SIST EN ISO 659:2009
(Main)Oilseeds - Determination of oil content (Reference method) (ISO 659:2009)
Oilseeds - Determination of oil content (Reference method) (ISO 659:2009)
This International Standard specifies a reference method for the determination of the hexane extract (or light petroleum extract), called "oil content", of oilseeds used as industrial raw materials. The procedure for sunflower seeds is different from the other seeds as it includes a second moisture content determination after the first mechanical grind. The method has been tested on rapeseed, soya beans and sunflower seeds. This does not, however, preclude its applicability to other commercial seeds. If required, the pure seeds and the impurities (see 9.4) may be analysed separately. In the case of groundnuts, the pure seeds, the total fines, the non-oleaginous impurities and the oleaginous impurities (see 10.1.6) may be analysed separately.
Ölsamen - Bestimmung des Ölgehaltes (Referenzverfahren) (ISO 659:2009)
Diese Internationale Norm legt ein Referenzverfahren zur Bestimmung des Hexan-Extrakts (oder des Petrolether-
Extrakts), bezeichnet als „Ölgehalt“, von Ölsamen fest, die als Rohstoffe in der Industrie verwendet
werden. Das Verfahren für Sonnenblumensamen unterscheidet sich von den anderen Samen, da es eine
zusätzliche Bestimmung des Feuchtigkeitsgehaltes enthält, nachdem der Samen gemahlen wurde, um die
Untersuchungsprobe herzustellen.
Das Verfahren ist an Rapssamen, Sojabohnen und Sonnenblumensamen geprüft worden. Dies schließt
jedoch seine Anwendbarkeit auf andere handelsüblichen Samen nicht aus.
Falls erforderlich, können die reinen Samen und die Verunreinigungen (siehe 9.4) getrennt untersucht
werden. Im Fall von Erdnüssen (siehe 10.1.6) können die reinen Samen, das gesamte Feingut, die nicht
ölhaltigen Verunreinigungen und die ölhaltigen Verunreinigungen getrennt untersucht werden.
Graines oléagineuses - Détermination de la teneur en huile (Méthode de référence) (ISO 659:2009)
L'ISO 659:2009 spécifie une méthode de référence pour la détermination de l'extrait à l'hexane (ou à l'éther de pétrole), dit «teneur en huile», des graines oléagineuses utilisées comme matière première industrielle. Le mode opératoire utilisé pour les graines de tournesol est différent de celui utilisé pour les autres graines car il inclut une étape supplémentaire pour la détermination de la teneur en eau après la préparation de l'échantillon pour essai par broyage des graines.
La méthode a été soumise à essai sur des graines de colza, de soja et de tournesol. Cela n'exclut pas, toutefois, la possibilité d'appliquer cette méthode à d'autres graines disponibles dans le commerce.
Si nécessaire, les graines pures et les impuretés peuvent être analysées séparément. Dans le cas de l'arachide, les graines pures, les poussières totales et les impuretés non oléagineuses et oléagineuses peuvent être analysées séparément.
Oljna semena - Določevanje olja (referenčna metoda) (ISO 659:2009)
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
SIST EN ISO 659:2009
01-december-2009
1DGRPHãþD
SIST EN ISO 659:1998
2OMQDVHPHQD'RORþHYDQMHROMD UHIHUHQþQDPHWRGD ,62
Oilseeds - Determination of oil content (Reference method) (ISO 659:2009)
Ölsamen - Bestimmung des Ölgehaltes (Referenzverfahren) (ISO 659:2009)
Graines oléagineuses - Détermination de la teneur en huile (Méthode de référence) (ISO
659:2009)
Ta slovenski standard je istoveten z: EN ISO 659:2009
ICS:
67.200.20 Oljnice Oilseeds
SIST EN ISO 659:2009 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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SIST EN ISO 659:2009
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SIST EN ISO 659:2009
EUROPEAN STANDARD
EN ISO 659
NORME EUROPÉENNE
EUROPÄISCHE NORM
July 2009
ICS 67.200.20 Supersedes EN ISO 659:1998
English Version
Oilseeds - Determination of oil content (Reference method) (ISO
659:2009)
Graines oléagineuses - Détermination de la teneur en huile Ölsamen - Bestimmung des Ölgehaltes
(Méthode de référence) (ISO 659:2009) (Referenzverfahren) (ISO 659:2009)
This European Standard was approved by CEN on 3 June 2009.
