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IS 3579 (1966): Methods of test for oilseeds [FAD 13: Oils

and Oilseeds]

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IS : 3579 - 1966
(Reaffirmed 2000)

Indian Standard
METHODS OF TEST FOR
OILSEEDS
( Third Reprint MARCH 1994 )

UDC

63385 : 543

0 Copyright 1967
BUREAU
MANAK

OF
BHAVAN.

INDIAN
9
NEW

Gr 3

BAHADUR

STANDARDS
SHAH

ZAFAR

MARG

DELHI-110002

August 1967

lsr3579-1966

Indian Standard
METHODS OF TEST FOR
OILSEEDS
Oils and Oilseeds Sectional Committee, CAFDC 5
Refmsenting

Chaiwnan

Swastik Oil Mills Ltd, Bombay

DR J. S, BADAMI

Members
SHRI V. A. PARS= ( Alternate to

Dr J. S. Badami )
Regional Research Laboratory ( CSIR ), Hyderabad
DR K, T. ACHAYA
DR G. LAUSWMINARAYANA
( A&mate )
Directorate of Marketing & Inspection ( Ministry of
SHRI V. P. ANANTANARAYANAN
Food & Agriculture ), Nagpur
SHRSV. CHANDRAMOULY( Alternate)
National Test House, Calcutta
SHRI R. C. DAS GUPTA
SHRI K. C. ~&HTA ( Altrmah )
The Tata Oil Mills Co Ltd, Bombay
SHRI N. DESIXCACHAR
DR B. G. GIJNDE( Alternate )
Indian Agricultural Research Institute, New Delhi
DR K. C. GULATI
Hindustan Lever Ltd. Bombay
DR G. S. HATTIANCDI
Directorate of Sugar & Vanaspati ( Ministry of Food
SHRI K. P. JAIN
& Agriculture )
SHRI F. G1 T. MENEZES( Altunate)
Italab Private Ltd, Bombay
DR S. M. KAJI
SHRI J. C. DEY (, Alternate ) ( Calcutta )
SHRI S. S. HONAVAR ( Alternate ) ( Madras )
Central Committee for Food Standards ( Ministry of
DR B. D. NARANG
Health )
SHRI D. S. CHADH~ ( Alternate)
Bombay Oilseeds and Oils Exchange Ltd, Bombay
SHRI N. P. NO~ANI
SHR~ C. V. MARIWALA ( Akna~e )
Godrej Soaps Private Ltd, Bombay
SHRI V. M. PAI
SHRI B. V. KANTAK ( Al&ma&)
The Vanaspati Manufacturers AsJbciation of ,India,
SHRI S. S. RAMA.SWAMY
Bombay
Directorate General of Technical
Development,
DR H. G. R. REDD~
New Delhi
Oil Technological Research Institute, Anantapur
REPRE~ENTATWE
Solvent Extractors Association of India, Rombay
SHRI RAM SHARMA
SHRI P. P. SHARMA(Al&male)
Khadi and Village Industries Commission, Bombay
SHRI P. V. SHR~~ANTARAO
SHRI P. V. GUJARATHI( Alterna~c)

( Continuedonpage 2 )

BUREAU
OF INDIAN
STANDARD
S
MANAKBHAVAN, 9 BAHADUR SHAH ZAFAR MARG
NEW DELI-Ii 110002

ls:3579-1966
( Continuedfrom page 1 )
Members
Rejresen fing
SHRI L. R. SUD
Ministry of Defence ( R & D )
SHRI A. P. CHAKRAVERTY( Alternate )
DR SADGOPAL,
Director General, ISI ( Ex-o#cio Member)
Director ( Chem )
Secretaries
SHRI S.

SUBRAHMANYAN

Deputy Director
SHR~R. C.

