Cereals, cereals-based products and animal feeding stuffs - Determination of crude fat and total fat content by the Randall extraction method (ISO 11085:2015)

This International Standard specifies procedures for the determination of the fat content of cereals,
cereal-based products, and animal feeding stuffs. These procedures are not applicable to oilseeds and
oleaginous fruits.
The choice of procedure to be used depends on the nature and composition of the material analysed
and the reason for carrying out the analysis.
Procedure A is a method for the determination of directly extractable crude fats, applicable to all
materials, except those included within the scope of procedure B.
Procedure B is a method for the determination of total fats, applicable to all materials from which the
oils and fats cannot be completely extracted without prior hydrolysis.
NOTE Most cereals, as well as feeds of animal origin, yeasts, potato protein, compound feeds with milk
products, glutens, and products subjected to processes such as extrusion, flaking, and heating, yield significantly
higher total fat contents when tested by procedure B than by procedure A. See Annex B.

Getreide, Getreideerzeugnisse und Futtermittel - Bestimmung des Rohfettgehalts und des Gesamtfettgehalts mit dem Extraktionsverfahren nach Randall (ISO 11085:2015)

Diese Internationale Norm legt Verfahren zur Bestimmung des Fettgehalts von Getreide, Getreideerzeug¬nissen und Futtermitteln fest. Auf Ölsaaten und ölhaltige Früchte sind diese Verfahren nicht anwendbar.
Die Auswahl des anzuwendenden Verfahrens hängt von der Art und Zusammensetzung des zu analysie¬renden Materials und dem Grund für die Durchführung der Analyse ab.
Verfahren A dient zur Bestimmung des direkt extrahierbaren Rohfettgehalts und ist auf alle Materialien mit Ausnahme der im Anwendungsbereich von Verfahren B angegebenen Materialien anwendbar.
Verfahren B dient zur Bestimmung des Gesamtfettgehalts und ist auf alle Materialien anwendbar, aus denen Öle und Fette ohne vorherige Hydrolyse nicht vollständig extrahiert werden können.
ANMERKUNG   Die meisten Getreide sowie Futtermittel tierischen Ursprungs, Hefen, Kartoffelprotein, Mischfuttermittel mit Milcherzeugnissen, Gluten und Erzeugnisse, die durch Pressvorgänge, Flockenbildung und unter Erwärmung ver¬arbeitet werden, ergeben bei Prüfung nach Verfahren B merklich höhere Gesamtfettgehalte als bei Prüfung nach Verfahren A. Siehe Anhang B.

Céréales, produits céréaliers et aliments des animaux - Détermination de la teneur en matières grasses brutes et en matières grasses totales par la méthode d'extraction de Randall (ISO 11085:2015)

ISO 11085:2015 spécifie des modes opératoires pour la détermination de la teneur en matières grasses des céréales, des produits céréaliers et des aliments pour animaux. Ces modes opératoires ne sont pas applicables aux graines et aux fruits oléagineux.
Le choix de l'un ou l'autre des modes opératoires à utiliser dépend de la nature et de la composition du produit analysé, ainsi que de l'objet de l'analyse.
Le mode opératoire A est une méthode de détermination des matières grasses brutes directement extractibles, applicable à tous les produits sauf ceux relevant du domaine d'application du mode opératoire B.
Le mode opératoire B est une méthode de détermination des matières grasses totales, applicable à tous les produits dont il n'est pas possible d'extraire complètement les huiles et graisses sans procéder à une hydrolyse préalable.
NOTE La plupart des céréales, ainsi que les aliments pour animaux d'origine animale, les levures, les protéines de pomme de terre, les aliments composés pour animaux contenant des produits laitiers, les glutens et les produits transformés par des techniques telles que l'extrusion, le floconnage et le chauffage donnent des teneurs en matières grasses totales significativement plus élevées lorsqu'elles sont soumises à essai avec le mode opératoire B, qu'avec le mode opératoire A. Voir l'Annexe B.

