EXPERIMENT 11 PROXIMATE
COMPOSITION OF
COARSE GRAINS
Structure
11.1 Introduction
Objective
11.2 Experiment
Principle
Requirements
Procedure
Observations
Calculations
Results
11.1 INTRODUCTION
Grains are routinely tested for their chemical make up in terms of the contents of
moisture, protein, fat (lipids), ash and crude fibre. These constituents are determined
as gram per 100 gms of flour. Carbohydrate content (starch, sugar, etc.) is then
computed by difference. Composition of grains is an indication of their nutritive
value. Following are the actual procedure followed for their determination.
11.2 EXPERIMENT PROCEDURE
11.2.1 Moisture content
All food grains contain certain amount of water, which is normally referred to as
moisture content. Moisture in food grains exists as free or bound. Free moisture
is normally determined by a drying method and the figure obtained will vary
according to the temperature and duration of the heating operation.
A widely used method is to heat a 5 gm, sample in an aluminium dish and heat in
an air oven maintained at 105°C for 18 hours (generally overnight). Quicker
methods of heating for 1 hour at 130°C or for 15 minutes at 155°C are also
available. When comparisons are to be made, all the figures must be obtained by
the same procedure or adjusted by appropriate factors. In general, the moisture
content of flour is in the region 13.0 to 15.0 percent.
Calculations
Moisture content % = (W1 - W) x 100
(WI - W)
Where W = weight of empty aluminium dish, gms
W 1 = Weight of dish + flour, before drying, gms
W 2 = Weight of dish + flour, after drying, gms
Several meters are also available for determination of the moisture content. These
work on the principle of dielectric principle or on conductance, which vary , .
according to the moisture content of the sample. Generally, these work in a moisture
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range of 10 to 20 %. However, these need to be calibrated against the moisture Proximate Composition of
Coarse Grains
content determined in an oven as indicated above.
Express the weight of moisture as % of weight of the flour.
11.2.2· Ash content
The ash content of flour which contains no mineral additions is an index of the
extent to which the flour is contarriinated with bran powders or sand (silica), and
hence the grade and quality of the flour, because the ash content of the skins of
the grains is normally in the region of thirty times as great as the ash of pure
endosperm. A suitable method of determining the ash content of flour is as follows:
About 2 to 5 grams of the flour is weighed into a tared silica or platinum dish and
placed in a muffle furnace maintained at a temperature of 550°C to 575°C for 6
to 8 hours. When a white ash has been obtained, remove the dish to a desiccator
and when it is cool, weight it quickly. The amount of mineral residue of ash is
expressed as percentage of original sample.
Calculations
Ash content = C - B x 100
A-B
Where A = weight of silica dish + sample (before ashing), gms
B = weight of empty silica dish, gms
C = weight of silica dish + sample (after ashing), gms
Express the weight of ash as % of weight of the flour.
Ash is boiled with 0.1 N HCl for 30 minutes on a water bath, after which it is
filtered through an ashless filter paper (normally Wattman No. 42). It is washed
further till acid is completely washed. The filtrate obtained is made up to a standard
volume (about 100 ml), This is used for the estimation of minerals like iron, calcium
and phosphorus. The ashless filter paper is put back to the silica dish and ashed
further and its weight is noted.
Acid insoluble ash = Total Ash- weight of ashed filter paper
11.2.3 Protein content
The protein content is.arrived at by determining the nitrogen content and multiplying
by a factor which is normally 6.25 (taking the nitrogen content present in protein
as 16%). ..
The grain sample should be coarsely ground on a hand-operated coffee mill and a
1 gm, aliquot of the ground material used for the test. Selenium is a suitable catalyst.
In the laboratory 1 gm of the ground flour sample, 20 rnl of concentrated sulphuric
acid, with a digestion mixture containing 9 gm of potassium sulphate, S gm copper
sulphate and 0.05 to 0.1 gm of powdered selenium are digested in a Kjeldahl flask
for a few hours, till a clear blue solution results. The digested solution is made up
to 100 rnl with distilled water. An aliquot (5 ml) is put into the distillation unit and
distilled for about 15 minutes into ~OOml of a 1 percent solution of boric acid
which has been neutralised to the indicator used in the subsequent titration
(Bromocresol green + Methyl red - 4 drops). When the distillation has been
completed, the distillate is titrated, using the above-mentioned indicator, with NI
70 hydrochloric acid to an end poitn of light green to red colour. 31
Practical Manual for Calculations
Maize and Coarse Grains
Normality ofHCl used for titration = 0.0163 N
Weight of HCl per ltr, = 0.0163 x 36.5 = 0.595 gms of HCl
It is known that 14 parts of Nitrogen = 36.5 parts of HCl (equivalent weights)
Therefore 0.595 parts of HCl = 0.595 x 14 or 0.228 gms of N per ltr.
36.5
Therefore Nitrogen % in the distillate =
0.228 x Vol. of distillate made up x Titre Vol. of HCl x 100
1000 Vol. of aliquot taken Vol. of sample taken
Calculate the protein content as mg N x 6.25 to obtain protein content of the flour.