( Chem),

IS1

MISRA

Assistant Director ( Ctem ), IS1

Oilseeds Subcommittee,

CAFDC

5 :5

Conwner
SHR1 C. V. MAR1wALA

Bombay Oilseeds and Oils Exchange

Ltd, Bombay

Members

Regional Research Laboratory ( CSIR ), Hyderabad

DRK. T. ACHAYA
DR G. LAKSHMINARAYANA
( Alternate )
Directorate of Marketing & Inspection ( Ministry of
SHRr k. p. ANANTANARAYANAN
Food & Agriculrure), Nagpur
SHRI V. CHANDRAMOULY
( Akernate )
The East Asiatic Company ( India ) Private Ltd,
DR K. C. DANDONA
Madras
Bengal Oii %Iil!s Association, Calcutta
SHRI S. L. GARG
The Tata Oil Mills Co Ltd, Bomba)
Da B. G. GUNDE
Hindustan Lever Ltd, Bombay
Da G. S. HATTIANCDI
Indian Agricultural Research Institutq, Xew Delhi
Da A. R. S. MARTHA
Central
Food Technological
Research
Institute
SHRIS.K.kfAJuMDAR
( CSIR ), Mysore
Swasrik Oil Mills Ltd, Bombay
SHRI V. A:PARIKH
The Grain, Rice and Oilseeds &lerchants AssociaSHRI PREMJIBHANJI
tion, Bombay
S~a1 VASANJILAKHAMSI( Alternate)
Botanical Survey of India, Calcutta
DR J. SEN
Sna1 S. N. MITRA ( -4lternale)
Indian Standards Institution, New Delhi
SRRI B. N. %NoH
The Central Organization for Oil Industry and
S~a1 MADDI
SULJERSANAM
Trade, Bombay
S~a1 KRISHANNARA~N ( Alternate )
Central Warehousing Corporation, New Delhi
SHRI P. M. THOMAS
Sna1 P. RAM DAS ( Alternate )
Panel

for Methods

DR K. T. HCHAYA

of Test for Oilseeds, CAFDC

Regional Research Laboratory

5 :5 :2
( CSIR 3, Hyderabad

x3:3579-1966

Indian Standard
METHODS OF TEST FOR
OILSEEDS
0.

FOREWORD

0.1 This Indian Standard was adopted by the Indian Standards Institution
on 24 November 1966, after the draft fir&zed by the Oils and Oilseeds
Sectional Committee had been approved by the Chemical Division Council
and the Agricultural and Food Products Division Council.
0.2 India produces large quantities of different oil bearing seeds and fruits.
With a view to introducing uniform methods of test for these oleaginous
materials in the country, this standard is being published.
Prior to Ahe
publication of this standard, there were no uniform methods of test for the
purpose, nor any standard on this subject in the country.
0.3 The methods of test prescribed in this standard are based on the
methods followed by the manufacturers, consumers and testing authorities
concerned in the country.
This standard will enable the producers as well
as the consumers to assess the quality of oilseeds.
0.4 Due consideration has also been given to the need for alignment of the
niethods with those prescribed in the publications of international organizations including IS0 for testing of oilseeds, and these considerations have led
the Sectional Committee to refer to the documents issued by the Oleaginous
Seeds and Fruits Subcommittee, ISO/TC 34/SC2 and to the following
publication :
Methods of sampling and analysis of oils, fats and oilseeds, 1962.
International Association of Seed Crushers, London.
0.5 In reporting the result of a test or analysis made in accordance with
this standard, if the final value, observed or calculated, is to be rounded off,
it shall be done in accordance with IS ; 2-1960*.

1. SCOPE

1.1 This standard prescribes the methods of test for oilseeds, including the
oil bearing fixits.
2. TERMINOLOGY
2.0 For the purpose of this standard the following definitions shall apply.
*Rules for rounding

off numerical

values ( rccaied ).

2.1 Pod or Gaps&Fruit which is dry and non-fleshy when ripe, and
which on splitting open releati its seeds; for example, groundnut and
castor.
2.2 Fruit - Fleshy product of a tree or plant surrounding or embedding
the seed, and sometimes the source of an oil; for example, red palm or
olive.
2.3 Seed -A
mature ovule, consisting of an embryo together with a store
of food, the wholi surrounded by a protective coat which may be a thin
testa, as in groundnut, a leathery skin as in sesame, a hard hull as in castor
or a woody shell as in coconut.
2.4 Kernel - Softer body enclosed by the seed coat or shell which carries* ,I>
d
_-the oil; sometimes termed meats.
2.5 Damaged and Weevilled - Seeds or kernels or pieces of these which
have sprouted or are internally damaged as a result of heat, moisture, insect
or microbial action.
2.6 Slightly Damaged - Seeds or kernels that are damaged, for example,
by abiasion, in such a way as not to affect their quality.
2.7 Shrivelled and Immature
- Seeds or kernels that are shrunk out of
shape, or are not fully mature or developed, and are often discoloured.
2.8 Split Kernels - Kernels which are split into two halves, but are
otherwise full and mature, as in groundnut.
\\
pieces of kernels which are bigger than
2.9 Broken Kernels -Broken
one-sixteenth the size of the kernel.
Broken pieces of kernels smaller than one-sixteenth the size

2.10 Nooks of the kernel.

2.11 Impurities
- Foreign bodies other than pure seeds or parts thereof,
which could consist of the following:
a) Durt - Particles passing through 1*Omm IS Sieve conforming to
IS .* 460- 1962 * .
b) Non-Oleaginous Bodies - Stalks, fibrous matter, stones, debris and
other matter which does not pass through the above sieve.
c) Other OiLweds- Seeds other than those specified.
3. SAMPLING
3;l Representative samples for the purpose of these tests shall be drawn in
accordance with 1S : 4115 - I967 t
-

l!jpc&fkation
t&fcthods

for test sieves ( retied ).

