BRITISH STANDARD BS EN ISO

734-2:2008

Oilseed meals —
Determination of oil
content
Part 2: Rapid extraction method (ISO
734-2:2008)

ICS 67.200.20

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BS EN ISO 734-2:2008

National foreword

This British Standard is the UK implementation of EN ISO 734-2:2008.

It supersedes BS EN ISO 734-2:2001 which is withdrawn.
The UK participation in its preparation was entrusted to Technical
Committee AW/307, Oil seeds, animal and vegetable fats and oils and
their by products.
A list of organizations represented on this committee can be obtained on
request to its secretary.
This publication does not purport to include all the necessary provisions
of a contract. Users are responsible for its correct application.
Compliance with a British Standard cannot confer immunity
from legal obligations.

This British Standard Amendments/corrigenda issued since publication

was published under the
authority of the
Standards Policy and Date Comments
Strategy Committee on 30
April 2009
© BSI 2009

ISBN 978 0 580 53600 7

EUROPEAN STANDARD EN ISO 734-2
NORME EUROPÉENNE
EUROPÄISCHE NORM July 2008

ICS 67.200.20 Supersedes EN ISO 734-2:2000

English Version

Oilseed meals - Determination of oil content - Part 2: Rapid

extraction method (ISO 734-2:2008)

Tourteaux de graines oléagineuses - Détermination de la Ölsamenschrote - Bestimmung des Ölgehaltes - Teil 2:

teneur en huile - Partie 2: Méthode rapide par extraction Schnellextraktionsverfahren (ISO 734-2:2008)
(ISO 734-2:2008)

This European Standard was approved by CEN on 21 June 2008.

CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European
Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national
standards may be obtained on application to the CEN Management Centre or to any CEN member.

This European Standard exists in three official versions (English, French, German). A version in any other language made by translation
under the responsibility of a CEN member into its own language and notified to the CEN Management Centre has the same status as the
official versions.

CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland,
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© 2008 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 734-2:2008: E
worldwide for CEN national Members.
BS EN ISO 734-2:2008
EN ISO 734-2:2008 (E)

Foreword
This document (EN ISO 734-2:2008) has been prepared by Technical Committee ISO/TC 34 "Agricultural
food products" in collaboration with Technical Committee CEN/TC 307 “Oilseeds, vegetable and animal fats
and oils and their by-products - Methods of sampling and analysis” the secretariat of which is held by AFNOR.

This European Standard shall be given the status of a national standard, either by publication of an identical
text or by endorsement, at the latest by January 2009, and conflicting national standards shall be withdrawn at
the latest by January 2009.

Attention is drawn to the possibility that some of the elements of this document may be the subject of patent
rights. CEN [and/or CENELEC] shall not be held responsible for identifying any or all such patent rights.

This document supersedes EN ISO 734-2:2000.

According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following
countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Cyprus, Czech
Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia,
Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain,
Sweden, Switzerland and the United Kingdom.

Endorsement notice

The text of ISO 734-2:2008 has been approved by CEN as a EN ISO 734-2:2008 without any modification.

3
 BS EN ISO 734-2:2008
ISO 734-2:2008(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 734-2 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 734-2:1998), 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 2008 – All rights reserved iii

BS EN ISO 734-2:2008
 BS EN ISO 734-2:2008
INTERNATIONAL STANDARD ISO 734-2:2008(E)

Oilseed meals — Determination of oil content —

Part 2:
Rapid extraction method

1 Scope
This part of ISO 734 specifies an extraction method which may be used to assess the efficiency of a de-oiling
process by comparing the oil content of the oilseed with the residual oil content of the corresponding
extraction meals, pellets and expeller cakes.

It is not applicable to disputed cases, for which ISO 734-1 is applicable.

It is applicable to oilseed meals obtained from oilseeds by expelling or by extraction with a solvent, as well as
to the pellets made from the residues.

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
sum of the mass fractions of the substances extracted under the operating conditions specified in this part of
ISO 734 on the basis of the product as received

NOTE 1 The mass fraction is expressed as a percentage.

NOTE 2 On request, the oil content may be expressed relative to dry matter.

4 Principle
The test portion is ground in a micro-ball mill in the presence of a solvent and subsequently extracted with the
same solvent in a suitable apparatus. The solvent is removed from the extract by distillation, then the residue
is weighed after drying.

