BS EN ISO 734:2015 — Tracked Changes

compares BS EN ISO 734:2015

with BS EN ISO 734-1:2006

Oilseed meals — Determination of oil

content — Extraction method with hexane
(or light petroleum)
TRACKED CHANGES

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About Tracked Changes

This document is a PDF containing a Tracked Changes version of
BS EN ISO 734, which compares BS EN ISO 734:2015 with
BS EN ISO 734-1:2006.

The original version of BS EN ISO 734:2015, appended at the end of this

document, should be considered the version of record for this
publication.

© The British Standards Institution 2020

Published by BSI Standards Limited 2020
ISBN 978 0 539 10630 5

Amendments/corrigenda issued since publication

Date Text affected
BS EN ISO 734:2015 — Tracked Changes

National foreword
This British Standard was published by BSI. It is the UK implementation of
EN ISO 734-1:2006.EN ISO 734:2015. It supersedes
BS EN ISO 734-1:2001BS EN ISO 734-1:2006 which is withdrawn.
The UK participation in its preparation was entrusted to Technical
Committee AW/307, Oil seedsOilseeds, animal and vegetable fats and oils
and their by-products.
A list of organizations represented on AW/307this 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.
© BSI 2006The British Standards Institution 2016.
Published by BSI Standards Limited 2016
ISBN 0 580 49713 5978 0 580 86665 4

ICS 67.200.20
Compliance with a British Standard cannot confer immunity from
legal obligations.
This British Standard was published under the authority of the Standards Policy
and Strategy Committee on 30 November 200631 January 2016.

Amendments/corrigenda issued since publication

Amd. No. Date Comments

Date Text affected

 BS EN ISO 734:2015 — Tracked Changes

EUROPEAN STANDARD EN ISO 734-1

NORME EUROPÉENNE
EUROPÄISCHE NORM November 2006December 2015

ICS 67.200.20 Supersedes EN ISO 734-1:2006

English Version

Oilseed meals - Determination of oil content - Part 1:

Extraction method with hexane (or light petroleum)
(ISO 734-1:2006ISO 734:2015)
Tourteaux de graines oléagineuses - Détermination Ölsamenschrote - Bestimmung des Ölgehaltes - Teil 1:
de la teneur en huile - Partie 1: Méthode par Extraktionsverfahren mit Hexan (oder Petrolether)
extraction à l'hexane (ou à l'éther de pétrole) (ISO 734-1:2006ISO 734:2015)
(ISO 734-1:2006ISO 734:2015)

This European Standard was approved by CEN on 28 October 200626 September 2015.

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 Central SecretariatCEN-CENELEC 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 Central SecretariatCEN-CENELEC
Management Centre has the same status as the official versions.

CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,
Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania,
Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and
United Kingdom.

EUROPEAN COMMITTEE FOR STANDARDIZATION

COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG

CEN-CENELEC Management Centre: rue de Stassart, 36 Avenue Marnix 17, B-10501000 Brussels

© 20062015 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 734-1:20062015: E
worldwide for CEN national Members.
 BS EN ISO 734:2015 — Tracked Changes

ForewordEuropean foreword

This document (EN ISO 734-1:2006EN ISO 734:2015) has been prepared by Technical Committee
ISO/TC 34 "Agricultural foodFood 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 May 2007June 2016, and conflicting national
standards shall be withdrawn at the latest by May 2007June 2016.

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 734-1:2006.

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,
Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of
Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania,
Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain,
Sweden, Switzerland, Turkey and the United Kingdom.

Endorsement notice

The text of ISO 734-1:2006ISO 734:2015 has been approved by CEN as EN ISO 734-1:2006
EN ISO 734:2015 without any modificationsmodification.

