ISO

INTERNATIONAL STANDARD
734-1
Second edition 2006-11-01

Oilseed meals — Determination of oil content — Part 1:

Extraction method with hexane (or light petroleum)
Tourteaux de graines oléagineuses — Détermination de la teneur en huile —
Partie 1: Méthode par extraction à l'hexane (ou à l'éther de pétrole)
Reference number ISO 734-1:2006(E)
© ISO 2006
ISO 734-1:2006(E)
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ISO 734-1:2006(E)

Foreword
ISO (the International Organization for Standardization) is a worldwide federation of national standards
bodies (ISO member bodies). The work of preparing International Standards is normally carried out
through ISO technical committees. Each member body interested in a subject for which a technical
committee has been established has the right to be represented on that committee. International
organizations, governmental and non-governmental, in liaison with ISO, also take part in the work. ISO
collaborates closely with the International Electrotechnical Commission (IEC) on all matters of
electrotechnical standardization.
International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2.
The main task of technical committees is to prepare International Standards. Draft International Standards
adopted by the technical committees are circulated to the member bodies for voting. Publication as an
International Standard requires approval by at least 75 % of the member bodies casting a vote.
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. ISO shall not be held responsible for identifying any or all such patent rights.
ISO 734-1 was prepared by Technical Committee ISO/TC 34, Food products, Subcommittee SC 2,
Oleaginous seeds and fruits and oilseed meals.
This second edition cancels and replaces the first edition (ISO 734-1:1998), Annex A of which has been
technically revised.
ISO 734 consists of the following parts, under the general title Oilseed meals — Determination of oil
content:
⎯ Part 1: Extraction method with hexane (or light petroleum)
⎯ Part 2: Rapid extraction method
© ISO 2006 – All rights reserved iii
ISO 734-1:2006(E)

Introduction
A method for the determination of the oil content of oilseeds has been specified in ISO 659. It is therefore
necessary to provide for control of oil production by establishing a reference method for the determination
of the oil content of oilseed meals in the same way.
iv © ISO 2006 – All rights reserved
INTERNATIONAL STANDARD ISO 734-1:2006(E)

Oilseed meals — Determination of oil content —

Part 1: Extraction method with hexane (or light petroleum)
1 Scope
This part of ISO 734 specifies a method for the determination of the hexane extract (or light-petroleum
extract), called “oil content”, of meals (excluding compounded products) obtained by the extraction of oil
from oilseeds by pressure or solvents.

2 Normative references
The following referenced documents are indispensable for the application of this document. For dated
references, only the edition cited applies. For undated references, the latest edition of the referenced
document (including any amendments) applies.
ISO 771, Oilseed residues — Determination of moisture and volatile matter content
ISO 5502, Oilseed residues — Preparation of test samples

3 Terms and definitions

For the purposes of this document, the following terms and definitions apply.
3.1 oil content all of the substances extracted under the operating conditions specified in this part of ISO
734, and expressed as a mass fraction, in percent, of the product as received
NOTE The oil content may also be expressed relative to dry matter.

4 Principle
A test portion of the product is extracted in a suitable apparatus, with technical hexane or, failing this, light
petroleum. The solvent is eliminated and the extract obtained is weighed.

5 Reagents
Use only reagents of recognized analytical grade, unless otherwise specified.
5.1 Technical hexane, n-hexane or light petroleum, essentially composed of hydrocarbons with six carbon
atoms.
Less than 5 % shall distil below 50 °C and more than 95 % between 50 °C and 70 °C.
For any of these solvents, the residue on complete evaporation shall not exceed 2 mg per 100 ml.
© ISO 2006 – All rights reserved

