exclude an excessive amount of froth
which may enter the sampler at the end of the discharge.
iv. In order to minimize evaporation and deterioration during
sampling, the distance between the point of sampling and
the discharge into the sample bucket should be kept as short
as possible.
v. The sample bucket shall be situated so that contamination of
the contents from outside sources is avoided.
vi. A spare sampling tube shall be provided to permit cleaning
which shall be carried out at least once per shift.
vii. The mixed j uice bucket and contents shall be taken to the
laboratory every hour and the juice sub-sampled for analytical
purposes on a pro rata basis in relation to the total weight of
juice weighed during each hour.
6. Last expressed j uice
When a continuous sample is not taken, a catch sample shall be drawn
along the full length of the roller at the same time as the bagasse is
sampled, and the juice sub-sampled in the laboratory.
7. Sulphited mixed juice
A catch sample of mixed juice for acidity and sulphur dioxide determina-
tion should be taken from the j uice-tempering tanks.
8. Clarified j uice and filtered j uice
These samples should be taken automatically wherever possible, or catch
samples may be taken at frequent intervals.
9. Filter cake
This sample should be taken from the truck which is receiving the filter
cake. The sample should be taken with a long tube.
10. Syrup
This sample should be taken automatically wherever possible or catch
samples may be taken immediately before the syrup enters the pans.
FIGURE 5
MI XED JUI CE SAMPLER
34 1962
11. Massecuite (from pan)
A catch sample is required as the massecuite comes from the pan, avoiding
the first runnings and steamings.
12. Massecuite (from crystallizer)
A catch sample is taken as required.
13. Molasses
a. Run-off molasses from centrifugals: A catch sample is required, as
nearly as possible representative of the bulk of the run-off.
b. Molasses prepared for boiling: A catch sample is required.
c. Molasses for sale: A representative continuous or catch sample
should be taken as each tank car is being filled.
d. Final molasses: Samples should be taken continuously from the
discharge side of the molasses pump or from the scales. Otherwise
catch samples should be taken as frequently as required for
representative sampling.
14. Sugar
a. Sampling procedures
i. To enable the factory manager to check effectively the quality
of his product, sugar is usually sampled, either continuously
or semi-continuously, at a suitable point before being bagged,
shipped in bulk or leaving the factory for storage.
Sampling procedures may differ according to local con-
ditions but it is always essential that the sample is thoroughly
representative and that it will not undergo any change before
analysis.
Samples may represent one strike or all the sugar
produced during a fixed period of time. Composite samples
representing the sugar produced during a day or a week are
often prepared.
ii. When sugar is bagged and sampling at the scales is feasible,
the primary samples should be drawn from not less than one
in every 5 to 10 bags and should be at least in the proportion
of 10 g per 200 lb. of sugar.
iii. Where sampling at the scales is not feasible, the same fre-
quency of sampling and proportion of weights should be
aimed at.
iv. Where raw sugar is shipped in bulk, samples can often
be taken suitably from a conveyor belt or from the chute
leading to the railway truck. For automatic sampling through
an opening in a chute, a mechanically operated device to
extract the sample regularly is strongly recommended.
v. To sample closed j ute, hessian or cotton bags (sampling of
sugar packed in paper bags is often not practicable) a trier
should be used. The trier should be the "short trier"* as
used by the United States Treasury Department and specified
by the United States Bureau of Standards. The dimensions
of the trier should be as follows:
Overall length: 40.6 cm
Length of spoon: 22.9 cm
Length of shank: 17.8 cm
Length of handle: 26.7 cm
Width of spoon: 2.7 cm
Depth of spoon: 0.8 cm
Diameter of handle: 3.8 cm
vi. In the sugar industry it is normal to sample one in every 5
to 25 bags, depending on the size of the lot.
vii. The S. A. Bureau of Standards specifies that from lots compris-
ing 10-1000, 1001-3000 or more than 3000 containers 10, 20
or 30 containers respectively shall be taken at random. The
trier should be plunged into the middle of the package and
withdrawn filled with sugar. If the trier has the correct
length, all the layers of sugar, from the outside to the centre
of the package should be correctly represented. Great care
should be taken not to obtain a surface sample, because of
the variations caused by drying or absorption of moisture.
The total contents of each trier should be emptied into a
suitable receptacle and the trier left clean for the next sample,
the whole operation being conducted as rapidly as possible.
b. Receptacles
i. A suitable model is seamless, 260 mm high and 178 mm in
diameter, fitted with a funnel shaped concave lid with a hole
32 mm in diameter. The funnel should have a depth of 45 mm.
When sampling hot sugars in particular, a receptacle
with a close-fitting trapdoor operated by a foot lever has
certain advantages,
ii. Before removing the sample, the receptacle should be well
shaken to redistribute regularly over the sugar any moisture
which may have condensed on its inside wall,
iii. The frequency at which receptacles should be replaced and
emptied depends on local conditions. Once every hour, or
once per 50 tons of sugar, is often adequate.
c. Sub-sampling
i. Whether sub-samples are prepared from the contents of one
or of more than one receptacle depends on local conditions,
but mixing the contents of more than three receptacles is
* An illustration of the trier will be found in Spencer and Meade, Cane Sugar
Handbook, New York, John Wiley and Sons, Inc., 8th edition, p. 506.
normally not done. Mixing and sub-sampling should be
done with the utmost despatch to avoid loss or absorption of
moisture by the sugar,
ii. The contents of the receptacle(s) are passed through a wire
screen with openings of 9 to 10 mm (or th inch mesh) on to
a metal table-top. All lumps on the screen are broken up and
added to the sample. Bits of bag, fibre, bagasse, string and
other foreign matter are discarded,
iii. The preparation of the sub-samples should be done by the
standard procedure of "coning and quartering". The final
sub-sample should weigh not more than 350 g but must be
sufficient to completely fill the sample bottle of 250-275 g
capacity. After filling, the sample bottle must be closed with
a lid which hermetically seals it.
d. Analysis of sub-samples
The quantity to be weighed out for analysis should be removed
from the bottle by means of a suitable trier which penetrates the
sugar completely from top to bottom. The trier must be constructed
so that a similar quantity will be removed from each layer of sugar
in the bottle and it is recommended that the dimensions of the trier
should be such that the quantity extracted in one operation be as
close as practicable to the amount which it is desired to weigh.
CHAPTER VI
RE AGE NTS
1. General
In addition to the name and strength of the reagent, the date of its
preparation should be shown on the label. Solutions should be made
in distilled or deionized water. Volumes should be completed at a
temperature as near 20C as circumstances will allow.
2. Clarifying reagents
a. Lead subacetate solution for general use: Lead subacetate solution
of 30 Be is prepared by dissolving dry subacetate of lead powder
in hot distilled water and subsequently diluting to 30 Be (54 Bx,
1.25 S.G.).
Note: Bottles containing solutions of lead subacetate should always be
provided with a soda-lime tube as a protection against the carbon dioxide of
the atmosphere.
b. Neutral lead acetate solution: Dissolve neutral lead acetate crystals
in distilled water to make a saturated solution, then add glacial
acetic acid to render the solution faintly acid to litmus paper.
Dilute to 30 Be (54 Bx, 1.25 S.G.).
c. Dry subacetate of lead
i. The salt produced shall be dry and conform to the following
specifications of the American Chemical Society which,
together with the methods of testing, have been taken from
I. & E.C., Anal. Ed., 16 (1944) 282.
Basic lead ( PbO) : not less than 33 %
Insoluble in acetic acid: not more than 0.05 %
Insoluble in water: not more than 2.0%
Moisture (loss at 100C): not more than 1.5%
Chloride (CI): not more than 0.005 %
Nitrate ( N0
3
) : to pass test (limit about 0.003 %)
Substances not precipitated
by hydrogen sulphide: not more than 0.30%
Copper ( Cu) : not more than 0.005 %
Iron( Fe) : not more than 0.005 %
The salt must also conform to the following specifications for
fineness:
1. 100% to pass through a sieve with aperture 0.42 mm
(35-mesh Tyler sieve).
2. 70% to pass through a sieve with aperture 0.125 mm
(115-mesh Tyler sieve).
ii. Whenever containers of bulk quantities of this powder are
opened, the powder shall be transferred to air-tight glass
receptacles. This clarifying agent should be kept out of
contact with the atmosphere (in so far as is compatible with
routine laboratory practice).
iii. P ROCEDURES FOR TESTING BASIC LEAD ACETATE
The methods of analysis given below are those specified by
the American Chemical Society.
B ASI C LEAD : Weigh accurately about 5 grams and dissolve in 100 ml
of carbon dioxide-free water in a 500 ml volumetric flask. Add 50 ml of
normal acetic acid and 100 ml of a carbon dioxide-free 3% solution of
sodium oxalate. Mix thoroughly, dilute to volume with carbon dioxide-
free water, and allow the precipitate to settle. Titrate 100 ml of the clear
supernatant liquid with normal sodium hydroxide, using phenolphthalein
indicator. Each millilitre of normal acetic acid consumed is equivalent
to 0.1116 gram of PbO.
I NSOLUB LE I N ACETI C ACI D : Dissolve 5 grams in 100 ml of
water and 5 ml of acetic acid, warming if necessary to complete solution.
If an insoluble residue remains, filter and wash until the washings are
no longer darkened by hydrogen sulphide. Dry at 105-110C. The weight
of the residue should not exceed 0.0025 gram.
I NSOLUB LE IN W ATER: Agitate 1 gram in a small stoppered flask
with 50 ml of carbon dioxide-free water and filter at once. Wash with
carbon dioxide-free water and dry at 105-110C. The weight of the residue
should not exceed 0.0200 gram.
M OI STURE : Weigh accurately about 0.5 gram and dry for 2 hours at
105-110C. Cool and reweigh. The loss in weight should not exceed
1.5%.
CHLORI D E : Dissolve 1 gram in 50 ml of water and add 1 ml of nitric
acid and 1 ml of 0.1 N silver nitrate. Any turbidity should not be greater
than is produced by 0.05 mg of chloride in an equal volume of solution
containing the quantities of reagents used in the test.
NI TRATE : Dissolve 1 gram in 9 ml of water containing 5 mg of sodium
chloride. Add 0.7 ml of acetic acid, 0.2 ml of indigo carmine solution
(1 to 1000), and 10 ml of sulphuric acid. Stir thoroughly and allow to
stand for 10 minutes. The blue colour of the clear solution should not
be completely discharged.
SUB STANCES NOT P RECI P I TATED B Y HY D ROGEN SULP HI D E:
Dilute 10 ml of solution A (see footnote) to 100 ml, pass hydrogen
sulphide through the solution to precipitate all the lead, and filter.
Evaporate 50 ml of the filtrate to dryness and ignite gently. The weight
of the residue should not exceed 0.0015 gram.
COP P ER : To 25 ml of solution A (see footnote) add about 0.05 gram
of aluminium chloride and a few crystals of ammonium persulphate.
Neutralize with ammonium hydroxide and add a very slight excess.
Heat to boiling, cool and filter. Save the precipitate for the determination
of iron. Neutralize the filtrate to phenolphthalein, add 0.25 ml of acetic
acid in excess and 0.25 ml of a freshly prepared 10 % solution of potassium
Solution A: Dissolve 5 grams in 42 ml of water and 3 ml of acetic acid, and add
5 ml of sulphuric acid. After standing for about 10 minutes, filter the solution.
ferrocyanide. Any pink colour produced should not exceed that pro-
duced by 0.125 mg of copper in an equal volume of solution containing
the quantities of reagents used in the test.
I RON : Wash the precipitate of iron and aluminium hydroxides obtained
in the previous test sufficiently to remove most of the acetate. Dissolve
the precipitate in 10 ml of hot dilute hydrochloric acid (1 + 5 ) , wash
the paper and dilute to 50 ml. Dilute 20 ml of this solution to 45 ml and
add a few crystals of ammonium persulphate, 3 ml of hydrochloric acid,
and 3 ml of a 30% solution of ammonium thiocyanate. The colour
should not be more than is produced by 0.05 mg of ferric iron in 45 ml
of water to which are added 3 ml of hydrochloric acid and 3 ml of a
30% solution of ammonium thiocyanate.
d. Alumina cream {aluminium hydroxide): To a cold saturated solution
of common alum (aluminium potassium sulphate) in water, add
ammonia with constant stirring until in slight excess, and allow the
precipitate to settle. Pour off the supernatant liquid and wash the
precipitate by decantation until the wash water shows only a slight
content of sulphate when tested with barium chloride solution. The
excess water is poured off and the creamy suspension stored for use.