© ISO 2008 – All rights reserved 1

BS EN ISO 734-2:2008
ISO 734-2:2008(E)

5 Reagents and materials

Use only reagents of recognized analytical grade, unless otherwise specified.

5.1 Technical hexane, n-hexane or light petroleum ether, essentially composed of hydrocarbons with six
carbon atoms, of which less than 5 % distils below 50 °C and more than 95 % distils between 50 °C and 70 °C.

For either solvent, the residue on complete evaporation shall not exceed 2 mg per 100 ml.

The solvent recovered from the extract by distillation should not be used for further determinations.

5.2 Cotton wool, fat-free.

EXAMPLE Defatted cotton wool for ophthalmic use.

6 Apparatus and materials

Usual laboratory apparatus and, in particular, the following.

6.1 Analytical balance, capable of being read to the nearest 0,001 g.

6.2 Drying oven, capable of being maintained at 103 °C ± 2 °C.

6.3 Mechanical microgrinder, capable of wet grinding in the presence of light petroleum ether and
reducing the test portion to an average particle size of less than 10 µm. A commercially available ball mill1) is
suitable.

When using grinding beakers made of polytetrafluoroethylene, cooling is obligatory. A suitable cooling jacket
is shown in Figure 1.

Figure 1 — Grinding beaker with cooling mantle

6.4 Funnel, made of light petroleum ether-resistant plastic, with a diameter of 70 mm, a stem external
diameter of 10 mm and a stem length of 100 mm to 150 mm.

The stem shall just reach into the extraction thimble on placing the funnel in the extraction apparatus as
described in 9.3.4. There is a fixed metal pin in the funnel to retain the stainless steel balls (see Figure 2).

1) The Dangoumau ball mill is an example of a suitable product available commercially and has been studied in a ring
test (Annex A). 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 product. Equivalent products may be used if they can be shown to lead to the same results.

2 © ISO 2008 – All rights reserved

 BS EN ISO 734-2:2008
ISO 734-2:2008(E)

Dimensions in millimetres

Figure 2 — Funnel with stanced metal pin

6.5 Continuous extraction apparatus 2), with ground joints, consisting of a flat bottomed flask of capacity
100 ml to 200 ml, a connecting tube (extractor) to hold the extraction thimble, and a reflux condenser. The
apparatus should include a suitable heating element for boiling technical hexane under reflux conditions. This
might be a water bath, steam bath or safety-approved electrical heating unit.

NOTE 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.

6.6 Extraction thimbles, of dimensions 25 mm × 100 mm, of wall thickness 1,5 mm and a reinforced
bottom part.

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].

8 Preparation of test sample

Prepare the test sample in accordance with ISO 5502.

2) The Twisselmann and Butt extractors are examples of suitable products 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 these
products. The Butt-type extractor is described in AOCS Official method Aa 4-38 [4].

© ISO 2008 – All rights reserved 3

BS EN ISO 734-2:2008
ISO 734-2:2008(E)

9 Procedure

9.1 General

If it is required to check whether the repeatability limit (11.2) is met, carry out two single determinations in
accordance with 9.2 to 9.3.11.

9.2 Test portion

Weigh, to the nearest 0,001 g, 5 g of the well-mixed test sample in an extraction thimble (6.6).

9.3 Determination

9.3.1 Transfer the contents of the thimble to the beaker or tube of the mechanical microgrinder (6.3)
containing all stainless-steels balls.

9.3.2 Add about 20 ml of solvent (5.1). Close the grinding beaker or tube and shake in the microgrinder
(6.3) for 10 min or shake the stainless steel tubes horizontally on a flat bed shaker for 45 min horizontally at a
frequency of 240 min−1, with a horizontal displacement of 35 mm.

9.3.3 Place the thimble (6.6) in the connecting tube (extractor) of the extraction apparatus (6.5) and connect
this to a dried and weighed flask.

9.3.4 Place the funnel (6.4) in the connecting tube in such a manner that the stem of the funnel reaches into
the upper quarter of the thimble.

9.3.5 Then pour the contents of the grinding beaker through the funnel into the extraction thimble in such a
manner that the balls remain on the metal pin in the funnel. Carefully rinse the grinding beaker, its lid and the
balls with solvent in order to transfer all sample particles quantitatively into the extraction thimble. This
requires about 50 ml of solvent, the total volume of which is therefore about 70 ml.