of sampling

of oilseeds

.
4

Is:357911966
EXAMINATION

4. PHYSICAL

4.1 Take a sample of 500 g of the material

( seeds or kernels ). Sieve

through l$O-mm IS Sieve ( conforming to IS : 460-1962* ). Collect the
dust passing down the sieve, weigh and report as a percentage ( arithmetic
mean of two determinations ).
4.1.1 Examine the sample left on the sieve for other oilseeds and
non-oleaginous bodies. Separate these from the specified seeds by handpicking with the help of forceps. Report the percentage of impurities as
the arithmetic mean of two determinations to an accuracy of 0.01 percent.
-

_\

4.1.2 Continue with the above samples. Separate the specified seeds by
hand-picking and visual examination and report as follows:
4 Damaged and weevilled seeds or kernels, percent by weight,
b) Slightly damaged seeds or kernels, percent by weight,
cl Shrivelled and immature seeds or kernels, percent by weight,
4 Split and broken kernels, percent by .weight,
-4 Nooks, percent by weight, and
f 1 Impurities, percent by weight .( whichever be applicable to the
seeds or kernels under examination ).

5. CHEMICAL

EXAMINATION

5.1 Determination

of Moisture

Content

5.1.0 General - The percentage of moisture in either the sample under

analysis or separately in the separated impurities and in the seed is
determined by drying to constant weight at a temperature of 105 f 1C.

5.1.1

Apparatus

5.1.1.1 Moisture dish -made

of aluminium sheet about 0.45 to

@56 mm thickness, 70 to 80 mm in diameter and 20 mm deep; provided
with tight-fitting slip-over cover.
5.1.1.2 Desiccatorcontaining
an efficient desiccant,
such as
phosphorus pentoxide.
5.1.1.3 Air-oven - preferably electrically heated, with temperature
control device.
5.1.2 Procedure-Weigh
accurately 2 f 0.5 g of the sample into a
moisture dish which has been dried previously, cooled in the desiccator and
then weighed. Place the dish in the air-oven for approximately one hour
at 105 f 1C. Remove the dish from the oven, cool in the desiccator to
room temperature and weigh. Repeat this procedure but keep the dish
+Qm$kation

for test sicva

( r&d).

Is:3579-1966
in the oven only for half an hour each time until the difference between
the two successive weighings does not exceed one milligram.
5.1.3

Caictdation
100 w
Moisture, percent by weight = w-

where
w = loss in weight in g of the material upon drying, and
W = weight in g of the material taken for the test.
5.1.4 Rejorting - Indicate clearly whether the result
moiqture content of the whole sample or of the pure seeds.

represents

the

5.2 Determination of Oil Content

5.2.0 General - The oil content is determined by extractions with a
petroleum hydrocarbon solvent ( conforming to IS : 174 5- 196 1* ) .
5.2.1 Preparation of the Sam@Crush the seeds in a suitable crusher.
Mix thoroughly to make it uniform mass. Take an aliquot for the
determination of oil content.
512.1.1 Carry out the determination on the oilseeds or on the pure
seeds and impurities separated from the sample.
5.2.2

Afipparatus

5.2.2.1 Soxhlet extraction apparatus heating and disti!ling accessories.

5.2.2.2

Air-oven

5.2.2.3

G1ass~ask.s -

of suitable capacity equipped with

150 to 250 ml capacity.

5.2.2.4 Cru.&~- Pestle and mortar or mechanical mortar or mill. A

coffee grinder is quite suitable for grinding of small whole seeds, reduced
seed obtained in grinding, and extraction residues.
5.2.2.5
5.2.3

Extraction thimbles

Reagents

3.2.3.1 Petroleum hydrocarbon solvent 60/801961* ) re-distilled before use.

( conforming to IS : 1743-

5.2.3.2 Sand- About 180 microns ( see IS : 460-1962t ) washed with

hydrochloric acid and calcined;or quartz powder of about 180 microns.
*Specification

for petroleum

TSpecification

for test sieves ( mised ).

hydrocarbon

solvents. (Since

wised

).