3. Indicators
a. Indicators for measurement of pH: A complete list of indicators
with directions for their preparation is given in Browne and Zerban,
Sugar Analysis, New York, J ohn Wiley & Sons, Inc. (3rd edition),
p. 559. While it is agreed that indicators can be successfully employed
in chemical control when proper precautions are taken, it is never-
theless recommended that use be made, wherever possible, of pH
meters of which reliable models are available. The use of indicator
paper for pH control in the factory is not recommended since such
paper has often been found to yield erroneous results.
b. Neutral water for dilution of indicators: Distilled water which has
been boiled for about 5 minutes and cooled in a flask fitted with
a soda-lime tube, if continuously protected from the atmosphere,
will read 7.0 pH (very nearly) and will constitute a suitable un-
buffered water for dilution.
c. Buffer solutions: Ranges of buffered solutions may be purchased.
The use of these commercial buffers is recommended, but chemists
who prefer to make their own buffer standards are referred to
Browne and Zerban, Sugar Analysis, New York, John Wiley &
Sons, Inc. (3rd edition), p. 556.
It may be recorded that the pH of a 1 % solution of
ammonium acetate is very nearly equal to 7.0 and again that a
solution of 1.02 g of potassium hydrogen phthalate crystals in
100 ml of distilled water has a constant pH of 4.0 between 18 and
40C. These buffer solutions will be found suitable for readjusting
pH-meters.
4 0 1962 Laboratory Manual for S. Af r . Sugar Factories
d. Indicator solutions made up in the laboratory
i. P HENOLP HTHALEI N: A 1% solution of the powder in
rectified spirits. The phenolphthalein may be dissolved in
about half the required volume of alcohol and diluted with
water. The solution should always be rendered very faintly
pink before use by addition of an alkali,
ii. METHYLENE BLUE: 1 %aqueous solution.
iii. ALP HA- NAP HTHOL: 4 % alcoholic solution.
iv. STARCH FOR I OD I NE TI TRATI ONS: A starch indicator
which keeps indefinitely may be prepared by dissolving 1 g
of salicylic acid in 100 ml water, boiling and pouring into it
1 g starch mixed with a little water. Boil gently till the starch
is dissolved, let cool somewhat, then dilute with cold water
to one litre.
4. Standard acid and alkali solutions
a. A reagent solution, of which the strength has been accurately
determined, is called a " standard" solution.
b. A " normal" solution of a reagent is one that contains in one litre
that proportion of its molecular weight in grams which corresponds
to 1.008 g of available hydrogen, or its equivalent.
c. Preparation of standard acid and alkali solutions
i. N- HY D ROCHLORI C ACI D SOLUTI ON: Dilute 100 ml
concentrated hydrochloric acid (S.G. 1.15) to 1 litre. From
this solution diluted standards such as N/10 HC1, etc., may
be prepared. These solutions can be standardized against
sodium carbonate or standard caustic soda, as described
under 4, d, below.
ii. N- S OD I UM HY D ROX I D E SOLUTI ON: Weigh out rapidly
approximately 41 g caustic soda (A.R.) and dissolve in a
one litre flask. Allow the solution to cool while being pro-
tected from the carbon dioxide of the atmosphere by a soda-
lime tube. Then dilute to one litre, and keep the solution
protected from carbon dioxide.
From this solution diluted standards such as N/10
Na OH, etc., may be prepared.
These solutions may be standardized against potassium
hydrogen phthalate or standard hydrochloric acid solution as
described under 4, d, below.
d. Standardization of acid and alkali solutions: Weigh out an
exact amount of about 4.1 g potassium hydrogen phthalate,
C
6
H
4
.COOH.COOK. Prior to use this salt should be dried at
120C for 2 hours and allowed to cool in a desiccator. Dissolve in
Laboratory Manual for S. Af r . Sugar Factori es 1962 4 1
recently boiled distilled water and titrate 20 ml aliquots with
N- Na OH solution contained in a burette, using phenolphthalein as
indicator.
5. lodimetry
a. General
A standardized iodine solution is generally used for measuring the
amount of what is usually termed " SO
2
in j uice". Since one litre
of N/32 iodine solution corresponds to 1 g of S0
2
, it is convenient
to titrate the juice with an iodine solution of this concentration.
The (unstable) N/32 iodine solution is prepared from N/1.6
iodine stock solution and at least once per 24 hours titrated against
N/32 sodium thiosulphate solution. The thiosulphate solution
should be standardized against potassium iodate at least twice per
month.
b. Preparation of N/32 sodium thiosulphate solution
i. A solution of sodium thiosulphate prepared from the pure
salt in pure water (conductivity water) is quite stable. Slow
decomposition, however, usually occurs, partly due to an
excess of carbon dioxide in the water, partly as a result of the
growth of micro-organisms. Thiosulphate solutions therefore
must be standardized twice per month,
ii. N/32 sodium thiosulphate solution contains 7.753 g/litre
Na
2
S
2
0
3
.5H
2
0, but it is not possible to prepare sodium
thiosulphate solutions of definite strength by weighing out the
pure salt as purchased because sodium thiosulphate penta-
hydrate effloresces very easily,
iii. Dissolve 7.75 g of the pentahydrate in 1 litre of freshly boiled,
cooled water, and add 0.1 g of sodium carbonate to the
solution in order to retard deterioration.
c. Standardization of N/32 sodium thiosulphate solution
Potassium iodate reacts with potassium iodide in acid solution to
liberate iodine which can be titrated with thiosulphate:
K I0
3
+ 5KI + 3H
2
S0
4
= 3K
2
S0
4
+ 3I
2
-+- 3 H
2
0
Potassium iodate has an equivalent weight of 35.67 and the A.R.
salt has a purity of 99.9 per cent. It should be dried at 120C
before use. Weigh out accurately about 1.2 g of pure potassium
iodate, say 1.213 g. Dissolve in water and make up to one litre in
a volumetric flask. Pipette out 25 ml of this solution into a 250 ml
Erlenmeyer flask, add 0.5 g pure potassium iodide and 2 ml of
N-sulphuric acid. Titrate the liberated iodine with the thiosulphate
solution and when the colour has become a pale yellow dilute to
about 200 ml with distilled water. Add 2 ml of starch solution and
continue the titration until the blue colour j ust vanishes. Suppose
that 21.7 ml of the thiosulphate solution were used. Then the
normality of the solution is
d. Preparation of iodine stock solution, N/1.6 approximately: Weigh out
180 g of potassium iodide and transfer to a clean one litre volumetric
flask. Dissolve in the minimum quantity of distilled water and add
80 g of iodine. Rotate until iodine is completely dissolved then
dilute with distilled water to 1000 ml. Keep the stock solution in
a cool dark place.
e. Preparation of N/32 iodine solution: 100 ml of the stock solution
diluted to 2 litres constitutes the N/32 solution required for SO
2
determinations. This diluted iodine solution should be standardized
against N/32 thiosulphate solution every 24 hours.
f. Standardization of N/32 iodine solution: Thiosulphate is oxidized to
tetrathionate by iodine:
The solution should be faintly acid otherwise part of the thiosulphate
may be converted into sulphate:
Add 1 ml of 30% sulphuric acid to 25 ml N/32 iodine solution
pipetted into a 250 ml Erlenmeyer flask and titrate with standardized
N/32 thiosulphate solution until a faint yellow shade is obtained.
Add a few drops of starch solution and titrate until colourless.
6. For the determination of sucrose
a. Hydrochloric acid solution: Dilute concentrated hydrochloric acid
to 24.85 bx (add approximately 1750 ml concentrated hydrochloric
acid to 1000 ml water), corresponding to approximately 20 % by
weight
b. Sodium chloride solution: A solution containing 231.5 g A.R.
sodium chloride per litre is required.
7. For the determination of reducing sugars
a. Preparation of standard invert sugar solution: For this solution the
sugar used should be of the highest standard obtainable, e.g. A.R.
sucrose or high grade refined sugar. This sugar should be dried
and kept in an air-tight glass container.
Dissolve 9.500 g of the above dried sugar in 70 ml water in a
1 litre volumetric flask. Add 10 ml hydrochloric acid solution
see under 6, a aboveand set aside at laboratory temperature for
5 days. Add sodium hydroxide solution to raise the pH to about
3 (a separate titration against 10 ml hydrochloric acid indicates the
quantity of alkali required) followed by 2 g benzoic acid dissolved
in distilled water. Make up to volume with distilled water. This
solution contains 1 g invert sugar per 100 ml.
For use 50 ml of this 1% invert solution is pipetted into a
100 ml volumetric flask and made up to volume with distilled
water. This solution contains 0.5 g invert sugar per 100 ml.
b. Preparation of Fehling's solution, Soxhlet's modification: Large
quantities of the component solutions comprising the Fehling's
solution are generally required. A.R. salts should be used in the
preparation of the solutions which are made up in quantities of
2 litres as follows:
Solution A dissolve 138.556 g of copper sulphate,
CuS0
4
.5H
2
0, in water and dilute to 2000 ml in a volumetric flask.
Solution B dissolve 692 g of sodium potassium tartrate
(Rochelle salt) in about 1000 ml of water, mix with 400 ml of a
solution containing 200 g sodium hydroxide and complete the
volume to 2000 ml.
It will be found sometimes that a slight sediment settles in
both solutions on standing. This sediment may be removed by
decanting the clear supernatant liquids. It is necessary to keep
solutions A and B separate, and these should be mixed in equal
proportions only when required and immediately before use. In
every case where Fehling's solution is mentioned, a mixture of
exactly equal parts of solutions A and B is understood.
c. Standardization of Fehling's solution: The neutralized invert sugar
solution prepared as under a above, is titrated against 25.0 ml
Fehling's solution. If the Fehling's solution is of correct strength,
24.8 ml of invert solution will be used. If less than 24.8 ml of invert
sugar solution is required, the Fehling's solution is too weak and
copper sulphate should be added to solution A until the desired
24.8 ml is used. Similarly, if more than 24.8 ml is used, solution A
should be diluted until 25 ml Fehling's solution corresponds to
24.8 ml invert sugar solution.
d. Preparation of Luff-Schoorl solution
i. SOLUTI ON A: Prepare solution A by dissolving with
slight heating 17.3 g A.R. copper sulphate ( CuS0
4
.5H
2
0)
and 115 g A.R. citric acid in 200 ml water.
ii. SOLUTI ON B: Dissolve 185.3 g of anhydrous sodium
carbonate, analytical reagent, previously dried for 30 minutes
at 250C in a hot-air oven, in 500 ml water.
4 4 1962 Laboratory Manual for S. Af r . Sugar Factories
iii. LUFF SOLUTION: Add solution B slowly and with constant
shaking to solution A. Never add solution A to solution B.
Cool and make up to 1 litre.
iv. POTASSIUM IODIDE SOLUTION: Dissolve 20 g A.R.
potassium iodide in 80 ml of water. (This solution must be
iodate-free.)
v. DI LUTE SULP HURI C ACID ( 1: 5 ) : Prepare from ana-
lytical reagent-grade sulphuric acid by adding 1 vol. acid to
5 vols water.
vi. STARCH INDICATOR SOLUTION: See under 3, d, iv
above.
vii. THI OSULP HATE SOLUTION ( N/ 10 ) : Dissolve 25 g of
A.R. sodium thiosulphate crystals plus 0.2 g anhydrous
sodium carbonate in distilled water and make up to 1 litre.
Standardize against A.R. potassium iodate as described
under 5, c above.
8. Juice preservative
Dissolve 150 g of mercuric chloride in hot water and add solid potassium
iodide until the precipitate first formed is redissolved. Dilute to 1 Utre.
Use 0.2 ml of the solution for every litre of juice.
9. For the determination of calcium and magnesium
a. Ethylenediaminetetraacetic acid: The solution consists of approxi-
mately 8 g of the disodium salt of ethylenediaminetetraacetic acid
("versenate") and 1.5 g of A.R. caustic soda dissolved in water and
made up to 1 litre.
b. Standard calcium chloride solution: This solution may be prepared
by accurately weighing out 1.5 g of A.R. calcium carbonate, dis-
solving in a small excess of hydrochloric acid, and making up to one
Utre. This solution is used to standardize solution a above.
c. Buffer solution (according to Saunier and Lemaitre): 6.75 g of
ammonium chloride, 57 ml of ammonia solution (S.G. 0.9) and
0.1 g of potassium chromate are dissolved in water and made up
to 100 ml. This solution is then mixed with 100 ml of a saturated
solution of sodium potassium tartrate.
d. Eriochrome-black T: 0.5 g of the dye-stuff is ground in a mortar
with 100 g of A.R. sodium chloride or A.R. sucrose. The mixture
is kept in an airtight jar.
e. Murexide: 0.2 g of murexide and 1.5 g naphthol green B are ground
with 100 g of A.R. sodium chloride to a fine powder. The mixture
should be protected from the damp atmosphere. The naphthol
Green B which acts as a screening agent may be omitted if so desired.
f. Caustic soda solution: This should be made from A.R. caustic
soda, and should be approximately 6N i.e. 240 g per litre.
g. Standardization of the ethylenediaminetetraacetic acid solution: The
solution of ethylenediaminetetraacetic acid should be standardized
against a calcium chloride solution. To do this, 80 ml of tap water
(containing magnesium salts), 4 ml of the buffer solution and
0.2 g of Eriochrome black T indicator are measured into a 350 ml
Erlenmeyer flask. The solution of ethylenediaminetetraacetic acid
is then added drop-wise from a burette until the colour of the
indicator changes from red to blue. 20 ml of the standard calcium
chloride solution is then added by means of a pipette, and after the
burette has again been filled to the 0 ml mark, the titration is
continued until the endpoint is again reached. Since the molarity
of the calcium chloride solution is known, the strength of the
titrating solution can be calculated in terms of millimols of calcium
or magnesium per litre.