9.3.6 Cover the contents of the extraction thimble with a wad of cotton wool (5.2). Connect the flask and
connecting tube (extractor) to the condenser and place the whole apparatus on the heating apparatus.

9.3.7 Extract for 1 h, calculated from when the solvent begins to boil, while maintaining a reflux rate of at
least 5 ml/min.

9.3.8 Collect the bulk of the solvent in the collecting vessel of the extraction apparatus using the appropriate
actions. Discard recovered solvent.

9.3.9 Remove the flask from the extraction apparatus and leave for about 5 min on the boiling water bath to
evaporate any residual solvent.

9.3.10 Dry the flask containing the oil for 1,5 h in the drying oven (6.2) maintained at 103 °C, and weigh after
cooling to room temperature.

CAUTION — Drying of highly unsaturated oils (e.g. flaxseed oils) may cause the oils to start oxidizing.
This might require special attention if the oils are required for other tests.

9.3.11 Dry the flask for a further 10 min at the same temperature and weigh after cooling. The difference
between the two weighings shall not exceed 0,01 g. If this is not the case, repeat the drying and weighing
procedures.

4 © ISO 2008 – All rights reserved

 BS EN ISO 734-2:2008
ISO 734-2:2008(E)

10 Expression of results
10.1 Calculate the oil content, wo, expressed as a percentage mass fraction, in the test sample, from
Equation (1):

m1
wo = × 100 (1)
m0

where

m0 is the mass, in grams, of the test sample (9.2);

m1 is the mass, in grams, of the extract after drying (9.3.10).

Express the result to one decimal place.

10.2 On request, the oil content may be expressed as a percentage mass fraction of the dry matter, wod,
derived from Equation (2):

100
wod = wo × (2)
100 − wmv

where wmv is the percentage mass fraction of moisture and volatile matter, determined as specified in ISO 771.

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 exceed 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 with 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

Mean value oil content Repeatability limit Reproducibility limit

Sample wo r R
% mass fraction % mass fraction % mass fraction
Rapeseed, soya, and sunflower meals 0 to 5 0,3 0,8

© ISO 2008 – All rights reserved 5

BS EN ISO 734-2:2008
ISO 734-2:2008(E)

12 Test report
The test report shall contain at least the following information:

a) all information necessary for the complete identification of the sample;

b) the sampling method used, if known;

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;

f) if the repeatability has been checked, the final quoted result obtained.

6 © ISO 2008 – All rights reserved

 BS EN ISO 734-2:2008
ISO 734-2:2008(E)

Annex A
(informative)

Results of interlaboratory test

An international collaborative test was organized in 1994 by the German member body (DIN) involving 11
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[2] and ISO 5725-2[3]
to give the precision data shown in Table A.1.

Table A.1 — Results of the interlaboratory test

Sample
Parameter Rapeseed Sunflower
Soya meal
meal meal

No. participating laboratories 11 11 11

No. laboratories retained after eliminating outliers 10 10 11
No. test results in all laboratories 20 20 22
Mean value of oil content, % mass fraction 3,90 1,33 2,93
Repeatability standard deviation, sr 0,08 0,04 0,07

Coefficient of variation of repeatability, CV(r), % 1,9 2,6 2,4

Repeatability limit, r 0,21 0,10 0,20
Reproducibility standard deviation, sR 0,23 0,13 0,29

Coefficient of variation of repeatability, CV(R), % 5,8 10,0 9,7

Reproducibility limit, R 0,64 0,37 0,80

© ISO 2008 – All rights reserved 7

BS EN ISO 734-2:2008
ISO 734-2:2008(E)

Bibliography

[1] ISO 5500, Oilseed residues — Sampling

[2] ISO 5725-1:1994, Accuracy (trueness and precision) of measurement methods and results — Part 1:
General principles and definitions

[3] ISO 5725-2:1994, Accuracy (trueness and precision) of measurement methods and results — Part 2:
Basic method for the determination of repeatability and reproducibility of a standard measurement
method

[4] AOCS Official Method Am 2.93: Determination of oil content in oilseeds. In: Official methods and
recommended practices of the AOCS, 5th edition, FIRESTONE, D.E., editor. AOCS Press, Urbana, IL,
2008

8 © ISO 2008 – All rights reserved

BS EN ISO 734-2:2008
BS EN ISO
734-2:2008
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