1s : 3579 - 1966
5.2.4 Procedure
- Crush the whole seeds in a mortar.
Carefully mix the
ground sample or small seeds and accurately weigh a quantity sufficient to
give 2 g of oil.
Transfer the weighed material to an extraction
thimble,
avoiding any losses.
Place the thimble in the extractor, previously fitted
with a weighed flask.
Where a mortar has been used, rinse it and its
pestle with petroleum hydrocarbon
solvent transferring the washings to the
Add the quantity of solvent required for efficient working of the
extractor.
extractor
to this apparatus;
aflix the condenser and allow through it a
current of cold water to flow; and heat the extractor
so that the action is
moderate and not violent.
5.2.4.1
Continue
the extraction
for four hours.
Then remove the
extractor from its bath, take the extraction
thimble, after it has drained,
out of the extractor and allow solvent to evaporate from it in a current of
air,
5.2.4.2
Dry the thimble and contents in the oven at 103 5 2C for
Empty the thimble into a mortar and add approximately
30 minutes.
10 g of fine sand or quartz ( unless every oil sell on the sample is broken,
Grind the mixture as finely as possible.
extraction
will be incomplete ).
Transfer the ground material to the thimble again; place the thimble in
the extractor;
rinse pestle and mortar with solvent and transfer rinsings to
Repeat the extraction process further for two hours.
the extractor.
5.2.4.3
Again remove the thimble from the extractor, dry it with the
conteuts as before; and grind the contents again without the addition of
more sand or quartz.
Again transfer the ground material to the extractor.
Fit a second weighed iiask to the extractor.
Rinse pestle and mortar with
solvent as before and extract for two hours.
5.2.4.4
Remove the greater part of the solvent in thr two flasks by
distillation
from a hot water bath.
Heat the flasks in an oven at
103 _& 2C for one hour to remove solvent.
Cool them to room temperature and weigh.
Repeat the heating process and cooling until the weight
of ti.e flasks is constant.
If the weight of oil in the second flask does not
exceed 10 mg, the extractiou
is complete;
should it excectd this amount,
repeat
the extraction
of the ground
material,
re-grinding
between
extraction, until the weight of material removed in a given extraction
does
not exceed 10 mg.
5.2.4.5
Add together the weights
flasks as found in this manner.

of oil extracted

into

the successive

5.2.4.6
If the oil recovered as above is not clear, it may be dissolved
in solvent and filtered through a filter paper.
The paper should be washed
thoroughly with solvent and the oil solution and the washings should be
combined.
Solvent should be evaporated as in 5.2.4.4 and the flask containing the oil dried and weighed as above to obtain the true amount of oil.
7

IS I 3579
5.2.5

1366

Calculation

Oil, percent

20% loo
by weight = 7

where
w = weight in g of the oil extracted, and
W = weight in g of the analysis sample taken for the test,
NOTE1 - Express percentage
(b) whole material, if necessary.

of oil (a) on moisture and impurities free basis, and

NOTE 2 -Duplicate
determinations should not difler by more than @3 percent. The
If the difference
figure to be reported shall be the arithmetic mean of such duplicates.
betwem duplicates shall be more than @3 percent, repeat the analysis on two further
portions of the sample.

5.3 Determination of Acid Valse of the Extracted Oil

5.3.0 Gettctal - This method determines the acidity of the extracted oil.
The acid value is determined by. directly titrating the material in an
alcoholic medium with aqueous sodium or potassium hydroxide solution.
5.3.1

Reagents

5.3.1.1

Diethyl ether

5.3.1.2
Ethyl alcohol - ninety-five percent (by volume), or rectified
spirit ( conforming to IS : 323-1959* ) neutral to phenolphthalein indicator.

5.3.1.3 ,Phenolphthalein
indicator sol&ion phenolphthalein in 100 ml of ethyl alcohol.

Dissolve

one

gram

of

NOTE- When testing oils or fats which give dark coloured soap solution, the
observation of the end point of the titration may be facilitated either (a) by using
thymolphthalein or alkali blue 6B in place of phenolphthalein or (b) by adding one
millilitre of a @ 1 percent ( w/v ) solution of mcthylene blue in water to each 100 ml of
phenolphthalein indicator solution before the titration.

5.3.1.4 Standard aqueous potassium hydroxide or sodium hydroxide solutions 0.1 N or 0.5 N.
5.3.2 Procedure - Mix the oil or melted fat thoroughly before weighing.
Weigh accurately a suitable quantity of the cooled oil or fat in a 200-ml
conical flask. The weight of the oil or fat taken for the test and the
strength
of the alkali used for the titration shall be such that the volume of
alkali required for the titration dJes not exceed 10 ml. Add 50 to 100 ml
of freshly neutralized hot ethyl alcohol, and about one miIIiIitre of
phenolphthalein indicator solution. Boil the mixture for about five minutes \
Specification

for rectified spirit (revised).

IS : 3579 - 1966
and titrate while as hot as possible with
shaking vigorously during titration.

standard

aqueous

alkali

solution,

NOTE--Where the acid value of oil extracted from oilseeds is required, it is essential
that the oil should be extracted immediatcty after the seed has been ground or shredded
as the acid value of ground or shredded seeds rises very rapidly.

5.3.3

Cakul,don
!%*I v 1
Acid value = -----WP

where

V = volume in ml of standard potassium h.ydroxide or sodium

hydroxide
N_= normality
hydroxide
W = weight

solution

used,

of standard potassium
solution, and

in g of the material

hydroxide

taken for the test.

or sodium

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