10. For the determination of available phosphate
a. Ammonium molybdate solution: 15.0 g ammonium molybdate is
dissolved in 300 ml water at 50C. After filtering and cooling,
350 ml of concentrated hydrochloric acid is added. The solution is
cooled and made to 1 litre. The solution should be stored in a dark
bottle and made up freshly every 2 months.
b. Reducing solution: 90 g sodium metabisulphite is dissolved in
800 ml of water. 7 g anhydrous sodium sulphite and 1.5 g 1-amino-
2-naphthol-4-sulphonic acid are dissolved in 100 ml of water. The
two solutions are mixed and diluted to one litre. Store in an amber
glass bottle under refrigeration.
c. Standard phosphate solution: Dissolve 0.7668 g A.R. monopotassium
phosphate ( KH
2
PO) in distilled water, and transfer quantitatively
to a 1 litre flask. Add 10 ml of sulphuric acid (S.G.1.3) and make
to the mark. This standard, of which 1 ml is equivalent to 0.4 mg
P
2
0
5
, keeps indefinitely.
d. Diluted standard phosphate solution: 25 ml of the above stock
solution is diluted to 1 litre. 1 ml = 0.01 mg P
2
O
5
.
11. For the determination of sulphur dioxide (modified Monier-
Williams method)
a. Hydrogen peroxide solution: A 3% solution adjusted to pH 4
with N/100 HC1, using a pH meter.
b. Hydrochloric acid, concentrated: Analytical reagent grade.
c. Sodium hydroxide solution: N/50 accurately standardized.
d. Alkaline pyrogallol solution: Dissolve 10 g of sodium hydroxide and
30 g of pyrogallol in water and dilute to 100 ml.
CHAPTER VI I
GE NE RAL ME TH OD S OF ANALYS I S
1. Temperature
Saccharimeters, volumetric glassware and brix hydrometers recommended
for this industry are all standardized at 20C and departure from this
temperature introduces errors. Temperature corrections can and should
be applied where necessary but it must be realised that these are only
approximations. Every attempt should therefore be made to install
constant temperature laboratories operating at 20C. In all cases however,
apparatus should be used at the laboratory or room temperature so as
to maintain a uniform temperature in the solution under test, e.g. in cases
where polarizations are to be made in a constant temperature room
at 20C, care must be taken to ensure that other operations such as making
to volume are also carried out at 20C.
2. Filtration
Where filtration is slow or delayed, adequate precautions must be taken
against evaporation by setting the funnel directly on the receiving vessel
and covering with a watch glass. For ordinary rapid working, this pre-
caution is not regarded as necessary for dilute solutions such as mill
juices or products diluted to the same density, or the dilute solutions
from bagasse or filter press cake. In testing sugar however, this pre-
caution must always be taken.
The first runnings from the filter must in all cases be discarded
after rinsing the receiving vessel.
3. Brix
Before filling hydrometer j ars to overflowing, samples should be well
mixed and strained through a 14 mesh copper wire sieve, the whole
operation being carried out as near room temperature as possible. The
reason for straining is to remove bagasse particles which may affect
the reading of the brix spindle. Samples should be left to stand at least
twenty minutes to allow all air bubbles to rise to the surface. Care
must be taken to ensure that the brix spindle, which must be clean and
dry, floats freely. To improve the accuracy, the approximate reading
is noted and after drying the spindle above the reading, it is carefully
reinserted to keep the stem dry above the liquid. A final reading to the
nearest 0.05 is taken, after the spindle has been floated for at least
two minutes, by bringing the eye level with the surface of the liquid
and noting where the meniscus intersects the scale. The film of liquid
drawn up around the stem should be disregarded. In Figure 6 the correct
reading is 2.1. Immediately after taking the reading (which is the
uncorrected brix) the temperature should be taken, or when the
hydrometer is provided with a scale showing the temperature corrections
to the brix readings, the appropriate correction should be applied to
provide the corrected brix.
BRIX
SPINDLE READING
Polarization, pol or apparent sucrose
a. Home's dry lead method: To an unmeasured quantity of solution
(say about 100 ml) in a beaker, add a minimum (usually about
1 g/100 ml) of powdered dry subacetate of lead, shake or stir
vigorously and when the clarification is complete, filter. Polarize
in a 200 mm tube.
The pol is calculated by means of the formula:
Pol
normal weight x saccharimeter reading Sr
Weight in grams of 100 ml solution
where: the normal weight is either 26.000 or 26.026 grams,
depending on the scale of the saccharimeter used.
the weight in grams of 100 ml solution is equal to 99.718 X
specific gravity solution at 20/20C.
In practice, the pol is found from Table III (Schmitz's Table) or
a modification of this table when a saccharimeter fitted with the
Ventzke scale is used.
b. Normal weight method: Weigh out the normal weight or a multiple
or fraction thereof into a 100 ml sugar flask. Make to the mark
with distilled water, add the minimum quantity of dry basic lead
acetate necessary for clarification, shake vigorously and filter.
FIGURE 6
48 1962
Instead of dry basic lead acetate, a solution of basic lead acetate
may be used by adding the minimum quantity necessary for clari-
fication before making to the mark. Polarize in a 200 mm tube.
If the normal weight has been used, the pol is equal to the sacchari-
meter reading, but when a multiple or a fraction of the normal
weight has been used, the saccharimeter reading must be multiplied
by the reciprocal of the normality used.
5. Sucrose
a. Using acid inversion (modified Jackson & GUI is method IV)
i. The solution to be analysed should be clarified with dry
subacetate of lead as described under 4, a above. If desired,
and this practice is recommended for molasses solutions, the
clarified filtrate is deleaded by adding pulverised anhydrous
potassium oxalate and filtering. Two 50 ml portions of the
filtrate (both portions should be taken either from the clarified
or from the deleaded filtrate, not one portion from the clarified
and the other from the deleaded filtrate) are pipetted into
two 100 ml sugar flasks. To the first flask add 10 ml of sodium
chloride solution containing 231.5 g per litre. If after addition
of the sodium chloride solution there develops a cloudiness
which cannot be removed by filtration, clearing by the addition
of a few drops of acetic acid is often practised. Make up to
100 ml with distilled water and shake thoroughly.
ii. To the flask containing the second 50 ml portion add 20 ml
water. Heat in a water bath to 65C and add immediately
10 ml hydrochloric acid =1.1029. Mix by rotating and
set aside for at least 30 minutes. Cool to room temperature
and make to the mark with distilled water, mixing the contents
by rotating j ust before the liquid reaches the level of the neck.
Shake thoroughly.
iii. Fill two j acketed tubes with these two solutions. Insert an
"inversion" type of thermometer into each tube, place the
tubes on a rack and leave them for 30 minutes in the sac-
charimeter room before polarizing. This procedure will
avoid a possible error due to mutarotation and will ensure
a constant temperature which should be similar in both
tubes. The temperature of the solution at the time of taking
the invert reading, should be recorded to the nearest 0.1 C.
The temperature of the two solutions should not differ by
more than 0.2C. The reading of the first solution is termed
the direct saccharimeter reading (Dr) and that of the second
solution the invert saccharimeter reading (Ir). The method
for calculating the percentage of sucrose in the solution
being analysed is given in detail under Mixed j uice, chapter
VIII, 5, c, iii, and Final molasses, chapter VIII, 10, c, i.
b. Using invertase
i. The invertase method is the only method which can be
depended upon to give correct sucrose values for cane products
which may contain fructose, reversion products, and amino
compounds, provided that the solution used for the direct
reading and the inverted solution have approximately the
same pH. Although invertase may be prepared in the labora-
tory from yeast, it is recommended that the commercial
product be purchased. In both cases a check on the activity
of the invertase solution is desirable.
ii. C H E C K O N A C T I V I T Y O F I N V E R T A S E S O L U T I O N :
Instead of determining the k-value of the solution (which
should be approximately 0.1) it is usually adequate for practical
purposes to carry out the following test:
Dilute 1 ml of the invertase preparation to 200 ml.
Transfer 10 g of pure sucrose (no. 1 refined) to a sugar flask
graduated at 100 and 110 ml, dissolve in 75 ml of water, add
2 drops of glacial acetic acid, and dilute to the 100 ml mark.
Make to the 110 ml mark with the diluted invertase solution
and mix thoroughly and rapidly, noting the exact time at
which the solutions are mixed. At the termination of exactly
60 minutes make a portion of the solution j ust alkaline to
litmus paper with small amounts of anhydrous sodium
carbonate and polarize in a 200 mm tube at 20C. If the
invertase solution is sufficiently active, the alkaline solution
will polarize approximately 31S without correcting for the
dilution to 110 ml and the optical activity of the invertase
solution.
Example: 10 grams of sucrose in 110 ml aqueous solution
show a reading in a 200 mm tube of 34.96S and after complete
inversion the reading will be 11.22S. If the invertase
solution is the correct strength, the reading in the above
test should be 31S, corresponding to a drop of
(34.9631.00) X 100
= 8.58 %
46.18
A reading lower than 31S indicates that the invertase con-
centrate is stronger than usual. If for example the reading
is 26S instead of 31S which corresponds to a drop in pol
of 19.4%, the activity of the invertase is
19.40
-------- = 2.26 so a correspondingly smaller volume of the
8.58
invertase solution shall be required for the analysis, as des-
cribed in 5, b, iii, below and in chapter VIII, 5, d and 10, c, ii.
19.40
8.58
(34.9631.00)
46.18
X 100
= 8.58%
50 1962
iii. THE D ETERM I NATI ON: To determine sucrose using in-
vertase, the clarified solution 4, a, above, must be deleaded
with the minimum of anhydrous potassium oxalate and filtered
again. Three 50 ml portions are pipetted into three 100 ml
flasks. The first flask is made up to the mark and thoroughly
mixed. The second portion is used to determine the quantity
of glacial acetic acid required to reduce the pH to 4.7 0.2.
The volume of acetic acid required is noted and this volume
is added to the third flask. Then add the requisite quantity
of the invertase solution (10 ml of the invertase concentrate
is adequate), and mix thoroughly. Place the flask in a water-
bath and allow it to maintain a temperature of 5758C
for fifteen minutes with occasional shaking. Cool and add
carefully with constant shaking a concentrated solution of
sodium carbonate until distinctly alkaline to a minute piece
of litmus paper in the flask. Dilute to the mark and mix
thoroughly. Fill two j acketed tubes with these two solutions.
Insert an inversion type of thermometer into each tube,
place the tubes on a rack and leave them for 30 minutes in
the saccharimeter room before polarizing. The reading of the
first solution is termed the direct saccharimeter reading (Dr)
and the second reading, which must be corrected for the
rotation of the invertase present, the invert saccharimeter
reading (Ir). The temperature of the solution at the time of
taking the invert reading should be noted to the nearest
0.1C. The temperature of the two solutions should not
differ by more than 0.2C.
The saccharimeter readings are converted into the
sucrose percentage of the analysed solution as described in
detail under Mixed juice, chapter VIII, 5, d, iii and Final
molasses, chapter VIII, 10, c, ii.
iv. When very accurate results are required it is preferable to
carry out the inversion at room temperature by allowing the
solution, after addition of invertase, to stand overnight before
taking the invert reading. A further reading is taken several
hours later and if there is no change from the previous reading,
the inversion is complete.
c. The "chemical" method: Sucrose may be estimated chemically by
the determination of reducing sugars, both before and after in-
version, either by acid or invertase. If the difference between the
percentages of reducing sugars obtained is multiplied by 0.95, the
result will represent the weight of sucrose before hydrolysis. This
method of sucrose determination is recommended in the case of
molasses where solutions are often too dark to obtain accurate
optical readings (see chapter VIII, 10, c, ii).
6. Reducing sugars
a. The Lane and Eynon method
For solutions of unknown titre an approximate titration is carried
out as described under "Incremental method" Sub. Par. a, i. This
is followed by the "Standard method" Sub. Par. a, ii. If the approxi-
mate titration is known proceed as under a, ii, omitting a, i.
i . I N C R E ME N T A L ME T HO D O F T I T R A T I O N
Usually 10 ml (but sometimes 25 ml) Fehling's solution is
pipetted accurately into a flat-bottomed narrow neck boiling
flask of 300400 ml capacity. The sugar solution is added
from a 50 ml burette. Initially 1 5 ml is run into the flask and
the mixture heated to boiling. If after the liquid has been
boiling for 10 to 15 seconds its colour shows that much of
the Fehling's solution has not been reduced, further additions
of sugar solution are made, e.g. 10 ml or 5 ml at a time, with
a few seconds actual boiling after each, until it is j udged
unsafe to add more without risk of exceeding the end-point.