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,
France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal,
Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre: Avenue Marnix 17, B-1000 Brussels
© 2009 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 659:2009: E
worldwide for CEN national Members.
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SIST EN ISO 659:2009
EN ISO 659:2009 (E)
Contents Page
Foreword .3
2
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SIST EN ISO 659:2009
EN ISO 659:2009 (E)
Foreword
This document (EN ISO 659:2009) 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 January 2010, and conflicting national standards shall be withdrawn at
the latest by January 2010.
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 659:1998.
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 659:2009 has been approved by CEN as a EN ISO 659:2009 without any modification.
3
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SIST EN ISO 659:2009
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SIST EN ISO 659:2009
INTERNATIONAL ISO
STANDARD 659
Fourth edition
2009-07-01
Oilseeds — Determination of oil content
(Reference method)
Graines oléagineuses — Détermination de la teneur en huile (Méthode
de référence)
Reference number
ISO 659:2009(E)
©
ISO 2009
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SIST EN ISO 659:2009
ISO 659:2009(E)
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ii © ISO 2009 – All rights reserved
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SIST EN ISO 659:2009
ISO 659:2009(E)
Contents Page
Foreword. iv
1 Scope . 1
2 Normative references . 1
3 Terms and definitions. 1
4 Principle. 1
5 Reagent. 2
6 Apparatus . 2
7 Sampling. 3
8 Preparation of test sample. 3
8.1 Reduction of laboratory sample. 3
8.2 Predrying . 3
8.3 Test sample . 4
9 Procedure . 5
9.1 General. 5
9.2 Test portion . 5
9.3 Determination. 6
9.4 “Oil content” of impurities. 7
10 Expression of results . 7
10.1 Method of calculation. 7
11 Precision. 10
11.1 Interlaboratory test programme . 10
11.2 Repeatability. 10
11.3 Reproducibility. 10
12 Test report . 10
Annex A (informative) Results of interlaboratory tests on the determination of oil content . 11
Bibliography . 12
© ISO 2009 – All rights reserved iii
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SIST EN ISO 659:2009
ISO 659:2009(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 659 was prepared by Technical Committee ISO/TC 34, Food products, Subcommittee SC 2, Oleaginous
seeds and fruits and oilseed meals.
1)
This fourth edition cancels and replaces the third edition (ISO 659:1998), which has been technically revised.
The main change is the inclusion of an additional subclause (Subclause 8.3.5) for the preparation of the test
sample in the case of sunflower seed. This different procedure for sunflower seed includes an extra step, viz
measurement of the moisture content after grinding the seed. This is necessary to correct for the loss of
moisture caused by the heating of the seed which occurs during grinding due to the particular physical nature
of sunflower seed.
1) Users should note that the front cover and foreword of ISO 659:1998 indicate erroneously that it is the second edition,
whereas it is in fact the third.
iv © ISO 2009 – All rights reserved
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SIST EN ISO 659:2009
INTERNATIONAL STANDARD ISO 659:2009(E)
Oilseeds — Determination of oil content (Reference method)
1 Scope
This International Standard specifies a reference method for the determination of the hexane extract (or light
petroleum extract), called the “oil content”, of oilseeds used as industrial raw materials. The procedure for
sunflower seed is different from those for other seeds as it includes an additional moisture content
determination after the seed has been ground to prepare the test sample.
The method has been tested on rapeseed, soya beans and sunflower seed. This does not, however, preclude
its applicability to other commercial seeds.
If required, the pure seeds and the impurities (see 9.4) can be analysed separately. In the case of groundnuts
(see 10.1.6), the pure seeds, the total fines, the non-oleaginous impurities and the oleaginous impurities can
be analysed separately.
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 658, Oilseeds — Determination of content of impurities
ISO 664, Oilseeds — Reduction of laboratory sample to test sample
ISO 665, Oilseeds — Determination of moisture and volatile matter content
3 Terms and definitions
For the purposes of this International Standard, the following terms and definitions apply.
3.1
hexane extract
“oil content”
all the substances extracted under the operating conditions specified in this International Standard, expressed
as a percentage by mass of the product as received, or on the cleaned seed
NOTE On request, it may be expressed relative to the dry matter.
4 Principle
The oil is extracted from a test portion, in a suitable apparatus, with hexane or light petroleum. The solvent is
removed from the extract and the extract weighed. Due to the varied nature of seeds, there are some
variations in the procedure for different seeds.