Žito in žitni proizvodi ter krma - Določevanje surove maščobe in skupne vsebnosti maščob z Randallovo ekstrakcijsko metodo (ISO 11085:2015)

Ta mednarodni standard določa postopke za določevanje maščobe v žitu,
žitnih proizvodih ter krmi. Ti postopki se ne uporabljajo za semena oljnic in oljnih plodov.
Izbira uporabljenega postopka je odvisna od narave in sestave analizirane snovi in razloga za izvedbo analize.
Postopek A je metoda za določevanje neposredno izločljive surove maščobe, ki velja za vse
snovi, razen tistih, ki so vključene v področje uporabe postopka B.
Postopek B je metoda za določevanje skupne količine maščob, ki velja za vse snovi, pri katerih brez predhodne hidrolize ni mogoče v celoti izločiti olj in maščob.
OPOMBA Večina žita, pa tudi krma živalskega izvora, kvas, krompirjeve beljakovine, krmne mešanice z mlečnimi izdelki, gluteni in proizvodi, podvrženi procesom, kot so izrivanje, kosmičenje in segrevanje, imajo pri preskušanju po postopku B bistveno višje skupne vsebnosti maščob kot po postopku A. Glej Dodatek B.

General Information

Status
Published
Public Enquiry End Date
29-Apr-2014
Publication Date
02-Nov-2015
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
06-Oct-2015
Due Date
11-Dec-2015
Completion Date
03-Nov-2015

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SLOVENSKI STANDARD
SIST EN ISO 11085:2015
01-december-2015
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SIST EN ISO 11085:2010

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Cereals, cereals-based products and animal feeding stuffs - Determination of crude fat

and total fat content by the Randall extraction method (ISO 11085:2015)

Getreide, Getreideerzeugnisse und Futtermittel - Bestimmung des Rohfettgehalts und

des Gesamtfettgehalts mit dem Extraktionsverfahren nach Randall (ISO 11085:2015)

Céréales, produits céréaliers et aliments des animaux - Détermination de la teneur en

matières grasses brutes et en matières grasses totales par la méthode d'extraction de

Randall (ISO 11085:2015)
Ta slovenski standard je istoveten z: EN ISO 11085:2015
ICS:
65.120 Krmila Animal feeding stuffs
67.060 äLWDVWURþQLFHLQSURL]YRGLL] Cereals, pulses and derived
QMLK products
SIST EN ISO 11085:2015 en

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST EN ISO 11085:2015
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SIST EN ISO 11085:2015
EN ISO 11085
EUROPEAN STANDARD
NORME EUROPÉENNE
September 2015
EUROPÄISCHE NORM
ICS 67.060 Supersedes EN ISO 11085:2010
English Version
Cereals, cereals-based products and animal feeding stuffs -
Determination of crude fat and total fat content by the
Randall extraction method (ISO 11085:2015)

Céréales, produits céréaliers et aliments des animaux - Getreide, Getreideerzeugnisse und Futtermittel -

Détermination de la teneur en matières grasses brutes Bestimmung des Rohfettgehalts und des

et en matières grasses totales par la méthode Gesamtfettgehalts mit dem Extraktionsverfahren nach

d'extraction de Randall (ISO 11085:2015) Randall (ISO 11085:2015)
This European Standard was approved by CEN on 13 June 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 11085:2015 E

worldwide for CEN national Members.
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SIST EN ISO 11085:2015
EN ISO 11085:2015 (E)
Contents Page

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

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SIST EN ISO 11085:2015
EN ISO 11085:2015 (E)
European foreword

This document (EN ISO 11085:2015) has been prepared by Technical Committee ISO/TC 34 "Food

products" in collaboration with Technical Committee CEN/TC 338 “Cereal and cereal products” 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 March 2016, and conflicting national standards shall

be withdrawn at the latest by March 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 11085:2010.