At this stage 34 drops of methylene blue are added, and
the addition of sugar solution is continued, 1 ml or less at
a time, at intervals of about 10 seconds, until the indicator
is completely decolourized. The boiling reaction liquid then
resumes the bright orange appearance (due to cuprous oxide)
which it had before the indicator was added. The burette
reading is the approximate titration. During the additions
to the boiling liquid, the burette is held in the hand, keeping
the main burette tube out of the steam.
ii. S T A N D A R D ME T HO D O F T I T R A T I O N
Proceed as in the "Incremental Method" but the initial
addition of sugar solution should be to within 1 ml (but
not closer than 0.5 ml) of the final titration. The contents
of the flask are well mixed in the cold by shaking and then
heated to boiling over a suitable flame or hot plate. The
liquid is kept in moderate ebullition for 2 minutes, and
34 drops of methylene blue solution then added preferably
without touching the sides of the flask. The titration is
completed in another minute by the addition of 23 drops
of the sugar solution at intervals of about 10 seconds, until
the colour of the indicator is completely discharged. Thus
the titration is completed in 3 minutes from the commencement
of the ebullition and during this time the mixture must be
kept boiling continuously as the emission of steam from the
neck of the flask is an effective safeguard against back oxidation
of the Fehling's solution or the indicator by air.
Duplicate titrations by this method should agree to
within 0.1 ml in the volume of sugar solution required. In
the titration of glucose, fructose or invert sugar in the presence
of an excess of sucrose it is especially important that the total
boiling time of 3 minutes be adhered to closely.
The concentration of invert sugar in mg per 100 ml is
obtained from Table IV. The following example illustrates
the calculations involved.
The dilute final molasses solution used in the titration contains 1.3 g
molasses per 100 ml.
Sucrose % molasses = 40%. Hence sucrose concentration in titration
solution is 1.3 x = 0.5 g/100 ml.
This figure indicates the column in Table IV which must be consulted.
Titre = 25.5 ml.
From the 2nd column and by interpolation the concentration of invert
sugar is 199 mg/100 ml or 0.199 g/100 ml
.
.
. R.S. % molasses = x 100 = 15. 31%
b. The Luff-Schoorl method: This method which is recommended for
sugars and is laid down in the Specifications of the S.A. Bureau of
Standards for commercial sucrose, is described in chapter VIII, 11, b.
7. Sulphur dioxide
Methods a. and b. given below yield results which are frequently higher
than the true concentrations of sulphur dioxide present due to the presence
of some other reducing substances in the samples being analysed. However
these methods are sufficiently accurate for factory control purposes.
When highly accurate analyses are required, method c, the Monier-
Williams method, should be employed.
a. The iodine titration method: This method is applied especially
for the determination of S0
2
in juices. The specified volume of
j uice (see chapter VIII, 4, e) or any other solution is diluted with the
appropriate volume of water and titrated against N/32 iodine
solution, using a few drops of starch indicator to determine the
end-point. The end-point may be made sharper by adding a few
drops of concentrated hydrochloric acid when near the end of the
titration.
b. The rapid method of determining available S0
2
in sugars: Available
sulphur dioxide may be determined rapidly in sugars by titration
with an iodine solution. 100 g of the sugar is dissolved in 150 ml
distilled water in a 500 ml Erlenmeyer flask. 5 ml of approximately
6 N sulphuric acid is added followed by a measured amount of
N/32 iodine solution run in from a burette until there is a slight
excess of iodine. Add 1 ml of starch solution and back-titrate
the excess iodine with N/32 thiosulphate solution until the colour
due to the starch iodine complex j ust vanishes. The available
S0
2
content of the sugar in parts per million = 10 x ( number of
ml N/32 iodine used number of ml N/32 thiosulphate used).
c. The Monier-Williams method
i. This method should be used, if only occasionally, to check
the iodine titration method. The method is also laid down
in the Specifications of the S.A. Bureau of Standards for
commercial sucrose.
ii. Connect a 750 ml round-bottomed resistance glass flask B
(see Figure 7) to a sloping reflux condenser D, the lower
end of which has been cut off at an angle. Pass nitrogen
from a cylinder through the alkaline pyrogallol solution in
a wash bottle A to remove traces of oxygen. Where nitrogen
is not readily available, scrubbed carbon dioxide may be
FIGURE 7
AP P ARATUS FOR DETERMI NATI ON OF SO2 BY MONI ER- WI LLI AMS METHOD
used. Connect a dropping funnel K to B by a three-holed
stopper C. Use tube E to connect the upper end of the
condenser to a 100 ml Erlenmeyer flask F, which is followed
by a Peligot tube G. The delivery tube extends to the bottom
of the receiver F. One Peligot tube is sufficient to trap traces
of sulphur dioxide swept through flask F. Use rubber stoppers
throughout. The receiver F contains 25 ml of 3 % hydrogen
peroxide while the Peligot tube contains 5 ml of hydrogen
peroxide. After connecting the apparatus, introduce 200 ml
of water and 20 ml hydrochloric acid into flask B and boil
for a short time in a current of nitrogen. Add 250 g of the
sample directly by means of the dropping funnel with the
aid of as little distilled water as possible. After the introduction
of the sample, boil the mixture for 1 hour in a slow current of
nitrogen, stopping the flow of the water in the condenser
j ust before the end of the distillation. This causes the condenser
to become hot and drives over residual traces of sulphur
dioxide retained in the condenser. When the delivery tube
j ust above the receiver F becomes hot to the touch, remove
stopper J immediately. Wash the contents of the delivery
tube and the Peligot tube into the flask F.
iii. Titrate the solution at room temperature with N/50NaOH
to pH 6 using a pH meter and note the volume of sodium
hydroxide used. Alternatively Bromophenol Blue may be
used as an indicator for the titration. 1 ml of N/50 sodium
hydroxide 0.64 mg sulphur dioxide.
8. The conductivity of solutions of white sugars
a. After thoroughly rinsing the conductivity cell with conductivity
water it is filled with the conductivity water to be used and its
conductance measured. Any batch having a specific conductivity
greater than 1.8 reciprocal megohms is rejected.
b. 5.00 g of sugar are weighed into a 100 ml volumetric flask which
has been rinsed with conductivity water. The sugar is dissolved
and the flask made to volume with conductivity water. The con-
ductivity of the solution is then measured at 20C.
c. If a temperature slightly lower or higher than 20C is used for
measurement, a correction of 2% per degree centrigrade should
be made. For temperatures below 20C, the correction should
be added while for those above 20C, the correction should be
subtracted.
d. The conductivity of the sugar solution minus 0.4 times the conducti-
vity of the water used in making up the sugar solution, gives the
nett specific conductivity of the sugar solution.
e. For the determination of the cell constant, a standard potassium
chloride solution is most convenient. An N/100 KC1 solution
has a specific conductivity of 0.001225 ohm
- 1
cm
- 1
at 18C; 0.001278
at 20C; 0.001413 at 25C; and 0.001552 at 30C. Thus if the
resistance of a cell in N/100 KC1 solution at 20C is found to be
R ohms, the cell constant is 0.001278 x R. The specific conductance
of a solution is found by dividing the cell constant by the resistance
of the solution in the cell.
f. Further information concerning details of instruments and pro-
cedures may be found in Browne & Zerban, Sugar Analysis, New
York, J ohn Wiley & Sons, Inc. (3rd edition), pp. 10211032.
9. Calcium and magnesium (by a modification of the Schwarzenbach
method)
a. Calcium and magnesium: A solution of the product to be analysed
must be prepared as described in chapter VIII, 4, g. A 20 ml
portion of this prepared solution is pipetted into a 350 ml conical
flask and diluted with 80 ml of distilled water. 4 ml of the buffer
and approximately 0.2 g of the indicator are added, and the solution
is titrated with ethylenediaminetetraacetic acid until there is no
further colour change. The concentration of calcium and magnesium
in the solution may be calculated in millimols per litre.
b. Calcium only: For the determination of calcium alone, murexide
indicator is used (see chapter VI, 9, e). In accurate work it is
necessary to restandardize the ethylenediaminetetraacetic acid with
this indicator. 20 ml of the standard calcium solution is diluted
with 60 ml of distilled water and 5 ml of 6 N caustic soda solution.
0.2 g of murexide indicator is added and the solution is titrated
immediately with the ethylenediaminetetraacetic acid solution until
the colour changes from olive-grey to clear blue-green. A blank
determination should be carried out on 80 ml of distilled water
and the blank titre subtracted from the titre obtained in the
standardization. The strength of the titrating solution is calculated
as before. For the actual determination 20 ml of the prepared
solution is used instead of the standard calcium chloride solution
and the titration is carried out as described above. The con-
centration of calcium in the unknown may be calculated in millimols
per litre. The concentration of magnesium is found by subtracting
the calcium concentration from the total concentration of calcium
and magnesium found as above. To convert millimols per litre
to milligrams of CaO per litre, multiply by 56.08; to milligrams of
MgO per litre, multiply by 40.32.
10. Moisture
See special directions for each material in chapter VIII.
11. pH
The pH of solutions is best determined by glass electrode pH meters,
which are strongly recommended.
12. Titrated acidity or alkalinity
The determination of pH has largely superseded the measurement of
acidity by titration. Whereas pH gives the effective acidity or hydrogen
ion concentration, the titration method gives the total acidity or alkalinity.
The titration of acid juices (diluted if necessary) is carried out with
N/10, N/28, or N/32 Na OH using phenolphthalein as indicator. The
results are expressed as milligrams CaO or SO
2
(where acidity is due to
SO
2
) per litre.
Alkaline juices are titrated with N/10 or N/28 HC1 and the results
expressed as milligrams CaO per litre of juice.
13. Sulphated ash
Weigh out into a platinum or porcelain dish 525 g of the material
depending on its ash content. Add 25 to 30 drops of concentrated
sulphuric acid. Heat gently until carbonized, then ignite in an oxidizing
atmosphere and muffle at 550C. Cool and add a few drops of concen-
trated sulphuric acid to moisten the ash thoroughly. Heat gently over a
flame to drive off the excess acid and then ignite for one hour in the
muffle at 800C. Cool and weigh. Results should be expressed as per-
centage sulphated ash without deduction.
14. Test for traces of sugar in waters (Skarblom test)
A test tube approximately 10 mm in diameter and 80 mm in length is
filled with a sample of the water and inverted for a few seconds, allowing
most of the water to drain. Upon replacing the test tube in an upright
position approximately 0.2 ml of water will accumulate in the bottom
of the tube. To this is then added one to two drops of 4% alcoholic
alpha-naphthol solution followed by 15 to 20 drops of concentrated
sulphuric acid. On mixing the contents of the tube by shaking, the
development of a violet colour within 30 seconds is indicative of the
presence of sugar.
CHAPTER VI I I
ANALYS I S OF P ROD UC TS
a. Sucrose % cane: The method used to determine sucrose % cane
depends mainly on the size of the parcel of cane to be analysed.
i. GENERAL FACTORY M ETHOD : The weight of sucrose
in a quantity of cane crushed in a period which begins and
ends with an empty mill train is determined by adding the
weights of sucrose in the mixed j uice and the bagasse produced
from that quantity of cane. This method is generally used by
the factories to assess the weight of sucrose in cane crushed
in a weekly period. The method is also applicable for shorter
periods but the results are less accurate owing to the difficulty
of assessing the weights of mixed juice and bagasse corres-
ponding to a relatively small quantity of cane.
ii. J A VA R A T I O ME T H O D : The percentage of sucrose in an
individual consignment of cane is assessed by a different
method. The consignment is crushed and the sucrose (po1)
percentage of the first expressed j uice is determined. Sucrose
% cane is found by multiplying sucrose % first expressed juice
by the so-called Java ratio. This factor is the average ratio
of sucrose % cane to sucrose (pol) % first expressed juice
determined for the weekly period in which the consignment is
crushed. One of the drawbacks of this method is that the
juice content of the cane of the individual consignments is
not taken into account. The method is applied for cane
payment purposes.
iii. T E S T MI L L A N A L Y S I S : Owing to the considerable varia-
tion in the composition of the units constituting a parcel of
cane, a satisfactory method of assessing its sucrose content
by obtaining a representative sample has not yet been found,
in spite of extensive attempts carried out in many countries
including South Africa.
The following test mill analysis of a sample is carried
out when the greatest accuracy is not required. The sample,
after being weighed, is crushed in a test mill. Usually, only
the weight of the bagasse produced is determined and the
weight of the juice is calculated as the difference between the
weight of the cane and the weight of the bagasse. If facilities
exist for the weighing of both bagasse and j uice this should
be done. Any shortage from the total weight of the cane is
then divided between the bagasse and the j uice in the ratio
of 1:2.
