DIN EN ISO 11085-2016 Cereals cereals-based products and animal feeding stuffs - Determination of crude fat and total fat content by the Randall extraction method (ISO 11085 2015) .pdf

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1、February 2016 English price group 12No part of this translation may be reproduced without prior permission ofDIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,has the exclusive right of sale for German Standards (DIN-Normen).ICS 67.060!%LR“2414794www.din.deDIN

2、 EN ISO 11085Cereals, cereals-based products and animal feeding stuffs Determination of crude fat and total fat content by the Randall extraction method (ISO 11085:2015);English version EN ISO 11085:2015,English translation of DIN EN ISO 11085:2016-02Getreide, Getreideerzeugnisse und Futtermittel Be

3、stimmung des Rohfettgehalts und des Gesamtfettgehalts mit dem Extraktionsverfahren nach Randall (ISO 11085:2015);Englische Fassung EN ISO 11085:2015,Englische bersetzung von DIN EN ISO 11085:2016-02Crales, produits craliers et aliments des animaux Dtermination de la teneur en matires grasses brutes

4、et en matires grasses totales par la mthode dextraction de Randall (ISO 11085:2015);Version anglaise EN ISO 11085:2015,Traduction anglaise de DIN EN ISO 11085:2016-02SupersedesDIN EN ISO 11085:2010-08www.beuth.deDocument comprises 24 pagesDTranslation by DIN-Sprachendienst.In case of doubt, the Germ

5、an-language original shall be considered authoritative.03.16DIN EN ISO 11085:2016-02 2 A comma is used as the decimal marker. National foreword This document (EN ISO 11085:2015) has been prepared by Technical Committee ISO/TC 34 “Food products” (Secretariat: AFNOR, France), Subcommittee SC 4 “Cereal

6、s and pulses” (Secretariat: SAC, China) in collaboration with Technical Committee CEN/TC 338 “Cereal and cereal products” (Secretariat: AFNOR, France). Based on the results of parallel voting, Technical Committee CEN/TC 338 decided to adopt ISO 11085:2015 as a European Standard. The responsible Germ

7、an body involved in its preparation was DIN-Normenausschuss Lebensmittel und landwirtschaftliche Produkte (DIN Standards Committee Food and Agricultural Products), Working Committee NA 057-05-06 AA Getreide und Getreideerzeugnisse. The DIN Standards corresponding to the International Standards refer

8、red to in this document are as follows: ISO 3696 DIN ISO 3696 ISO 5725-1 DIN ISO 5725-1 ISO 5725-2 DIN ISO 5725-2 ISO 6498 DIN EN ISO 6498 ISO 24333 DIN EN ISO 24333 Amendments This standard differs from DIN EN ISO 11085:2010-08 as follows: a) Clause 2 “Normative references” has been updated to incl

9、ude ISO 6498, which brings the preparation of samples as specified here in compliance with ISO 6492 “Animal feeding stuffs Determination of fat content”; b) in Clause 4, last paragraph, a high fat content of at least 150 g/kg instead of “at least 100 g/kg” is given. Previous editions DIN EN ISO 1108

10、5: 2010-08 DIN EN ISO 11085:2016-02 3 National Annex NA (informative) Bibliography DIN EN ISO 6498, Animal feeding stuffs Guidelines for sample preparation DIN EN ISO 24333, Cereals and cereal products Sampling DIN ISO 3696, Water for analytical laboratory use Specification and test methods DIN ISO

11、5725-1, Accuracy (trueness and precision) of measurement methods and results Part 1: General principles and definitions DIN ISO 5725-2, Accuracy (trueness and precision) of measurement methods and results Part 2: Basic method for the determination of repeatability and reproducibility of a standard m

12、easurement method DIN EN ISO 11085:2016-02 4 Page intentionally left blank EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 11085 September 2015 ICS 67.060 Supersedes EN ISO 11085:2010English Version Cereals, cereals-based products and animal feeding stuffs -Determination of crude fat and to

13、tal fat content by the Randall extraction method (ISO 11085:2015) Crales, produits craliers et aliments des animaux -Dtermination de la teneur en matires grasses brutes et en matires grasses totales par la mthode dextraction de Randall (ISO 11085:2015) Getreide, Getreideerzeugnisse und Futtermittel

14、- Bestimmung des Rohfettgehalts und des Gesamtfettgehalts mit dem Extraktionsverfahren nach 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 Eu