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 11085:2015 has been approved by CEN as EN ISO 11085:2015 without any modification.

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SIST EN ISO 11085:2015
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SIST EN ISO 11085:2015
INTERNATIONAL ISO
STANDARD 11085
Second edition
2015-09-01
Cereals, cereals-based products
and animal feeding stuffs —
Determination of crude fat and total
fat content by the Randall extraction
method
Céréales, produits céréaliers et aliments des animaux —
Détermination de la teneur en matières grasses brutes et en matières
grasses totales par la méthode d’extraction de Randall
Reference number
ISO 11085:2015(E)
ISO 2015
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SIST EN ISO 11085:2015
ISO 11085:2015(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2015, Published in Switzerland

All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized otherwise in any form

or by any means, electronic or mechanical, including photocopying, or posting on the internet or an intranet, without prior

written permission. Permission can be requested from either ISO at the address below or ISO’s member body in the country of

the requester.
ISO copyright office
Ch. de Blandonnet 8 • CP 401
CH-1214 Vernier, Geneva, Switzerland
Tel. +41 22 749 01 11
Fax +41 22 749 09 47
copyright@iso.org
www.iso.org
ii © ISO 2015 – All rights reserved
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SIST EN ISO 11085:2015
ISO 11085:2015(E)
Contents Page

Foreword ........................................................................................................................................................................................................................................iv

1 Scope ................................................................................................................................................................................................................................. 1

2 Normative references ...................................................................................................................................................................................... 1

3 Terms and definitions ..................................................................................................................................................................................... 1

4 Principle ........................................................................................................................................................................................................................ 1

5 Reagents ........................................................................................................................................................................................................................ 2

6 Apparatus ..................................................................................................................................................................................................................... 2

7 Sampling ........................................................................................................................................................................................................................ 3

8 Procedure..................................................................................................................................................................................................................... 3

8.1 Preparation of the test sample .................................................................................................................................................. 3

8.2 Test portion ................................................................................................................................................................................................ 3

8.3 Preliminary extraction ..................................................................................................................................................................... 3

8.4 Hydrolysis .................................................................................................................................................................................................... 4

8.4.1 General...................................................................................................................................................................................... 4

8.4.2 Hydrolysis with apparatus I (6.2) ..................................................................................................................... 4

8.4.3 Hydrolysis with apparatus II (6.3) ................................................................................................................... 4

8.5 Extraction .................................................................................................................................................................................................... 5

9 Calculation and expression of results ............................................................................................................................................. 6

9.1 Determination with preliminary extraction .................................................................................................................. 6

9.2 Determination without preliminary extraction.......................................................................................................... 6

10 Precision ....................................................................................................................................................................................................................... 6

10.1 Interlaboratory test............................................................................................................................................................................. 6

10.2 Repeatability ............................................................................................................................................................................................. 6

10.3 Reproducibility ....................................................................................................................................................................................... 7

10.4 Critical difference.................................................................................................................................................................................. 7

10.4.1 General...................................................................................................................................................................................... 7

10.4.2 Comparison of two groups of measurements in one laboratory ............................................ 7

10.4.3 Comparison of two groups of measurements in two laboratories ....................................... 7

10.5 Measurement uncertainty ............................................................................................................................................................. 8

11 Test report ................................................................................................................................................................................................................... 8

Annex A (informative) Results of an interlaboratory test .............................................................................................................. 9

Annex B (informative) Comparison of fat contents for the samples used in the

interlaboratory test ........................................................................................................................................................................................14

Bibliography .............................................................................................................................................................................................................................16

© ISO 2015 – All rights reserved iii
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SIST EN ISO 11085:2015
ISO 11085:2015(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. 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. 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

The committee responsible for this document is ISO/TC 34, Food products, Subcommittee SC 4, Cereals

and pulses.