The juice is analysed in the ordinary way for brix and
pol (sucrose)see under Mixed juice, chapter VIII, 5; the
analysis of the bagasse however is more complicated.
The bagasse is shredded or chopped, the operation being
conducted as quickly as possible to avoid loss of moisture.
The pol is then determined as under Final bagasse, altering
the amount of water taken to allow for the weight of fibre
in bagasse, so as to give an approximately half normal
solution.
N.B. In the case of chopped bagasse, care should be taken that the
final sample is representative of the trash, rind and pith originally present.
Then pol % cane =
Fibre % cane =
where Fibre % bagasse = Dry matter % bagassebrix %
bagasse
and brix % bagasse = X 100.
This method is generally used by the factories to assess the
fibre percentage of the cane crushed in a weekly period.
ii. D I R E C T M E T H O D : The fibre percentage of a sample of
50-100 lb. of cane can be determined with sufficient accuracy
as follows: The sample is sub-sampled as described in
chapter V, 2, b. The sub-sample is passed through a suitable
laboratory disintegrator or shredder and all the shredded
material is collected in a large bucket. When the material
has been well mixed 100 g are weighed out in duplicate into
tared 500 ml beakers. The samples are transferred quanti-
tatively to strong linen bags which are then tied with string.
The bags are placed in briskly boiling water for an hour and
X 100.
b. Fibre % cane
i. GE N E R A L F ACTO R Y ME T HO D: The fibre percentage of
a quantity of cane crushed in a period which begins and ends
with an empty mill train is determined by substituting the
relevant data in the expression,
then in cold running water for another hour. During the
second hour the bags should be squeezed at intervals. Finally
the bags are pressed to eliminate surplus water and are dried
at 110-130C to constant weight. The bags are cooled in a
desiccator before weighing. The fibre is then removed from
the bags and the bags are weighed empty. The percentage of
fibre in cane is found by subtracting the weight of the empty
bag from the weight of the bag + fibre in each case.
iii. I ND I RECT M ETHOD : If an experimental mill is available,
the fibre percentage of a sample of cane can be assessed by
a method similar to that described in 1, b, i above. The
weighed sample is crushed and the purity of the expressed
juice and the weight, pol and moisture content of the bagasse
is determined. Pol % bagasse and moisture % bagasse are
determined by the methods described under 2, a and 2, b
below. The method of calculating the final result is similar
to that described in 1, b, i above.
2. Final bagasse
a. Pol % bagasse: Since the error made is insignificant, sucrose %
bagasse is generally assumed to be equal to pol % bagasse and this
latter value is determined. The apparatus for the determination of
pol in bagasse is described in chapter IV, 2, n. 520 g of unchopped
bagasse are weighed out into a digester and 3,775 g of hot water
containing 80 ml of a 5 % sodium carbonate solution are added.
These quantities have been selected so that the resulting extract is
a half normal solution, as explained below.
The average moisture content of Natal bagasse being 53 % and its brix content
being 3.25%, its average fibre content F is 43.8%. Assuming 30% brix-free
water to be present, the amount of juice in bagasse available to mix with the
water added is:
520 x = 225 g (approximately 225 ml)
hence:
4000 225 3775 ml water required to bring the extract volume to
4000 ml.
The perforated plate is placed on the bagasse and pressed below
the surface of the liquid. The cover and condenser are attached and
the water is brought to the boil. After boiling continuously for one
hour, a sample of the solution is withdrawn and cooled to room
temperature. It is clarified with the minimum amount of powdered
lead sub acetate necessary for clarification and polarized in a 400 mm
tube. The reading gives the percentage pol (sucrose) in bagasse
directly.
b. Moisture % bagasse: 100 g of bagasse are weighed into trays
20 cm by 20 cm by 2 cm made with suitable gauze bottoms and
dried for 8 hours at 100-105C.
Although a normal drying oven can be used, a Spencer type
oven is recommended. In order to reduce the time required for an
analysis, a special type of oven in which heated air is blown through
the sample placed on a tray provided with a metal gauze bottom
is used in some factories. Special care is required to ensure that
fine particles are not blown out of the tray and that the openings
of the gauze are not blocked. Where greater accuracy is required,
samples of 1000 g must be used for the analysis. Apparatus for
this purpose is on the market.
3. Bagaci l l o
A rough test to assess the value of bagacillo as a filter aid for use with
rotary vacuum filters.
One hundred grams bagacillo are dried for 4 hours at 105C. The dried
sample is sieved on an 8 inch diameter 20 mesh Tyler screen. Sieving is
carried out manually for 4 minutes using a rotary motion only. The
weight of bagacillo passing through the screen is expressed as a percentage
of the weight of the dried sample. The bagacillo may be classified as
follows:
4. All juices other than mixed juice
a. Brix: Brix is determined as described in chapter VII, 3.
b. Pol: Normally the method given in chapter VII, 4, a is used.
Otherwise the method in chapter VII, 4, b may be used.
c. Reducing sugars: A solution of juice should be prepared so that
15-50 ml will be used in the titration. With a j uice containing
0.6 to 0.7 % of reducing sugars, 50 ml may be pipetted into a 200 ml
flask and the solution made up to volume. This solution is titrated
against Fehling's solution in the manner described in chapter
VII, 6, a. When the sucrose content of the solution is known, the
concentration of reducing sugars per 100 ml solution is found
from the appropriate column in Table IV, interpolating if necessary.
Percentage of reducing sugars in juice =
x 100.
d. Acidity or alkalinity: See chapter VII, 12.
e. Sulphur dioxide: 10 ml of a sample of sulphited juice or 50 ml of
clarified juice are used for the determination of sulphur dioxide by
the iodine method (see chapter VII, 7, a). A 10 ml measuring
Percentage passing 20 mesh
90
85
80
Rating
Excellent
Satisfactory
Minimum requirement
X 100.
cylinder or a pipette with a large tip should be used for measuring
out sulphited j uice. Millilitres of iodine solution (N/32) used are
multiplied by 100 (when 10 ml of the sample were taken) or by 20
(when 50 ml of the sample were taken) to obtain the concentration
of sulphur dioxide in milligrams per litre. If the volume of iodine
required is abnormally large, an N/16 solution of iodine may be
used. In this case the factor becomes 200 (when 10 ml of the sample
were taken) for sulphited juice.
f. pH: See chapter VII, 11.
g. Calcium and magnesium: The following procedure may be used to
prepare either mixed or clarified juices for the titration. Approxi-
mately 200 ml of juice are treated with 2 g of basic lead acetate and
the precipitate filtered off. A fast, calcium-free filter paper such as
Whatman No. 4 should be used. The filtrate is collected in a dry
350 ml Erlenmeyer flask and heated to 60C. The flask is fitted
with a rubber stopper through which pass a delivery and an exit
tube. Hydrogen sulphide from a Kipps apparatus is passed through
the solution for 30 seconds (in a fume-cupboard), then the exit tube
is clamped and the flask left for 3-5 minutes with occasional shaking
under pressure of hydrogen sulphide. After filtering through a
fast, calcium-free filter paper, an aliquot is tested with potassium
iodide solution to ensure complete removal of lead. If a yellow
precipitate forms, the treatment with hydrogen sulphide must be
repeated. 20 ml of the cooled filtrate is measured out in duplicate
from a burette or pipette into conical flasks. The titration is carried
out as described in chapter VII, 9, a and 9, b.
5. Mixed jui ce
a. Brix: As described in chapter VII, 3.
b. Pol: The pol of mixed juice should normally be determined using
the method given in chapter VII, 4, a. Sometimes, for example,
when juice contains much suspended matter (clay) it is advisable to
use the method given under chapter VII, 4, b.
c. Clerget sucrose by the Jackson and Gillis method IV
i. The cooled sample of mixed j uice is brought into the
laboratory and thoroughly mixed. The density of the hourly
sample is determined in the usual manner with a brix hydro-
meter. A sub-sample from each hourly sample is added to a
wide-mouthed glass-stoppered bottle. The weight of each
sub-sample must always be in the same proportion to the
weight of j uice recorded by the factory mixed juice scales
during the period in which the sample was collected. Dry
basic lead acetate is added to the composite sample with
every sub-sample at the rate of 1 g per 100 ml of j uice. The
amount of sub-sample and the weight of basic lead acetate
added must be carefully controlled. At the end of four hours
the composite sample is shaken and filtered.
ii. Two 50 ml portions are pipetted into 100 ml sugar flasks.
The sucrose determination is carried out as described in
chapter VII, 5, a.
iii. CALCULATI ON: The formula given in chapter VII, 4, a
shows how to convert the saccharimeter reading into the pol
(apparent sucrose content) of the solution analysed. A similar
formula (or Schmitz's table) should be used to convert the
readings Dr and Ir into P
D
and P
I
, i.e., the readings which
would have been obtained if a normal weight solution of the
juice had been analysed. To convert the " normal" readings
P
D
and Pj into the sucrose percentage of the juice, the following
formula should be used when the Jackson & Gillis method IV
has been followed:
where t = the temperature in C of the invert solution at the
time of polarization and m = the total weight in grams of
dry substance in 50 ml undiluted juice and may be calculated
using the formula:
For routine purposes it is recommended to calculate the divisor
by the use of Tables Va and Yb. Table Va gives the sum
of the first two terms of the divisor as a function of the
corrected brix before dilution whilst Table Vb gives the
temperature correction.
Alternatively Dr and Ir are converted into S' using a
formula similar to the one used to calculate S. Then S' is
converted into S (the sucrose percentage of the juice) either
by applying the formula given in chapter VII, 4, a or by
using Schmitz's table (Table III).
The divisor of this formula can also be found by using
Tables Va and Vb.
This method of calculating S' from Dr and Ir and
correcting S' for normality is generally used in the Natal
sugar industry and shall be used for cane payment purposes.
N.B. In the direct pol ( Home' s dry lead) method a 200 mm tube is used,
but in the double polarization method 400 mm tubes must be used to
take account of the dilution (50 to 100 ml) of the clarified juice.
1963 63
Example: It is assumed that the four hourly samples are of equal weight.
Otherwise a weighted average must be used when calculating the brix
of the sample.
Sample
1st hour
2nd
3rd
4th
Average
Observed Brix
18.40
19.25
17.50
17.95
Temperature
17C
19C
21C
21C
Corrected Brix
18.24
19.20
17.56
18.01
18.25
1 i
Calculation of S':
Temperature at time of Polarization: 22C
Dr: 60.2
Ir: - 18.3
Dr - I r : 78.5
Divisor corrected for m (from Table Va) : 132.37
Correction for t (from Ta le Vb) : 1.00
Corrected divisor: 131.37
d. Clerget sucrose by the invertase method
i. Catch samples should be clarified by adding dry lead sub-
acetate at the rate of 1 g per 100 ml and filtering. Composite
samples should be prepared as discussed in 5, c, i above. The
filtrates are de-leaded by adding a minimum quantity of
anhydrous potassium oxalate and filtering and are analysed as
described in chapter VII, 5, b, iii.
ii. Since 50 ml of the undiluted solution is diluted to 100 ml,
readings should be taken in 400 mm tubes, provided that the
solutions are sufficiently light in colour to permit accurate
readings. If 200 mm tubes are used, readings should be
multiplied by 2. The reading of the invert solution should be
corrected for the optical activity of the invertase solution.
iii. Calculation: The formula used to calculate S' from Dr and
Ir is:
S'
=
100 (Dr Ir)
132.1 + 0.0833 (m 13) 0.5 (t 20 )
where t = the temperature of the invert solution at the time of
polarization and m = the total weight in grams of dry sub-
stance in 50 ml undiluted juice.
S' is converted to S (the sucrose percentage of the original
solution) by the formula given in the example above or by
referring to Schmitz's table (Table III).
e. Reducing sugars: Reducing sugars should be determined on a
four-hourly composite sample of mixed j uice which has been
preserved with pulverised mercuric chloride (250 mg/litre). This
composite sample should be prepared in accordance with the
principles given under 5, c, i above but substituting pulverised
mercuric chloride for basic lead acetate. The sample which has
been preserved with basic lead acetate for sucrose analysis should
not be used since this practice often leads to low results.
It is not necessary to clarify the sample but where it contains
sand or other suspended matter which is liable to block the delivery
jet of the burette, it is advisable to filter or screen the sample before
proceeding with the analysis.
The Lane & Eynon method of analysis is followed. A portion
of the sample is pipetted off and suitably diluted so that 15-50 ml
will be used in the titration. (With an average mixed juice containing
0.6- 0.7% reducing sugars, 50 ml may be pipetted into a 200 ml
volumetric flask and made to volume.)