11.2.4 Oil (lipids I fat) content
As you have already learnt, lipid content of the flour is important for product
making. Lipids also play an important role in the keeping quality of the flour. Since
unsaturated fatty acids in cereallipids get oxidized to produce free fatty acids (FFA).
Changes that takes place in the lipid fraction during storage of the flour can be
monitored by the measurement of FFA and peroxide value as described in the
following section.
A weighed quantity of the sample shall be placed in an extraction thimble, which
shall then be placed in an extraction apparatus on a water bath and extracted with
petroleum spirit (boiling point 40-60°C). At the end of 3-4 hours the thimble shall
be removed from the apparatus, dried and its contents finely ground, preferably
with sand, in a small mortar previously rinsed with petroleum spirit. The substance
shall then be returned to the thimble, the mortar being washed out with petroleum
spirit, and the extraction continued for another hour. The extract should be free
from suspended matter. After evaporation of extract should be free from suspended
matter. After evaporation of the solvent, the oil shall be dried at 1000C and
weighted.
Express the oil content as % of weight of the flour.
11.2.5 Free Fatty acids (FFA)
Fat / oil is extracted from 100 gms of the flour with a pinch anhydrous sodium
sulphate with 200 rnl chloroform for 18 h and then filtered. 20 rnl of the filtrate is
evapourated and dried in vacuum. Weight of the extracted fat is determined.
Another 25 ml of the filtrate is mixed with hot meutralized alcohol adn titrated
against 0.1 N sodium hydroxide using phenolphthalein as indicator and FFA is
calculated as oleic acid (taking its mol. weight as 282) as follows:
FFA % (as oleic acid) = ml of NaOH x alkali factor x 28.2
Weight of the fat in gms
11.2.6 Peroxide value (PV)
25rnl of extracted fat aliquot mixed with acetic acid (2 parts) and water (3 parts)
and 0.5 ml of saturated potassium iodide and titrated against O.IN sodium
thiosulphate solution by using starch as an indicator. PV is calculated as follows:
)
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PV (in milliequivalents) = S x N x 1000 Proximate Composition of
Coarse Grains
weight of the fat
Where S = titre reading
N = normality of siodium thiosulphate.
11.2.7 Fibre content
''Two grams, accurately weighed, shall be extracted-with petroleum spirit (boiling
point 40-60"C) in an extraction apparatus, or at least three times by stirring, settling
and decantation, and the dry residue transferred to a conical 1000 milliliter flask.
The material must not be further ground during extraction. A volume of 200
milliliters of a solution containing 1.25 gm of sulphuric acid (H2SO 4) per 100
milliliters measured at ordinary temperature and brought to boiling point, shall be
added to the flask and heated. The contents of the flask must come to boiling within
1 min. and the boiling throughout must be gentle and continuous for exactly 30
min, the original volume being maintained.
The flask shall be rotated every few minutes in order to mix the contents and remove
particles from the sides. At the end of 30 minutes the flask shall be removed and
the contents poured at once into the shallow layer of hot water remaining in a funnel
fitted with a pump-plate or alternatively into the similar layer remaining in a Buchner
funnel. The funnel shall be prepared by cutting a piece of cotton cloth or filter paper
to cover the holes, so as to serve as a support for a disc of ordinary filter paper;
boiling water shall be poured into the funnel and allowed to remain until the funnel
is hot, whereupon suction is applied. the experiment shall be discarded if the time
of filtration of the bulk of the 200 milliliters exceeds 10 min. The residue shall be
washed with boiling water until the washings are free from acid. The residue shall
then be washed from the filter paper back into the flask with a volume of 2:00
milliliters of a solution of sodium hydroxide, containing 1.25 gms of sodium
hydroxide (NaOH) per 100 milliliter free or nearly free from sodium carbonate,
measured at ordinary temperature, and brought to boiling point.
The contents of the flask shall be boiled for exactly 30 min, the precautions given
forthe treatment with acid being observed. At the end of 30 minutes the flask
shall be removed and its contents immediately filtered through an ordinary filter
paper. The residue collected on the filter paper shall be washed with boiling water,
then with a solution of 1 % hydrochloric acid and again with boiling water until
free from acid. The residue shall then be washed twice with 95% alcohol, and
e
three times with ether. The residue at about 100 in an oven and weighed in its
D
weighing bottle until constant in weight. The ash of the paper and contents shall be
determined by incineration at a dull red heat. The weight of ash shall be subtracted
from the increase of weight found on the paper and the difference shall be reported
as fibre.
11.2.8 Carbohydrate content
This is normally calculated by difference taking into account the sum of contents
of moisture, protein. crude fibre, and oil contents.
11.2.9 Fair Average Quality (FAQ)
This factor is assuming importance to determine the quality of grains for procurement
under various governmental systems. Here different quality factors are determined
to fix standards which will help in fixing the procurement price as well as assuring
quality maintenance during storage.
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