15、ropean 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 versi

16、ons (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,

17、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, Sw

18、itzerland, Turkey andUnited Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR 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 worldwide for CEN natio

19、nal Members. Ref. No. EN ISO 11085:2015 EContents Page Foreword .41 Scope . 52 Normative references 53 Terms and definitions . 54 Principle 55 Reagents 66 Apparatus . 67 Sampling 78 Procedure. 78.1 Preparation of the test sample 78.2 Test portion 78.3 Preliminary extraction . 78.4 Hydrolysis 88.4.1

20、General 88.4.2 Hydrolysis with apparatus I (6.2) . 88.4.3 Hydrolysis with apparatus II (6.3) . 88.5 Extraction 99 Calculation and expression of results 109.1 Determination with preliminary extraction . 109.2 Determination without preliminary extraction. 1010 Precision 1010.1 Interlaboratory test 101

21、0.2 Repeatability 1010.3 Reproducibility 1110.4 Critical difference. 1110.4.1 General. 1110.4.2 Comparison of two groups of measurements in one laboratory . 1110.4.3 Comparison of two groups of measurements in two laboratories 1110.5 Measurement uncertainty 1211 Test report 12Annex A (informative) R

22、esults of an interlaboratory test 13Annex B (informative) Comparison of fat contents for the samples used in the interlaboratory test 18Bibliography .20European foreword.32 EN ISO 11085:2015 (E) DIN EN ISO 11085:2016-02European foreword This document (EN ISO 11085:2015) has been prepared by Technica

23、l 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

24、 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

25、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,

26、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

27、The text of ISO 11085:2015 has been approved by CEN as EN ISO 11085:2015 without any modification. 3EN ISO 11085:2015 (E)DIN EN ISO 11085:2016-02ForewordISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of pr

28、eparing 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, i

29、n 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/IE

30、C 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/directivesAttention is drawn to the possibility that so

31、me 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 declar

32、ations received. www.iso.org/patentsAny 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

33、s adherence to the WTO principles in the Technical Barriers to Trade (TBT) see the following URL: Foreword - Supplementary informationThe 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 t

34、he first edition (ISO 11085:2008), which has been technically revised.4 EN ISO 11085:2015 (E) DIN EN ISO 11085:2016-021 ScopeThis International Standard specifies procedures for the determination of the fat content of cereals, cereal-based products, and animal feeding stuffs. These procedures are no

35、t 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,

36、 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 pr

37、otein, 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 referencesThe following documents, in whole or in part

38、, 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 Specif

39、ication and test methodsISO 6498, Animal feeding stuffs Guidelines for sample preparation3 Terms and definitionsFor the purposes of this document, the following terms and definitions apply.3.1crude fat contentmass fraction of substances extracted from the sample by the specified procedure ANote 1 to

40、 entry: The crude fat content is expressed as a percentage mass fraction.3.2total fat contentmass fraction of substances extracted from the sample by the specified procedure BNote 1 to entry: The total fat content is expressed as a percentage mass fraction.4 PrincipleFat is extracted using light pet

41、roleum 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 5EN ISO 11085:2015 (E)DI

42、N EN ISO 11085:2016-02extraction, 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 f

43、ats 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

44、procedure B.5 ReagentsUse 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 les

45、s 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) unt

46、il acid-free, then dried at 130 C.5.6 Acetone.5.7 Cotton wool, defatted.5.8 Fat-free filter paper.6 ApparatusUsual 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 fluo

47、roelastomer 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

48、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 reflux condenser, used for hydrolysis according to 8.4.2.6.4 Drying oven, capable of being maintained at (103 2) C.6.5 Microwave oven, with defrost setting.6.6 Desiccator, c

49、ontaining an efficient desiccant.6 EN ISO 11085:2015 (E) DIN EN ISO 11085:2016-026.7 Filter cartridge, adapted to the hydrolysis apparatus used.6.8 Extraction thimbles, of cellulose, free from petroleum ether-extractable products, and stand to hold thimbles.6.9 Extraction cups, of aluminium or glass, compatible with the solvent extraction system (6.1).6.10 Glass thimbles for hydrolysis.6.11 Analytical balance, enabling weighing at 102mg accuracy.6.12 Mill or grinder, fitted with a 1 mm screen or for samples with a fat mass fractio