Titrate against 10 ml Fehling's solution in the manner described
in chapter VII, 6, a. The percentage of reducing sugars is calculated
as described above for juices generallysee under 4, c above.
f. Calcium and magnesium: The same procedure is used for mixed
juice as for other juicessee under 4, g above.
g. A vailable phosphate
i. Sufficient mixed juice is filtered to obtain about 20 ml of fairly
clear filtrate. 10 ml of this filtrate is pipetted into a 200 ml
volumetric flask and made up to volume. An aliquot of this
(usually about 20 ml depending on the amount of P
2
O
5
expected in the juice) is pipetted into a 100 ml flask. The
solution is diluted to approximately 70 ml with distilled
water and then 20.0 ml of ammonium molybdate solution is
pipetted into the flask, followed by 10.0 ml of the reducing
solution, after which it is made to the mark.
ii. The intensity of the blue colour developed is measured on a
suitable absorptiometer or spectrophotometer 15 minutes
after addition of the reducing solution. The equivalent
amount of P
2
0
5
is determined from a standard graph drawn
beforehand, using solutions of accurately known P
2
O
5
content.
When the degree of accuracy required is not great, the
colour developed may be compared visually with standards of
known P
2
O
5
content using various volumes of diluted standard
instead of j uice for colour development. When the equivalent
amount of P
2
O
s
in the unknown has been ascertained, either
from the standard graph or by visual matching, it is multiplied
by the dilution factor to obtain the P
2
O
5
content of the original
juice.
Example: 10 ml of filtered juice was diluted to 200 ml and 10 ml of this
solution was used for development of the blue colour the intensity of
which was found to be equivalent to 0.2 mg P
2
O
5
The P
2
O
5
content of the original mixed juice = 0.2 x 20 mg/10 ml juice
= 0.2 x 20 x 100 mg/litre
juice
= 400 mg/litre of juice.
6. Syrup
A quantity of the sample is accurately diluted with twice its weight of
water and this diluted sample is used for all determinations except the
measurement of pH.
a. Brix: As described in chapter VII, 3. The corrected brix multiplied
by 3 represents the brix of the original sample.
b. Pol: By method a in chapter VII, 4, a. The value of the pol found
from Table III, using the uncorrected brix of the diluted sample,
must be multiplied by 3 to give the pol of the original sample.
c. Reducing sugars: 50 ml of the diluted sample is made up to 200 ml
and titrated against Fehling's solution as described in chapter VII,
6, a. The percentage of reducing sugars found for the diluted
sample must be multiplied by 3 to give the percentage of reducing
sugars in the original sample.
d. Sulphur dioxide: 50 ml of the diluted sample is used for the
determination of sulphur dioxide by the iodine titration method as
described in chapter VII, 7, a. Millilitres of N/32 iodine solution
required multiplied by 60 gives the concentration of SO
2
in
milligrams per litre in the original sample.
e. Hydrogen ion concentration ( pH) : The pH of syrup is usually
determined on the original sample. If the sample were diluted prior
to measurement a higher pH value would often be found.
7. Filter cake
a. Pol: 25.5 g of the sample are triturated with water in a mortar
and washed with water into a 200 ml Kohlrausch flask. The volume
of liquid is made up to the 200 ml mark and the minimum quantity
of dry basic lead acetate needed for clarification is added. The
contents of the flask are thoroughly mixed by shaking, filtered, and
polarized in a 400 mm tube. The reading gives the sucrose %
filter cake directly.
b. Moisture: For moisture determination 50 g of the sample are
dried to constant weight in a flat-bottomed dish at a temperature
not exceeding 105C.
8. Massecuites
From every strike a sample is diluted accurately with four times its weight
of water. Care should be taken that all crystals of sugar are dissolved.
If hot water has been used for this purpose, the solution should be cooled
to about room temperature before proceeding with the analysis.
a. Brix: See chapter VII, 3.
b. Pol: See chapter VII, 4, a.
For both brix and pol, all readings must be multiplied by 5.
c. Crystal content: The crystal content of a massecuite may be calcu-
lated from the analyses of the massecuite and its mother liquor
(molasses). It is possible to use the true sucrose (or pol), dry solids
(or brix) or true purity (or apparent purity) data, but the use of
true sucrose or true purity data is recommended.
Brix should never be used as the basis of calculation.
The formula using sucrose data is as follows:
where C = crystal % massecuite
Smass = sucrose % massecuite
Smol = sucrose % mother liquor.
The formulae for use with pol or dry solids data are analogous to
that given above for use with sucrose data.
When purity is used as the basis of calculation, the formula is
where C = crystal % massecuite
Pmass = purity of massecuite
Pmol = purity of mother liquor
D.S.mass = dry solids % massecuite.
9. Molasses (excluding final molasses) and wash
The sample should represent as nearly as possible run-offs from individual
massecuites.
a. Brix: A quantity of the material is diluted accurately with four
times its weight of water. The brix of the solution is determined as
described in chapter VII, 3.
Brix of material = corrected brix of solution x 5.
b. Pol {for stocktaking): Determined on a further portion of the
diluted solution. Pol of material = pol of solution x 5.
10. Final molasses
a. Brix: A quantity of the material is dissolved in six times its weight
of distilled water and the brix determined as in chapter VII, 3.
The reading multiplied by 7 = brix of the original sample.
b. Dry substance: Approximately 40-50 g acid washed and ignited
quartz sand (about 40-100 mesh) in an aluminium dish together
with a small glass stirring rod are dried in an oven and cooled in
a desiccator. The dish shall have a tightly fitting lid, be 8 cm in
diameter, 1.5 cm in height and be made of 24 gauge aluminium. The
length of the glass stirring rod shall be slightly less than the diameter
of the aluminium dish.
About 20 g molasses are weighed accurately into a tared
weighing bottle provided with a stirrer and closely fitting lid.
Approximately 80 g water are added, the mixture stirred until homo-
geneous (a mechanical stirrer is recommended), the lid replaced and
the weighing bottle and contents reweighed.
From this diluted molasses a sample of approximately 10 ml
is pipetted into the weighed aluminium dish which is then reweighed.
The diluted molasses is mixed intimately with the sand using the
glass rod which, after mixing, is allowed to remain in the dish.
The International Commission for Uniform Methods of Sugar
Analysis specifies that the drying be carried out at a temperature
not exceeding 70C, preferably 60C, under a pressure not exceeding
5 cm Hg until successive weighings at two-hourly intervals do not
differ by more than 0.5 mg. The dried sample is cooled in a
desiccator before weighing.
Sucrose
i. THE J ACK SON & GI LLI S METHOD I V : Weigh out
32.5 g of molasses. Dissolve and make up to the mark with
water in a 250 ml flask. Part of this solution is used for the
determination of reducing sugars as described in 10, d below.
To the remainder add sufficient dry lead sub-acetate for clari-
fication (usually about 6 g), shake well and allow to stand for
a few minutes before filtering. To the filtrate add the minimum
of anhydrous potassium oxalate necessary for de-leading
(usually about 4 g), shake well and again filter. Now pipette
50 ml portions into 100 ml flasks and proceed with either
method a or b of chapter VII, 5. The readings are made in
200 mm tubes. If the solution is very dark, add a pinch of
zinc dust for decolourizing.
1962 Laboratory Manual for S. Af r . Sugar Factories
The actual saccharimeter readings multiplied by 4 in
each case will give PD and PI. To convert ( P D PI) into S,
the modified Clerget Formula in 5, c, iii (for acid inversion)
or 5, d, ii (for invertase inversion) above, should be used,
where m is the weight in grams of dry substance in the 50 ml
of solution taken for inversion. However, since the accuracy
of the sucrose determination in final molasses by the Jackson
and Gillis method is not very great, no significant error is
made if a constant value of 132.0 is taken for the divisor
when t is within the limits 19 to 21C.
When t is either more than 21C or less than 19C the
value 132.0 shall be corrected for t in the normal way. The
above simplification is permitted only if a sample of ordinary
final molasses is analysed. In other cases the usual concentra-
tion correction shall be calculated and applied, and if Table
Va is used the "Corrected brix before dilution" is the brix of
the half normal solution of the sample,
ii. THE CHEMI CAL M ETHOD * , USI NG I NV ERTASE: 26 g
of final molasses are weighed out and transferred quantita-
tively to a 200 ml volumetric flask. After making to volume
this solution is used for the determination of reducing sugars
before and after inversion as follows:
a. 20 ml of the filtrate are pipetted into a 200 ml volumetric
flask and made to volume. This solution is titrated against
10 ml of Fehling's solution for the determination of reducing
sugars.
b. 50 ml of the filtrate are pipetted into a 100 ml Erlenmeyer
flask and diluted to approximately 80 ml and brought to
pH 4.7 0.2 by the addition of a pre-determined volume of
glacial acetic acid. To this solution is added the invertase, the
appropriate quantity of which was determined by the method
given in chapter VII, 5, b, ii. If the concentrate is of normal
activity 2.5 ml are added, otherwise a pro rata volume. The
flask is placed in a water bath at 57-58C for 15 minutes with
occasional shaking. After cooling the solution is transferred
quantitatively to a 500 ml volumetric flask and made to
volume. This solution is titrated against 25 ml of Fehling's
solution for the determination of reducing sugars after
inversion.
The amount of reducing sugars found after inversion
gives the percentage of total sugars present. To calculate the
sucrose percentage both reducing sugar concentrations are
expressed as a percentage of the original sample. The per-
centage reducing sugars before inversion is deducted from the
* Especially for dark-coloured molasses, this method yields more
accurate results than the Jackson & Gillis method.
1963 69
total sugars and the difference multiplied by 0.95. This is
necessary to compensate for the fact that 95 parts of sucrose
on hydrolysis yield 100 parts of reducing sugars.
d. Reducing sugars: Pipette 20 ml of the diluted solution prepared for
the determination of sucrose (10, c above) into a 200 ml volumetric
flask and make to the mark with distilled water. Titrate this
solution, which is a 1.3% solution of original molasses, against
Fehling's solution as described in chapter VII, 6, a. From the
column for 0.5 g sucrose per 100 ml in Table IV obtain the
concentration of reducing sugars per 100 ml and express this
concentration as the percentage of reducing sugars in original
molasses.
e. Total sugars: As a gauge for the value of final molasses to secondary
industries, the percentage of total sugars is often calculated. The
percentage is found by adding the percentage of reducing sugars
and 1.05 x the percentage of sucrose.
f. Sulphated ash: As described in chapter VII, 13. About 5 g is
normally adequate for ashing.
11. Sugar s
a. Pol
i. The preparation of the solution of the sugar and the reading
of the saccharimeter should be carried out at or as near as
possible to 20C. The time of the day for the analysis of
composite samples should be chosen accordingly. If it is not
possible to work at 20C the volume of the solution in the
100 ml flask should be completed at the same temperature at
which the saccharimeter is read and the reading should be
corrected for the deviation of the temperature from 20C.
For every degree above 20C, 0.03S should be added to the
pol; for every degree below 20C, 0.03S should be deducted
from the pol.
ii. Dissolve the normal weight of the sugar in distilled water in
a 100 ml volumetric flask. Dilute to approximately 80 ml
and add 1.0 ml of lead sub-acetate solution. Mix the solution
by swirling and add water until the volume is roughly 96 ml.
Thoroughly mix and then wash down the sides of the flask
until the volume is approximately 99.5 ml. Disperse any
bubbles which have collected at the surface with one drop of
diethyl ether. Dry the inside neck of the flask above the
solution level with rolled filter paper and make the volume to
exactly 100 ml by adding water from a fine dropper. Mix the
solution thoroughly and allow to stand for 5 minutes. Filter
through an 18.5 cm fluted filter paper contained in a plain
stemless funnel, pouring all the contents of the flask into the
70 1963 Laboratory Manual for S. Af r . Sugar Factori es
paper. Immediately cover the funnel with a cover glass.
Discard the first 10 ml of filtrate and collect a further 30 ml
of filtrate for polarization in a 200 mm tube at 20C. It is
preferable to use a j acketed tube to prevent warming by
the hands.
All operations after weighing should be carried out at
a temperature as near 20C as possible. The funnel should
be sufficiently large to prevent the paper projecting above it
and during filtration should remain covered with a clock glass.
b. Reducing sugars by the Luff-Schoorl method: Weigh out accurately
20 g of the sample and transfer to a 100 ml volumetric flask. Dissolve
in distilled water and make up to volume. Shake well. (Normally
no clarification of the solution is required.) In the case of refined
and mill-white sugars, accurately pipette a 25 ml aliquot of the
solution into a 500 ml Erlenmeyer flask containing 25 ml of the
Luff solution. For raw sugars a 25 ml aliquot is normally satisfactory
but for raw sugars containing a high percentage of reducing sugars
it may be necessary to decrease the aliquot taken. In such a case
the volume must be made up to 25 ml with water, e.g. if a 10 ml
aliquot is taken 15 ml water must be added. To prevent boiling
over add a few pieces of washed and ignited unglazed porcelain.