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ISO 734-1:2006(E)
6 Apparatus
Usual laboratory apparatus and, in particular, the following.
6.1 Mechanical grinder, easy to clean and allowing the meals to be ground, without heating and without
appreciable change in moisture, volatile matter and oil content, to obtain particles which pass completely
through a sieve of aperture size 1 mm.
6.2 Mechanical microgrinder, of the Dangoumau type1) capable of producing a fineness of grinding of
oilseed meals of less than 160 μm, with the exception of the “shell” whose particles may reach 400 μm.
In laboratories where a microgrinder is not available, microgrinding of the ground sample (see 9.4.3) may
be replaced by trituration with a pestle and mortar, in the presence of about 10 g of sand that has been
washed with hydrochloric acid and then calcined. However, grinding in a mortar cannot be applied in the
case of multiple analyses because operator fatigue prevents sufficiently efficient grinding of numerous
samples, and the extraction of oil from a coarsely ground sample can never be complete.
6.3 Extraction thimble and cotton wool, or filter paper, free from matter soluble in hexane or light
petroleum.
6.4 Suitable extraction apparatus, fitted with a flask of capacity 200 ml to 250 ml.
NOTE Straight-through extractors, for example the Butt, Smalley, Twisselmann and Bolton-Williams
2)
are
suitable. The use of other extractors is conditional upon the results of a test on a standard material of known oil
content to confirm the suitability of the apparatus.
6.5 Electric heating bath (e.g. sand bath, water bath) or hot plate.
6.6 Electrically heated oven, with thermostatic control, permitting ventilation or obtaining reduced
pressure, capable of being maintained at 103 °C + 2 °C.
6.7 Desiccator, containing an efficient desiccant.
6.8 Pumice stone, in small particles, previously dried in an oven at 103 °C + 2 °C and cooled in a
dessicator.
6.9 Analytical balance, capable of weighing to an accuracy of + 0,001 g.

7 Sampling
A representative sample should have been sent to the laboratory. It should not have been damaged or
changed during transport or storage.
Sampling is not part of the method specified in this part of ISO 734. A recommended sampling method is
given in ISO 5500.
1) The Dangoumau mechanical microgrinder is an example of suitable apparatus available commercially. This
information is given for the convenience or users of this part of ISO 734 and does not constitute an endorsement by
ISO of this apparatus.
2) The Butt, Smalley, Twisselmann or Bolton-Williams straight-through extractors are examples of suitable apparatus
available commercially. This information is given for the convenience of users of this part of ISO 734 and does not
constitute an endorsement by ISO of this apparatus.
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© ISO 2006 – All rights reserved
ISO 734-1:2006(E)
8 Preparation of test sample
8.1 Prepare the test sample in accordance with ISO 5502.
8.2 If necessary, grind the test sample, in the previously well-cleaned mechanical mill (6.1). First, use
about one-twentieth of the sample to complete the cleaning of the mill, and reject these grindings. Then
grind the rest, collect the grindings, mix carefully and carry out the analysis without delay.

9 Procedure
9.1 Number of determinations
If it is required to check whether the repeatability (11.2) is met, carry out two single determinations in
accordance with 9.2 to 9.4.4.
9.2 Test portion
9.2.1 Weigh, to the nearest 0,001 g, about 10 g of the test sample (8.2).
9.2.2 Transfer this test portion to the extraction thimble (6.3) and close the latter with a wad of cotton wool
(6.3). If a filter paper is used, wrap the test portion in it.
9.3 Pre-drying
If the test portion is very moist [moisture and volatile matter content more than 10 % (mass fraction)],
leave the filled thimble for some time in an oven, maintained at a temperature not higher than 80 °C, to
reduce the moisture and volatile matter content to less than 10 % (mass fraction).
As an alternative to the pre-drying procedure described above, the test portion (9.2.1) may be mixed in a
suitable vessel with 2 g to 3 g of analytical quality anhydrous sodium sulfate per 5 g of grindings.
Continue as indicated in 9.2.2 and 9.4.
9.4 Determination
9.4.1 Preparation of the flask
Weigh, to the nearest 1 mg, the flask of the extraction apparatus (6.4) containing one or two particles of
pumice stone (6.8).
9.4.2 First extraction
Place the thimble (6.3) containing the test portion in the extraction apparatus (6.4). Pour into the flask the
necessary quantity of solvent (5.1). Fit the flask to the extraction apparatus on the electric heating bath or
hot- plate (6.5). Carry out the heating so that the rate of reflux is at least 3 drops per second (boiling
moderately, not violently).
After extracting for 4 h, allow to cool. Remove the thimble from the extraction apparatus and place it in a
current of air in order to expel the greater part of the residual solvent.
9.4.3 Second extraction
Empty the thimble into the microgrinder (6.2) and grind as finely as possible. Put the mixture back into the
thimble and put the latter back into the extraction apparatus. Re-extract for a further 2 h, using the same
flask containing the first extract.
© ISO 2006 – All rights reserved
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ISO 734-1:2006(E)
The solution obtained in the extraction flask shall be clear. If it is not, filter it through a filter paper,
collecting the filtrate in another previously dried and tared flask, then wash the first flask and filter paper
several times with the same solvent.
9.4.4 Elimination of solvent and weighing of the extract
Expel the greater part of the solvent from the flask by distillation on the electric heating bath or the hot
plate (6.5). Expel the last traces of solvent by heating the flask for about 20 min in the electrically heated
oven (6.6) set at 103 °C.
In the case of meals rich in volatile acids (meals from copra, palm kernel, etc.), drying of the extract
should be carried out at atmospheric pressure, and at 80 °C maximum.
Assist the removal of solvent either by blowing air or, preferably, an inert gas (such as nitrogen or carbon
dioxide) into the flask for short periods, or by reducing the pressure in the flask.
In the case of drying or semi-drying oilseed meals, it is preferable to remove the residual solvent by drying
under reduced pressure.
Allow the flask to cool in the dessicator (6.7), for at least 1 h, to ambient temperature and then weigh to
the nearest 1 mg.
Heat again for about 10 min under the same conditions. Allow to cool and reweigh.
The difference between the two weighings shall not exceed 10 mg. If it does, repeat the operations of
heating for 10 min, cooling and weighing until the difference between two successive weighings does not
exceed 10 mg. Note the final mass of the flask.