This second edition of ISO 11085 cancels and replaces the first edition (ISO 11085:2008), which has

been technically revised.
iv © ISO 2015 – All rights reserved
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SIST EN ISO 11085:2015
INTERNATIONAL STANDARD ISO 11085:2015(E)
Cereals, cereals-based products and animal feeding
stuffs — Determination of crude fat and total fat content by
the Randall extraction method
1 Scope

This International Standard specifies procedures for the determination of the fat content of cereals,

cereal-based products, and animal feeding stuffs. These procedures are not applicable to oilseeds and

oleaginous fruits.

The choice of procedure to be used depends on the nature and composition of the material analysed

and the reason for carrying out the analysis.

Procedure A is a method for the determination of directly extractable crude fats, applicable to all

materials, except those included within the scope of procedure B.

Procedure B is a method for the determination of total fats, applicable to all materials from which the

oils and fats cannot be completely extracted without prior hydrolysis.

NOTE Most cereals, as well as feeds of animal origin, yeasts, potato protein, compound feeds with milk

products, glutens, and products subjected to processes such as extrusion, flaking, and heating, yield significantly

higher total fat contents when tested by procedure B than by procedure A. See Annex B.

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 3696, Water for analytical laboratory use — Specification and test methods
ISO 6498, Animal feeding stuffs — Guidelines for sample preparation
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
3.1
crude fat content

mass fraction of substances extracted from the sample by the specified procedure A

Note 1 to entry: The crude fat content is expressed as a percentage mass fraction.

3.2
total fat content

mass fraction of substances extracted from the sample by the specified procedure B

Note 1 to entry: The total fat content is expressed as a percentage mass fraction.

4 Principle

Fat is extracted using light petroleum as a solvent and the Randall modification of the Soxhlet method.

The test portion is submerged in boiling solvent prior to rinsing in cold solvent, reducing the time

needed for extraction. The solvent dissolves fats, oils, pigments, and other soluble substances. After

© ISO 2015 – All rights reserved 1
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SIST EN ISO 11085:2015
ISO 11085:2015(E)

extraction, the solvent is evaporated and recovered by condensation. The resulting fat residue is

determined gravimetrically after drying.

For total fat determination, the sample is treated under heating with hydrochloric acid. Hydrolysis

makes chemically or mechanically bound fats accessible to solvent extraction. The mixture is cooled

and filtered. The residue is washed and dried and submitted to the above extraction procedure.

For total fat determinations of samples with a “high” fat content (i.e. at least 150 g/kg), a preliminary

extraction is performed before applying procedure B.
5 Reagents
Use only reagents of recognized analytical grade.
5.1 Water, complying with the requirements of at least grade 3 of ISO 3696.

5.2 Light petroleum (petroleum ether), consisting mainly of hydrocarbons with six carbon atoms,

boiling range 30 °C to 60 °C. The bromine value shall be less than one. The evaporation residue shall be

less than 20 mg/l.
5.3 Glass beads, of diameter 5 mm to 6 mm or silicon carbide chips.
5.4 Hydrochloric acid, c(HCl) = 3 mol/l.

5.5 Filtration aid, e.g. diatomaceous earth, boiled for 30 min in hydrochloric acid, c(HCl) = 6 mol/l,

washed with water (5.1) until acid-free, then dried at 130 °C.
5.6 Acetone.
5.7 Cotton wool, defatted.
5.8 Fat-free filter paper.
6 Apparatus
Usual laboratory apparatus and, in particular, the following.

6.1 Solvent extraction system, consisting of a 2-stage Randall extraction process unit enabling solvent

recovery, fitted with fluoroelastomer or polytetrafluoroethylene seals compatible with petroleum ether.

6.2 Hydrolysis apparatus I, multiple position unit enabling boiling with acid, compatible with the

solvent extraction system (6.1), used for hydrolysis according to 8.4.1.

6.3 Hydrolysis apparatus II, consisting of either a beaker of capacity 400 ml and, as a cover, a watch

glass of appropriate diameter, or a conical flask of capacity 300 ml with a re
...

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