Fit an upright condenser to the flask which rests on a copper gauze
over a circular opening with a diameter slightly less than that of
the bottom of the flask. Heat the flask so that the solution boils
within 3 minutes and continue boiling for exactly 5 minutes longer.
Cool the solution rapidly in running water, taking care that the
precipitated cuprous oxide does not come into contact with the
air. Immediately add 15 ml of potassium iodide solution and then
slowly, with careful swirling, 25 ml of sulphuric acid solution. As
soon as the evolution of carbon dioxide ceases titrate the liberated
iodine with the N/10 thiosulphate solution. When the end point is
approached add I ml of the starch solution. Carry out a blank
determination using 25 ml of distilled water in place of the sugar
solution. Refer the difference between the volume of N/10 thio-
sulphate solution required by the blank and the test, corrected for
normality, to Table VI and calculate the percentage reducing
sugars in the sample.
c. Colour of white sugars
i. SAM P LE P REP ARATI ON: Hot distilled water at a tempera-
ture of 90-100C is added to the weight of sugar required to
prepare a solution of a concentration of 50 0.2% refracto-
meter solids. The sugar-water mixture is stirred gently to
bring the sugar into solution. Cool the solution to about
room temperature before measurement. No filtration should
be made nor should the pH be adjusted.
N.B. Stainless steel or glass bottles or beakers should be used to prepare
the solution. Aluminium beakers should not be used as they introduce
turbidity.
ii. M EASUREM ENT: The solution should be measured in a
10 cm cell using a suitable spectrophotometer at wavelengths
420 my. and 720 my.. The cell should be located as close to
the photocell as possible.
iii. REFERENCE STAND ARD : The reference standard should
be a 50 0-2% solids colourless sucrose solution. For
practical purposes the reading with a colourless sugar solution
may be correlated with a secondary standard such as distilled
water or air and a balance point established on the scale
which will give the equivalent of a colourless sucrose solution.
d. Sulphur dioxide: For raw and refined sugars either the rapid method
or the Monier-Williams method is usedsee chapter VII, 7, b
and 7, c.
e. Moisture: For white sugars and raw or similar type sugars take 25
and 10 g of sample respectively. Accurately weigh the sample of
the sugar into a polished aluminium dish provided with a tight-
fitting cover. The dish shall be 8 cm in diameter, 1.1 cm in height
and made of 24-gauge aluminium sheet. Dry in an oven at 105C
for 3 hours. Replace the cover of the dish, cool in a desiccator
and weigh.
f. Sulphated ash: See chapter VII, 13.
g. Conductometric ash {for mill white and refined sugars): The gravi-
metric determination of bisulphated ash on a refined sugar
containing less than 0.03% ash requires the use of a precision
analytical balance, expensive platinum ware and very careful
analytical technique. A much simpler and often more reproducible
method is to measure the electrical conductance of a solution of
sugar which will then usually bear a direct relationship to the
soluble ash in the sugar. Electrical conductance is the reciprocal
of the electrical resistance and in the case of sugar solutions, specific
conductivity may be defined as the reciprocal of the resistance of
a column of liquid 1 cm long and having a cross-sectional area of
1 cm
2
. It is usually reported as reciprocal megohms but may be
converted to conductivity ash by multiplying by a factor. The
measurement of the conductivity of white sugar in solution at
20C is described in chapter VII, 8.
h. Grain size distribution: Refined or mill white sugars may be
screened as received but with raw sugars it is necessary to remove
the film of molasses surrounding the crystals prior to screening.
This may be achieved using the method described in I.C.U.M.S.A.,
10 (1949) 27. Full details of this method are given below.
EQ UI P M ENT
i. Erlenmeyer flask, 250 ml capacity, wide mouth ( l i in.
diam.), with a No. 8 solid rubber stopper. A wide-
mouth bottle of about the same capacity may be used,
ii. A strainer stopper made from the following: No. 7
rubber stopper, with central hole 3/4 in. to 7/8ths in. diam.;
rubber tubing 11/2 in. wide (used with carbon filter);
disc of 100-mesh wire cloth l1/4 in. diam. Cut a band
1 in. wide off rubber tubing. Work this over small end
of rubber stopper leaving about 3/16ths in. projecting
beyond the end. Peel back projecting tubing, place
metal cloth disc on small end of stopper and hold in
place by slipping over it the projecting part of rubber
tubing,
iii. Filter flask, 500 ml capacity, with side outlet.
REAGENTS
i. Absolute methanol,
ii. 95 % by vol. methanol, prepared by diluting 95 ml
absolute methanol to 100 ml.
iii. 90 % by vol. methanol, prepared from absolute methanol
or from 95 % methanol (100 ml to 5 ml H
2
0) .
iv. Diethyl ether.
P ROCED URE
Put 100 g raw sugar in Erlenmeyer flask; add 100 ml 90%
methanol; stop with solid stopper; shake contents to mix;
1962 73
allow to soak for 1 hour, shaking every 15 min. a few
times to mix. Then take flask in one hand, with the index
finger over stopper and the flask resting in palm of hand;
rock flask back and forth, causing sugar to be sluiced from
one end to the other. Do this for 2 min. making 120 cycles
per min. Let sugar settle and, with flask inclined, tilt to wash
crystals from around stopper.
Remove solid stopper; replace by strainer-stopper ii,
loosely inserted. Pour off methanol through strainer, finally
inverting Erlenmeyer flask over filter flask to drain into latter.
Apply suction to drain crystals and extract as much methanol
as possible.
Add 50 ml 95 % methanol, pouring some through
loosened strainer-stopper; then remove stopper and pour
remainder of methanol on stopper to wash crystals into
flask. Stop with solid stopper and shake for 2 min. as before,
etc. Repeat with 50 ml 95 % methanol three times, making
in all four applications of the 95 % methanol.
Then wash crystals in the same manner with four
50 ml portions of diethyl ether, shaking for 1 min. instead of
2 min. Most of the diethyl ether of the last wash can be
extracted by leaving the Erlenmeyer flask on the filter flask
under vacuum for several minutes.
Spread the washed crystals on a piece of clean paper to
air-dry; the crystals on the sides of the flask need not be
removed. When nearly dry (i.e. when crystals no longer feel
cold and begin to cake), return the sugar to the flask and shake
a few times; spread again on paper for a few minutes. Return
sugar to flask and shake a few times; crystals should now be
free running and dry.
SI EV I NG TEST
For mill white and refined sugars five Tyler standard screens
(10, 14, 20, 28 and 48 mesh) while for raw sugars four Tyler
standard screens (10, 16, 28 and 42 mesh) are used. The
sample for screening is weighed prior to placing on the top
sieve and sifting is carried out for 10 minutes (the Ro- Tap
hand or motor-operated machine is recommended), after
which the weights of the fractions are ascertained. The
weights of the fractions are expressed as percentages of the
total weight of the sugar sifted.
CALCULATI ON OF SP ECI FI C GRAI N SI Z E
The method of calculation given below is that described by
Douwes Dekker in S.A.S.T.A. Proceedings, 26 (1952) 46.
The main criterion calculated from the results of the
sieving test is the specific surface (U) of the material tested.
U is the ratio between the total surface of all particles and the
total surface of the same weight of particles the diameter of
which is 1 cm. The particles are supposed to be spheres. U is
calculated from Zunker' s formula,
in which d
1
= the diameter of the smallest particle
and d
2
= the diameter of the largest particle.
The specific grain size (S.G.S.) is calculated from U by
the simple formula:
In the following table the values for TJ and S.G.S., as
computed from the openings of the Tyler sieves, are given for
the six fractions of a sugar-sieving test. d
1
of the sixth fraction
is assumed to be 0.15 mm. Since the use of three decimals is
not necessary and suggests a false degree of accuracy the
values of U and S.G.S. which are actually used in the computa-
tion of a sugar-sieving test are also given.
First fraction
Second
Third
Fourth
Fifth
Sixth
U
4.712
7.235
10.17
14.37
24.47
48.49
S.G.S.
mm
2.122
1.382
0.983
0.695
0.409
0.206
U S.G.S.
For practical use in
sugar analysis
4.8
7.2
10.0
14.3
25.0
50.0
2.1
1.4
1.0
0.7
0.4
0.2
To calculate the specific grain size of a sugar from the
sieve test results, the weight of each fraction (expressed as a
percentage of the total weight) is multiplied by the corres-
ponding value of U. The products are added and the sum
divided by 100. The quotient is the specific surface of the
sugar tested which, divided into 10 gives the specific grain
size in mm.
Example:
First fraction
Second
Third
Fourth
Fifth
Sixth
Sieve test result, %
1
15
55
26
2
1
U
4.8
7.2
10.0
14.3
25.0
50.0
Product
4.8
108.0
550.0
371.8
50.0
50.0
The values of U for the fractions obtained when the 10,
16, 28 and 42 mesh screens are used are 4.4, 7.9, 13.2, 22.3
and 41.4 respectively.
TABLE I I
Temperature corrections to readings of brix hydrometers (20C)
Temperature
I5C .. .
I6C .. -
I7C .. .
I8C .. .
I9C .. .
2IC .. .
22C .. .
23C .. .
24C . . .
25C . . .
26C .. .
27C .. .
28C . . .
29C . . .
30C . . .
3IC .. .
32C . . .
33C .. .
34C . . .
35C .. .
Hydro-
meter
No. 0
0.21
0.18
0.14
0.10
0.05
0.05
0.10
0.16
0.22
0.28
0.34
0.40
0.47
0.54
0.61
0.68
0.76
0.84
0.92
1.00
Hydro-
meter
No. 1
Subtract
0.23
0.18
0.14
0.10
0.05
Ad d
0.05
0.11
0.17
0.23
0.29
0.35
0.42
0.49
0.56
0.63
0.70
0.78
0.86
0.94
1.03
Hydro-
meter
No. 2
Hydro-
meter
No. 3
From observed percent
0.26
0.21
0.16
0.11
0.05
to observed
0.06
0.12
0.18
0.25
0.32
0.39
0.45
0.52
0.60
0.67
0.75
0.83
0.91
0.99
1 .08
0.29
0.24
0.19
0.13
0.06
percent
0.06
0.13
0.20
0.27
0.33
0.40
0.47
0.55
0.63
0.71
0.79
0.88
0.96
1.04
1.13
Hydro-
meter
No. 4
0.33
0.27
0.21
0.14
0.07
0.07
0.15
0.22
0.30
0.37
0.44
0.52
0.60
0.68
0.76
0.84
0.93
1.01
1.09
1.18
Hydro-
meter
No. 5
0.37
0.30
0.22
0.15
0.08
0.08
0.16
0.23
0.31
0.39
0.47
0.55
0.63
0.71
0.80
0.88
0.97
1.05
1.13
1.22
78 1962
TABLE I V
Table giving mg invert sugar required to reduce 10 and 25 ml of Fehling's solution in the
presence of different amounts of sucrose
ml Sugar
Solution
Required
15 ..
16 ..
17 ..
18 . .
19
20
21 . .
22 ..
23
24
25
26
27 ..
28
29 ..
30
31 . .
32 . .
33 . .
34 . .
35 . .
36 . .
37 ..
38 ..
39 ..
40 . .
41 ..
42 . .
43 ..
44 ..
45 . .
46 ..
47 . .
48 ..
49 ..
50 ..
Og
336
316
298
282
267
255
243
232
222
213
! 205
197
190
184
178
172
166
161
157
152
148
144
140
137
133
130
127
124
121
119
116
114
III
109
107
105
0.5g
335
314
296
280
265
253
241
230
220
211
203
195
189
182
176
170
165
160
155
151
147
143
139
135
132
129
125
123
120
117
114
112
NO
108
106
103
10
mg
the
1g
333
312
295
278
264
251
239
228
219
210
202
194
187
180
174
168
163
158
153
149
145
141
137
134
130
127
124
121
118
116
113
111
108
106
104
102
ml F ehling' s Solution
deducing Sugars per 100
concentration of s
2g
329
309
291
274
260
249
236
225
216
207
198
191
184
178
171
166
161
156
151
147
143
139
135
131
128
125
122
119
116
114
111
109
106
104
103
100
3g 4g
325 ! 322
305
287
271
257
248
233
222
213
204
196
189
182
175
169
164
159
154
149
145
141
137
133
130
126
123
120
117
115
112
110
107
105
103
102
99
301
284
268
254
242
230
220
210
202
194
186
179
173
167
161
157
152
147
143
139
135
131
128
124
121
118
116
113
110
108
105
103
101
100
98
ml so ution
ucrose (g/100 ml)
5g
317
297
280
264
250
238
227
216
207
198
190
183
176
170
165
159
154
149
145
140
136
133
129
126
122
119
116
114
111
108
106
104
102
99
97
95
10g
307
288
271
256
243
231
220
210
200
192
184
177
170
164
159
153
148
143
139
135
131
127
124
120
117
114
III
109
106
103
101
99
96
94
92
90
25g
289
271
255
240
227
217
206
196
187
179
171
164
158
152
147
142
137
132
128
124
121
117
114
111
107
104
102
99
97
94
92
90
88
86
84
82
25 ml F ehling' s
1 Sol
when
is :
0g
824
772
727
687
651
619
589
563
539
1
517
496
477
460
444
428
414
401
389
377
366
356
346
337
328
320
312
304
297
290
284
278
272
266
261
255
251
Jtion
1g
817
766
722
682
846
614
585
559
534
512
492
473
456
440
424
410
397
385
373
363
352
342
333
325
316
308
301
294
287
281
275
269
263
258
252
248
Laboratory Manual for S. Af r . Sugar Factori es
1963 79
TABLE V a
Table giving the divisor, corrected for the brix of the solution, of the formula to be used in
the Jackson & Gillis method IV
Corrected Brix
Before Dilution
0
1
2
3
4
5
6
7
8
9
10
11
12
13
Divisor
131.60
131.64
131.68
131.72
131.76
131.80
131.84
131.88
1 31.92
13!.97
132.01
132.05
132.10
132.14
Corrected Brix
Before Dilution
14
15
16
17
18
19
20
21
22
23
24
25
26
Divisor
132.18
132.23
132.27
132.32
132.36
132.41
132.46
132.50
132.55
132.60
132.64
132.69
132.74
Temperature corrections for
Temp.