iii
BS EN ISO 734:2015 — Tracked Changes

Contents Page

Foreword .................................................................................................................................................................. v
Introduction ............................................................................................................................................................vi
1 Scope ............................................................................................................................................................. 1
2 Normative references .............................................................................................................................. 1
3 Terms and definitions .............................................................................................................................. 1
4 Principle ...................................................................................................................................................... 1
5 Reagents ...................................................................................................................................................... 1
6 Apparatus .................................................................................................................................................... 1
7 Sampling ...................................................................................................................................................... 2
8 Preparation of test sample ..................................................................................................................... 2
9 Procedure .................................................................................................................................................... 3
9.1 Number of determinations ................................................................................................................................... 3
9.2 Test portion .................................................................................................................................................................. 3
9.3 Pre-drying ...................................................................................................................................................................... 3
9.4 Determination ............................................................................................................................................................. 3
9.4.1 Preparation of the flask ........................................................................................................................ 3
9.4.2 First extraction ......................................................................................................................................... 3
9.4.3 Second extraction .................................................................................................................................... 3
9.4.4 Elimination of solvent and weighing of the extract ............................................................... 4
10 Expression of results ................................................................................................................................ 4
11 Precision ...................................................................................................................................................... 5
11.1 Interlaboratory test .................................................................................................................................................. 5
11.2 Repeatability ................................................................................................................................................................ 5
11.3 Reproducibility ........................................................................................................................................................... 5
12 Test report .................................................................................................................................................. 5
Annex A (informative) Results of an interlaboratory test .......................................................................................6
Bibliography ............................................................................................................................................................ 7

iv
© ISO 2015 – All rights reserved
 BS EN ISO 734:2015 — Tracked Changes

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.

The procedures used to develop this document and those intended for its further maintenance are
described in the ISO/IEC Directives, Part 1. In particular the different approval criteria needed for the
different types of ISO documents should be noted. This document was drafted in accordance with the
editorial rules of the ISO/IEC Directives, Part 2 (see www.iso.org/directives).
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. Details of
any patent rights identified during the development of the document will be in the Introduction and/or
on the ISO list of patent declarations received (see www.iso.org/patents).
Any trade name used in this document is information given for the convenience of users and does not
constitute an endorsement.
For an explanation on the meaning of ISO specific terms and expressions related to conformity
assessment, as well as information about ISO’s adherence to the WTO principles in the Technical
Barriers to Trade (TBT) see the following URL: Foreword - Supplementary information
ISO 734-1 was prepared by Technical Committee The committee responsible for this document is
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
ISO 734-1:2006, which has been technicallyrenumbered andeditorially 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 2015 – All rights reserved

v
 BS EN ISO 734:2015 — Tracked Changes

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.

vi
© ISO 2015 – All rights reserved
 BS EN ISO 734:2015 — Tracked Changes

INTERNATIONAL STANDARD

Oilseed meals — Determination of oil content —

Part 1:
Extraction method with hexane (or light petroleum)
1 Scope
This part of ISO 734International Standard 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 documents, in whole or in part, are normatively referenced documentsin this document and
are indispensable for theits 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 receivedInternational Standard,
NOTE and expressed as a mass fraction, in percent, of the product as received

Note 1 to entry: 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.

6 Apparatus
Usual laboratory apparatus and, in particular, the following.

1
© ISO 2015 – All rights reserved
 BS EN ISO 734:2015 — Tracked Changes

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-Williams2) 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.International Standard. A recommended
samplingmethod is given in ISO 5500.

8 Preparation of test sample

8.1 Prepare the test sample in accordance with ISO 5502.

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 734International Standard 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 734International Standard
and does not constitute an endorsement by ISO of this apparatus.

2
© ISO 2015 – All rights reserved
 BS EN ISO 734:2015 — Tracked Changes

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.
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.

3
© ISO 2015 – All rights reserved
 BS EN ISO 734:2015 — Tracked Changes

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
Formula (1):

where

m0 is the mass, in grams, of the test portion (9.2.1);

m1 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, wD. It
is then equal to Formula (2):

where
w is the mass fraction, in percent, of oil in the product as received (calculated according to 10.1);
wM is the mass fraction, in percent, of moisture and volatile matter, determined as specified in
ISO 771.

4
© ISO 2015 – All rights reserved
 BS EN ISO 734:2015 — Tracked Changes

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

Mean value oil content r R
Sample
% (mass fraction) % (mass fraction) % (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 the following:
a) all information necessary for the complete identification of the sample;
b) the sampling method used, if knowknown;
c) the test method used, with reference to this part ofInternational Standard, i.e. ISO 734;
d) all operating details not specified in this part of ISO 734International Standard, 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.