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SIST EN ISO 659:2009
ISO 659:2009(E)
5 Reagent
5.1 Technical hexane, n-hexane or light petroleum, essentially composed of hydrocarbons with six
carbon atoms, of which less than 5 % distils below 40 °C and more than 95 % distils between 40 °C and 60 °C
or between 50 °C and 70 °C, and which has a bromine value of less than 1. The residue on complete
evaporation shall not exceed 2 mg per 100 ml.
6 Apparatus
Usual laboratory apparatus and, in particular, the following:
6.1 Analytical balance, with an accuracy of ± 0,001 g.
6.2 Mechanical mill, easy to clean, appropriate for the nature of the oilseeds and allowing the oilseeds to
be ground to a uniform particle size without appreciable heating or change in moisture, volatile-matter or oil
content.
NOTE The following mills have been found to give satisfactory results:
2)
⎯ the Christy & Norris 8" laboratory mill , with perforated-plate or bar-type screens depending on seed type (e.g.
0,8 mm perforated plate, 3 mm and 6 mm bar screens; see 8.3.2, 8.3.3 and 8.3.4);
2)
⎯ the Retsch ZM 200 ultra-centrifugal mill , with a 1 mm screen for sunflower seed or with other screens depending on
seed type.
Other mills may be satisfactory, provided they conform to the criteria given above.
6.3 Mechanical microgrinder, capable of producing a fineness of grind of the oilseeds of less than 160 µm,
with the exception of the “shell”, particles of which may reach 400 µm. Coffee grinders and similar cutting-
action mechanical grinders shall not be used as microgrinders.
NOTE A ball mill comprising a stainless-steel tube of volume approximately 120 ml and 1 cm, 2 cm and 3 cm
diameter steel balls (weighing approximately 7 g, 30 g and 130 g), depending on the sample being ground, and utilizing
extremely rapid shaking, has been found to be suitable.
If the microgrinder and its closure are designed for use with solvents, a small amount (approximately 20 ml) of
solvent may be added to the cylinder in order to increase the speed of the extraction.
6.4 Extraction thimble (cellulose) and cotton wool, free from matter soluble in hexane or light petroleum.
6.5 Suitable extraction apparatus, fitted with a flask of capacity 200 ml to 250 ml.
Straight-through extractors, for example the Butt, Smalley or Bolton-Williams type, are preferred for safety
reasons and have been found to give a more efficient extraction.
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. If a Soxhlet syphoning-type extractor is used then, for safety
reasons, a 250 ml flask should be utilized and the volume of solvent used shall be at least 150 ml. This should
prevent rapid boiling on syphoning, which could otherwise cause loss of solvent and/or part of the test portion.
6.6 Pumice stone, in small particles, or other anti-bumping granules, previously dried in an oven at
(130 ± 2) °C and cooled in a desiccator.
2) The Christy & Norris 8" mill and the Retsch ZM 200 mill are examples of suitable products available commercially.
This information is given for the convenience of users of this International Standard and does not constitute an
endorsement by ISO of these products.
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SIST EN ISO 659:2009
ISO 659:2009(E)
6.7 Apparatus for safely removing solvent from extraction thimble (for example, in a current of inert
gas).
WARNING — This process should be carried out in a fume hood.
6.8 Electric heating bath (sand bath, water bath, heating mantle, etc.) or hot-plate.
6.9 Electrically heated oven, with thermostatic control, capable of being maintained at (103 ± 2) °C. The
oven shall be capable of being used at either atmospheric or reduced pressure (see 9.3.3).
6.10 Desiccator, containing an efficient desiccant (e.g. silica gel, with orange indicator, or P O ).
2 5
6.11 Electrically heated oven, capable of being maintained at (130 ± 2) °C (for cottonseed, see 8.3.6).
6.12 Metal dish, flat-bottomed, of diameter 100 mm and height approximately 40 mm.
7 Sampling
Sampling is not part of the method specified in this International Standard. A recommended sampling method
is given in ISO 542.
It is important that the laboratory receive a sample which is truly representative and has not been damaged or
changed during transport and storage.
8 Preparation of test sample
8.1 Reduction of laboratory sample
Prepare the test sample in accordance with ISO 664. If large non-oleaginous foreign bodies have been
separated before reduction of the laboratory sample, make allowance for this in the calculation (see 10.1.5).
Depending on the requirements of the contract or the instructions, take the sample as received or after
separation of the impurities.
8.2 Predrying
8.2.1 The moisture content of the test portion (see 9.2) shall be less than a mass fraction of 10 % when
extraction of the oil (see
...
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