( C)
15. 0
15. 1
15. 2
15. 3
15. 4
15. 5
15. 6
15. 7
15. 8
15. 9
20. 0
20. 1
20. 2
20. 3
20. 4
20. 5
20. 6
20. 7
20. 8
20. 9
21. 0
21 .1
21. 2
21. 3
21. 4
21. 5
21. 6
21. 7
21 . 8
21. 9
22. 0
22. 1
22. 2
22. 3
22. 4
22. 5
22. 6
22. 7
22. 8
22. 9
23. 0
Cor r ec-
ti on
2. 50
2. 45
2. 40
2. 35
2. 30
2. 25
2. 20
2. 15
2. 10
2. 05
0. 00
0. 05
0. 10
0. 15
0. 20
0. 25
0. 30
0. 35
0. 40
0. 45
0. 50
0. 55
0. 60
0. 65
0. 70
0. 75
0. 80
0. 85
0. 90
0. 95
1.00
1.05
1. 10
! . 15
1.20
1.25
1.30
1.35
1. 40
1.45
1 . 50
Temp.
( C)
Te
16. 0
16. 1
16. 2
16. 3
16. 4
16. 5
16. 6
16. 7
16. 8
16. 9
Tem
23. 0
23. 1
23. 2
23. 3
23. 4
23. 5
23. 6
23. 7
23. 8
23. 9
24. 0
24. 1
24. 2
24. 3
24. 4
24. 5
24. 6
24. 7
24. 8
24. 9
25. 0
25. 1
25. 2
25. 3
25. 4
25. 5
25. 6
25. 7
25. 8
25. 9
26. 0
T ABL E V b
the divisors for the Jackson & Gillis method for acid
Cor r ec-
ti on
Temp.
( C)
Cor r ec-
ti on
Temp.
( C)
Cor r ec-
t i on
mper at ur e correct i ons t o be added
2. 00
1.95
1.90
1.85
1.80
1.75
1 . 70
1.65
1 . 60
1.55
perat ure
1.50
1.55
1 . 60
1 . 65
1.70
1.75
1.80
1.85
1.90
1.95
2. 00
2. 05
2. 10
2. 15
2. 20
2. 25
2. 30
2. 35
2. 40
2. 45
2. 50
2. 55
2. 60
2. 65
2. 70
2. 75
2. 80
2. 85
2. 90
2. 95
3. 00
17. 0
17. 1
17. 2
17. 3
17. 4
17. 5
17. 6
17. 7
17. 8
17. 9
correcti
26. 0
26. 1
26. 2
26. 3
26. 4
26. 5
26. 6
26. 7
26. 8
26. 9
27. 0
27. 1
27. 2
27. 3
27. 4
27. 5
27. 6
27. 7
27. 8
27. 9
28. 0
28. 1
28. 2
28. 3
28. 4
28. 5
28. 6
28. 7
28. 8
28. 9
29. 0
1.50
1.45
1 . 40
1.35
1.30
1 . 25
1.20
1.15
i . 10
1.05
18. 0
18.1
18. 2
18. 3
18. 4
18. 5
18. 6
18. 7
18. 8
18. 9
1.00
0. 95
0. 90
0. 85
0. 80
0. 75
0. 70
0. 65
0. 60
0. 55
ons to be subtracted
3. 00
3. 05
3. 10
3. 15
3. 20
3. 25
3. 30
3. 35
3. 40
3. 45
3. 50
3. 55
3. 60
3. 65
3. 70
3. 75
3. 80
3. 85
3. 90
3. 95
4. 00
4. 05
4. 10
4. 15
4. 20
4. 25
4. 30
4. 35
4 . 4 0
4. 45
4. 50
29 . 0
29. 1
29. 2
29. 3
29. 4
29. 5
29. 6
29. 7
29. 8
29. 9
30. 0
30. 1
30. 2
30. 3
30. 4
30. 5
30. 6
30. 7
30. 8
30. 9
31 . 0
3 1 . 1
31 . 2
31 . 3
31. 4
31. 5
31. 6
31. 7
31. 8
31. 9
32. 0
4 . 5 0
4. 55
4. 60
4. 65
4. 70
4. 75
4. 80
4. 85
4. 90
4. 95
5. 00
5. 05
5. 10
5. 15
5. 20
5. 25
5. 30
5. 35
5. 40
5. 45
5. 50
5. 55
5. 60
5. 65
5. 70
5. 75
5. 80
5. 85
5. 90
5. 95
6. 00
Temp.
(C)
19. 0
19. 1
19. 2
19. 3
19. 4
19. 5
19. 6
19. 7
19. 8
19. 9
32. 0
32. 1
32. 2
32. 3
32. 4
32. 5
32. 6
32. 7
32. 8
32. 9
33. 0
33. 1
33. 2
33. 3
33. 4
33. 5
33. 6
33. 7
33. 8
33. 9
34. 0
34. 1
34. 2
34. 3
34. 4
34. 5
34. 6
34. 7
34. 8
34. 9
35. 0
inversion
Cor r ec-
t i on
0. 50
0. 45
0. 40
0. 35
0. 30
0. 25
0. 20
0. 15
0. 10
0. 05
6. 00
6. 05
6. 10
6. 15
6. 20
6. 25
6. 30
6. 35
6. 40
6. 45
6. 50
6. 55
6. 60
6. 65
6. 70
6. 75
6. 80
6. 85
6. 90
6. 95
7. 00
7. 05
7. 10
7. 15
7. 20
7. 25
7. 30
7. 35
7. 40
7. 45
7. 50
Mi l l i l i tres
thi osul phate,
N/ 10
8. 00
8. 10
8. 20
8. 30
8. 40
8. 50
8. 60
8. 70
8. 80
8. 90
9. 00
9. 10
9. 20
9. 30
9. 40
9. 50
9. 60
9. 70
9. 80
9. 90
10. 00
10. 10
10. 20
10. 30
10. 40
10. 50
10. 60
10. 70
10. 80
10. 90
I f . 0 0
11. 10
11. 20
11. 30
11. 40
11. 50
11. 60
11. 70
11. 80
11. 90
T ABL E V I ( c ont i nue d)
Milligrams red
1.25 g
sucrose
in
aliquot
24. 10
24. 40
24. 70
25. 00
25. 30
25. 65
25. 95
26. 25
26. 55
26. 85
27. 20
27. 50
27. 80
28. 10
28 40
28. 70
29. 00
29. 30
29. 60
29. 90
30. 25
30. 55
30. 85
31. 20
31. 50
31. 80
32. 10
32. 45
32. 75
33. 05
33. 40
33. 70
34. 00
34. 35
34. 65
34. 95
35. 30
35. 60
35. 90
36. 20
sugars
2 - 5 g
sucrose
in
al i quot
23. 55
23. 85
24. 15
24. 45
24. 75
25. 10
25. 40
25. 70
26. 00
26. 30
26. 65
26. 95
27. 25
27. 55
27. 85
28. 20
28. 50
28. 80
29. 10
29. 40
29. 75
30. 05
30. 35
30. 70
31. 00
31. 35
31. 65
32. 00
32. 30
32. 60
32. 95
33. 25
33. 55
33. 90
34. 20
34. 55
34. 85
35. 15
35. 50
35. 80
ucing
5 g
sucrose
in
al i quot
23. 00
23. 30
23. 60
23. 90
24. 20
24. 50
24. 80
25. 10
25. 40
25. 70
26. 00
26. 30
26. 60
26. 90
27. 20
27. 50
27. 80
28. 10
28. 40
28. 70
29. 05
29. 35
29. 65
29. 95
30. 25
30. 60
30. 90
31. 20
31 . 50
31. 80
32. 15
32. 45
32. 75
33. 05
33. 40
33. 70
34. 00
34. 35
34. 65
34. 95
Mi l l i l i tres
thi osul phate,
N/ 10
12. 00
12. 10
12. 20
12. 30
12. 40
12. 50
12. 60
12. 70
12. 80
12. 90
13. 00
13. 10
13. 20
13. 30
13. 40
13. 50
13. 60
13. 70
13. 80
13. 90
14. 00
14. 10
14. 20
14. 30
14. 40
14. 50
14. 60
14. 70
14. 80
14. 90
15. 00
15. 10
15. 20
15. 30
15. 40
15. 50
15. 60
15. 70
15. 80
15. 90
16. 00
Mi l l i grams red
1.25 g
sucrose
in
al i quot
36. 55
36. 85
37. 15
37. 50
37. 80
38. 10
38. 45
38. 75
39. 10
39. 40
39. 75
40. 05
40. 40
40. 70
41. 00
41. 35
41 . 65
42. 00
42. 30
42. 60
42. 95
43. 30
43. 60
43. 95
44. 30
44. 65
45. 00
45. 30
45. 60
45. 95
46. 25
46. 60
46. 90
47. 25
47. 60
47. 95
48. 30
48. 65
49. 00
49. 30
49. 65
sugars
2 - 5 g
sucrose
in
al i quot
36. 15
36. 45
36. 75
37. 05
37. 40
37. 70
38. 05
38. 35
38. 65
38. 95
39. 30
39. 60
39. 90
40. 25
40. 55
40. 90
41 . 20
41. 50
41. 85
42. 15
42. 50
42. 80
43. 15
43. 45
43. 80
44. 10
44. 45
44. 75
45. 10
45. 40
45. 75
46. 10
46. 40
46. 75
47. 10
47. 45
47. 80
48. 15
48. 50
48. 80
49. 15
ucing
5 g
sucrose
in
al i quot
35. 30
35. 60
35. 90
36. 25
36. 55
36. 90
37. 20
37. 50
37. 85
38. 15
38. 50
38. 80
39. 15
39. 45
39. 80
40. 10
40. 40
40. 75
41. 10
41. 40
41. 70
42. 00
42. 35
42. 65
43. 00
43. 30
43. 65
44. 00
44. 30
44. 65
44. 95
45. 30
45. 65
46. 00
46. 30
46. 65
47. 00
47. 35
47. 70
48. 00
48. 30
Product
Final bagasse
First expressed juice
Mixed juice
Last expressed juice
Sulphited juice (sulphur tower)
Clarified juice
Filter juice (clear filtrate)
Filter cake
Syrup
Massecuite
Molasses (run-off)
Wash
Final Molasses
Sugar
Method of Sampling
Catch
Continuous
Continuous
automatic
Continuous
Catch
Continuous
Catch
Catch
Catch
Catch
Catch when crystal-
lizer about 1/3 down
Catch from tank
Continuous
Semi-continuous
Period covered
by sample
1/4 hour
1 hour
1 hour
1/4 hour
2 hours
1 hour
1 hour
1 hour
1 hour (from
every tank)
Every strike (at
the discharge)
Every crystallizer
8 hours
24 hours
1 hour
Composite sample
1 hour
4-hour sample to be pre-
served in mill lab.
4-hour sample consisting
of aliquot parts of 1 hr.
samples
4-hour sample, preserva-
tive added
No
4-hour sample, preserva-
tive added
No
No
4-hour sample
No
No
No
6 days
Procedure followed depen
Analysis carried out on
primary sample

Pol
Brix
Pol
Brix, before addition
of lead subacetate

S0
2
pH
Pol
Brix
Pol
Moisture

Pol
Brix
Pol
Brix
Pol
Brix

ds on the circumstances
Analysis carried out on
composite sample
Pol
Moisture
Pol
Pol
Sucrose
Red. sugars
Pol
Brix
-
Pol
Brix
~
-
Pol
Brix
Red.sugars

Pol, brix, sucrose, Red
sugars, sulph. ash
TABLE III
DEGREES BRIX AND CORRESPONDING PER CENT SUCROSE ~

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