10 Expression of results
10.1 The oil content, w, expressed as a mass fraction, in percent, of the product as received, is equal to
w
=mm
01
×
100
%
where
m
0
is the mass, in grams, of the test portion (9.2.1);
m
1
is the mass, in grams, of the extract after drying (see 9.4.4).
Express the result to one decimal place.
10.2 On request, the oil content may be expressed as a mass fraction, in percent, of the dry matter, w
D
.
It is then equal to
wD
=w
×
100
100 −
w
M

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© ISO 2006 – All rights reserved %
where
w is the mass fraction, in percent, of oil in the product as received (calculated according to 10.1);
w
M
is the mass fraction, in percent, of moisture and volatile matter, determined as specified in ISO 771.
ISO 734-1:2006(E)
11 Precision
11.1 Interlaboratory test
Details of an interlaboratory test on the precision of the method are summarized in Annex A. The values
derived from this interlaboratory test may not be applicable to concentration ranges and matrices other
than those given.
11.2 Repeatability
The absolute difference between two independent single test results, obtained using the same method on
identical test material in the same laboratory by the same operator using the same equipment within a
short interval of time, will in not more than 5 % of cases be greater than the value of the repeatability limit
r given in Table 1.
11.3 Reproducibility
The absolute difference between two single test results, obtained using the same method on identical test
material in different laboratories by different operators using different equipment, will in not more than 5 %
of cases exceed the value of the reproducibility limit R given in Table 1.
Table 1 — Repeatability and reproducibility limits
Sample
Mean value oil content
% (mass fraction)
© ISO 2006 – All rights reserved
r
% (mass fraction)
R
% (mass fraction)
Rapeseed meal 0 to 5 0,3 1,1
Soya and sunflower meals 0 to 5 0,2 0,7

12 Test report
The test report shall specify:
a) all information necessary for the complete identification of the sample;
b) the sampling method used, if know;
c) the test method used, with reference to this part of ISO 734;
d) all operating details not specified in this part of ISO 734, or regarded as optional, together with details
of
any incidents which may have influenced the test result(s);
e) the test result(s) obtained and the solvent used, indicating clearly whether the result represents the oil
content of the product as received or the oil content in relation to the dry matter;
f) if the repeatability has been checked, the final quoted result obtained.
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Annex A (informative)
Results of an interlaboratory test
An international collaborative test was organized in 1994 by the Institut für Chemie und Physik der Fette
(BAGKF, Germany), involving 13 laboratories, each laboratory having performed a duplicate analysis of
each sample.
The test was carried out on three samples:
⎯ rapeseed meal;
⎯ soya meal;
⎯ sunflower meal.
The results obtained were subjected to statistical analysis in accordance with ISO 5725-1 and ISO 5725-2
to give the precision data shown in Table A.1.
Table A.1 — Results of the interlaboratory test
Parameter
Sample
Rapeseed meal Soya meal Sunflower meal
Number of participating laboratories 13 13 13
Number of laboratories retained after eliminating outliers 12 12 13
Number of test results in all laboratories 24 24 26
Mean oil content [% (mass fraction)] 3,84 1,30 3,04
Repeatability standard deviation, s
r
0,09 0,06 0,05
Repeatability coefficient of variation (%) 2,4 4,6 1,7
Repeatability limit, r (= 2,8 s
r
) 0,26 0,17 0,15
Reproducibility standard deviation, s
R
0,38 0,20 0,24
Reproducibility coefficient of variation (%) 10,0 15,1 7,8
Reproducibility limit, R (= 2,8 s
R
) 1,07 0,55 0,66

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