5
© ISO 2015 – All rights reserved
BS EN ISO 734:2015 — Tracked Changes

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

Sample
Parameter Sunflower
Rapeseed Soya meal
meal
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, sr 0,09 0,06 0,05
Repeatability coefficient of variation (%) 2,4 4,6 1,7
Repeatability limit, r (= 2,8 sr) 0,26 0,17 0,15
Reproducibility standard deviation, sR 0,38 0,20 0,24
Reproducibility coefficient of variation (%) 10,0 15,1 7,8
Reproducibility limit, R (= 2,8 sR) 1,07 0,55 0,66

6
© ISO 2015 – All rights reserved
 BS EN ISO 734:2015 — Tracked Changes

Bibliography

[1] ISO 659:1998, Oilseeds — Determination of oil content (Reference method)

[2] ISO 5500:1986, Oilseed residues — Sampling
[3] ISO 5725-1:1994, Accuracy (trueness and precision) of measurement methods and results —
Part 1:General principles and definitions
[4] 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

7
© ISO 2015 – All rights reserved
 BS EN ISO 734:2015

BSI Standards Publication

Oilseed meals —
Determination of oil
content — Extraction
method with hexane
(or light petroleum)
BS EN ISO 734:2015 BRITISH STANDARD

National foreword
This British Standard is the UK implementation of EN ISO 734:2015.
It supersedes BS EN ISO 734-1:2006 which is withdrawn.
The UK participation in its preparation was entrusted to Technical
Committee AW/307, Oilseeds, 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.
© The British Standards Institution 2016.
Published by BSI Standards Limited 2016
ISBN 978 0 580 86665 4
ICS 67.200.20
Compliance with a British Standard cannot confer immunity from
legal obligations.
This British Standard was published under the authority of the
Standards Policy and Strategy Committee on 31 January 2016.

Amendments/corrigenda issued since publication

Date Text affected

 BS EN ISO 734:2015

EUROPEAN STANDARD EN ISO 734

NORME EUROPÉENNE
EUROPÄISCHE NORM December 2015

ICS 67.200.20 Supersedes EN ISO 734-1:2006

English Version

Oilseed meals - Determination of oil content - Extraction

method with hexane (or light petroleum) (ISO 734:2015)
Tourteaux de graines oléagineuses - Détermination de Ölsamenschrote - Bestimmung des Ölgehaltes -
la teneur en huile - Méthode par extraction à l'hexane Extraktionsverfahren mit Hexan (oder Petrolether)
(ou à l'éther de pétrole) (ISO 734:2015) (ISO 734:2015)

This European Standard was approved by CEN on 26 September 2015.

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-CENELEC 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-CENELEC Management
Centre has the same status as the official versions.

CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,
Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania,
Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and
United Kingdom.

EUROPEAN COMMITTEE FOR STANDARDIZATION

COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG

CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels

© 2015 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 734:2015 E
worldwide for CEN national Members.
BS EN ISO 734:2015
EN ISO 734:2015 (E)

Contents Page

European foreword....................................................................................................................................................... 3

2
 BS EN ISO 734:2015
EN ISO 734:2015 (E)

European foreword

This document (EN ISO 734:2015) has been prepared by Technical Committee ISO/TC 34 "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 June 2016, and conflicting national standards shall be
withdrawn at the latest by June 2016.

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 734-1:2006.

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,
Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia,
France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta,
Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland,
Turkey and the United Kingdom.

Endorsement notice

The text of ISO 734:2015 has been approved by CEN as EN ISO 734:2015 without any modification.

3
 BS EN ISO 734:2015
ISO 734:2015(E)


Contents Page

Foreword......................................................................................................................................................................................................................................... iv
Introduction...................................................................................................................................................................................................................................v
1 Scope.................................................................................................................................................................................................................................. 1
2 Normative references....................................................................................................................................................................................... 1
3 Terms and definitions...................................................................................................................................................................................... 1
4 Principle......................................................................................................................................................................................................................... 1
5 Reagents......................................................................................................................................................................................................................... 1
6 Apparatus...................................................................................................................................................................................................................... 1
7 Sampling......................................................................................................................................................................................................................... 2
8 Preparation of test sample.......................................................................................................................................................................... 2
9 Procedure..................................................................................................................................................................................................................... 3
9.1 Number of determinations............................................................................................................................................................ 3
9.2 Test portion................................................................................................................................................................................................. 3
9.3 Pre-drying.................................................................................................................................................................................................... 3
9.4 Determination.......................................................................................................................................................................................... 3
9.4.1 Preparation of the flask............................................................................................................................................... 3
9.4.2 First extraction................................................................................................................................................................... 3
9.4.3 Second extraction............................................................................................................................................................. 3
9.4.4 Elimination of solvent and weighing of the extract............................................................................ 4
10 Expression of results......................................................................................................................................................................................... 4
11 Precision........................................................................................................................................................................................................................ 5
11.1 Interlaboratory test............................................................................................................................................................................. 5
11.2 Repeatability.............................................................................................................................................................................................. 5
11.3 Reproducibility........................................................................................................................................................................................ 5
12 Test report.................................................................................................................................................................................................................... 5
Annex A (informative) Results of an interlaboratory test............................................................................................................... 6
Bibliography................................................................................................................................................................................................................................. 7

© ISO 2015 – All rights reserved  iii

BS EN ISO 734:2015
ISO 734:2015(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.
The procedures used to develop this document and those intended for its further maintenance are
described in the ISO/IEC Directives, Part 1. In particular the different approval criteria needed for the
different types of ISO documents should be noted. This document was drafted in accordance with the
editorial rules of the ISO/IEC Directives, Part 2 (see www.iso.org/directives).
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. Details of
any patent rights identified during the development of the document will be in the Introduction and/or
on the ISO list of patent declarations received (see www.iso.org/patents).
Any trade name used in this document is information given for the convenience of users and does not
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For an explanation on the meaning of ISO specific terms and expressions related to conformity
assessment, as well as information about ISO’s adherence to the WTO principles in the Technical
Barriers to Trade (TBT) see the following URL: Foreword - Supplementary information
The committee responsible for this document is ISO/TC 34, Food products, Subcommittee SC 2,
Oleaginous seeds and fruits and oilseed meals.
This second edition cancels and replaces ISO 734-1:2006, which has been renumbered and
editorially revised.

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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.

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 BS EN ISO 734:2015

INTERNATIONAL STANDARD ISO 734:2015(E)

Oilseed meals — Determination of oil content — Extraction

method with hexane (or light petroleum)

1 Scope
This International Standard 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 documents, in whole or in part, are normatively referenced in this document and are
indispensable for its application. 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 International Standard,
and expressed as a mass fraction, in percent, of the product as received
Note 1 to entry: 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.

6 Apparatus
Usual laboratory apparatus and, in particular, the following.

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ISO 734:2015(E)


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-Williams2) 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 International Standard. A recommended sampling
method is given in ISO 5500.

8 Preparation of test sample

8.1 Prepare the test sample in accordance with ISO 5502.

1) The Dangoumau mechanical microgrinder is an example of suitable apparatus available commercially.

This information is given for the convenience or users of this International Standard 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 International
Standard and does not constitute an endorsement by ISO of this apparatus.

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ISO 734:2015(E)


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.
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.

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ISO 734:2015(E)


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 Formula (1):
m1
w= × 100% (1)
m0
where

m0 is the mass, in grams, of the test portion (9.2.1);

m1 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, wD. It
is then equal to Formula (2):

100
wD = w × % (2)
100 − w M
where

w is the mass fraction, in percent, of oil in the product as received (calculated according to 10.1);

wM is the mass fraction, in percent, of moisture and volatile matter, determined as specified in
ISO 771.

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 BS EN ISO 734:2015
ISO 734:2015(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

Mean value oil content r R
Sample
% (mass fraction) % (mass fraction) % (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 the following:
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 International Standard, i.e. ISO 734;
d) all operating details not specified in this International Standard, 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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BS EN ISO 734:2015
ISO 734:2015(E)


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

Sample
Parameter Sunflower
Rapeseed meal Soya meal
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, sr 0,09 0,06 0,05
Repeatability coefficient of variation (%) 2,4 4,6 1,7
Repeatability limit, r (= 2,8 sr) 0,26 0,17 0,15
Reproducibility standard deviation, sR 0,38 0,20 0,24
Reproducibility coefficient of variation (%) 10,0 15,1 7,8
Reproducibility limit, R (= 2,8 sR) 1,07 0,55 0,66

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 BS EN ISO 734:2015
ISO 734:2015(E)


Bibliography

[1] ISO 659:1998, Oilseeds — Determination of oil content (Reference method)

[2] ISO 5500:1986, Oilseed residues — Sampling
[3] ISO 5725-1:1994, Accuracy (trueness and precision) of measurement methods and results — Part 1:
General principles and definitions
[4] 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

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