DIN EN ISO 3960-2017 Animal and vegetable fats and oils - Determination of peroxide value - Iodometric (visual) endpoint determination (ISO 3960 2017) German version EN ISO 3960 20.pdf

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1、May 2017 English price group 11No 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 67.200.10!%dw“2659684www.din.deDIN E

2、N ISO 3960Animal and vegetable fats and oils Determination of peroxide value Iodometric (visual) endpoint determination (ISO 3960:2017);English version EN ISO 3960:2017,English translation of DIN EN ISO 3960:2017-05Tierische und pflanzliche Fette und le Bestimmung der Peroxidzahl Iodometrische (visu

3、elle) Endpunktbestimmung (ISO 3960:2017);Englische Fassung EN ISO 3960:2017,Englische bersetzung von DIN EN ISO 3960:2017-05Corps gras dorigines animale et vgtale Dtermination de lindice de peroxyde Dtermination avec point darrt iodomtrique (ISO 3960:2017);Version anglaise EN ISO 3960:2017,Traductio

4、n anglaise de DIN EN ISO 3960:2017-05SupersedesDIN EN ISO 3960:201008www.beuth.deDocument comprises 19 pagesDTranslation by DIN-Sprachendienst.In case of doubt, the German-language original shall be considered authoritative.05.17 DIN EN ISO 3960:2017-05 2 A comma is used as the decimal marker. Natio

5、nal foreword This document (EN ISO 3960:2017) has been prepared by Technical Committee ISO/TC 34 “Food products” (Secretariat: AFNOR, France) in collaboration with Technical Committee CEN/TC 307 “Oil seeds, vegetable and animal fats and oils and their by-products Methods of sampling and analysis” (S

6、ecretariat: AFNOR, France). The responsible German bodies involved in its preparation were DIN-Normenausschuss Lebensmittel und landwirtschaftliche Produkte (DIN Standards Committee Food and Agricultural Products) and the Deutsche Gesellschaft fr Fettwissenschaft (German Fat Research Society), Joint

7、 Working Committee NA 057-05-05 AA “Joint committee of DIN and DGF for the analysis of fats, oils and products thereof, related and primary products”. The DIN Standards corresponding to the International Standards referred to in this document are as follows: ISO 661 DIN EN ISO 661 ISO 5555 DIN EN IS

8、O 5555 ISO 5725-1 DIN ISO 5725-1 ISO 5725-2 DIN ISO 5725-2 ISO 27107 DIN EN ISO 27107 Amendments This standard differs from DIN EN ISO 3960:2010-08 as follows: a) milk and milk products (or fat coming from milk and milk products) are now excluded from the scope of the standard; b) the standard has b

9、een editorially revised and brought in line with the current rules of presentation. Previous editions DIN EN ISO 3960: 2005-03, 2009-02, 2010-08 DIN EN ISO 3960:2017-05 3 National Annex NA (informative) Bibliography DIN EN ISO 661, Animal and vegetable fats and oils Preparation of test sample DIN EN

10、 ISO 5555, Animal and vegetable fats and oils Sampling DIN EN ISO 27107, Animal and vegetable fats and oils Determination of iodine value Potentiometric end-point determination DIN ISO 5725-1, Accuracy (trueness and precision) of measurement methods and results Part 1: General principles and definit

11、ions 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 measurement method DIN EN ISO 3960:2017-05 4 This page is intentionally blank EUR

12、OPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 3960 February 2017 ICS 67.200.10 Supersedes EN ISO 3960:2010English Version Animal and vegetable fats and oils - Determination of peroxide value - Iodometric (visual) endpoint determination (ISO 3960:2017) Corps gras dorigines animale et vgtale -

13、 Dtermination de lindice de peroxyde - Dtermination avec point darrt iodomtrique (ISO 3960:2017) Tierische und pflanzliche Fette und le - Bestimmung der Peroxidzahl - Iodometrische (visuelle) Endpunktbestimmung (ISO 3960:2017) This European Standard was approved by CEN on 8 February 2017. CEN member

14、s 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

15、 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 Managemen

16、t 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, Li

17、thuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG CEN-CENELEC Management Centre: Avenue Ma

18、rnix 17, B-1000 Brussels 2017 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 3960:2017 EEuropean foreword .3Introduction 51 Scope . 62 Normative references 63 Terms and definitions . 64 Principle 75 Reagents 76 Apparatus . 87

19、Sampling 98 Preparation of test sample . 99 Procedure. 99.1 General . 99.2 Preparation and titre determination of the 0,01 N sodium thiosulfate standard solution . 99.2.1 Preparation of the 0,01 N sodium thiosulfate standard solution 99.2.2 Determination of the titre of the 0,01 N sodium thiosulfate

20、 standard solution (factor determination) . 109.3 Determination of peroxide value 1010 Calculation and expression of results 1111 Precision of the method . 1111.1 Interlaboratory test 1111.2 Repeatability 1111.3 Reproducibility 1212 Test report 12Annex A (informative) Results of an interlaboratory t

21、est . 13Bibliography .15Contents PageDIN EN ISO 3960:2017-05 EN ISO 3960:2017 (E) 2Foreword . 4European foreword This document (EN ISO 3960:2017) has been prepared by Technical Committee ISO/TC 34 “Food products” in collaboration with Technical Committee CEN/TC 307 “Oilseeds, vegetable and animal fa

22、ts 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 August 2017, and conflicting nation

23、al standards shall be withdrawn at the latest by August 2017. 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

24、 EN ISO 3960:2010. 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 Mac

25、edonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. Endorsement notice The text of ISO 3960:2017 has been approv

26、ed by CEN as EN ISO 3960:2017 without any modification. DIN EN ISO 3960:2017-05 EN ISO 3960:2017 (E)3 ForewordISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standards is normally

27、 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 w

28、ork. 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 dif

29、ferent 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 documen

30、t 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

31、/ 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 ISOs adherence to the World

32、Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT) see the following URL: www .iso. org/ iso/ foreword. html.This document was prepared by Technical Committee ISO/TC 34, Food products, Subcommittee SC 11, Animal and vegetable fats and oils.This fifth edition cancels and rep

33、laces the fourth edition (ISO 3960:2007), of which it constitutes a minor revision to exclude fat coming from milk and milk products.DIN EN ISO 3960:2017-05 EN ISO 3960:2017 (E) 4 IntroductionOver a period of many years, various methods have been developed for the determination of peroxides in fats

34、and oils. The general principle of most of the methods is the liberation of iodine from potassium iodide in an acid medium. The method according to Wheeler was standardized more than 50 years ago by different standardization bodies, and it is widely used to control commodities by producers, receiver

35、s and official laboratories. In national and international food legislation (including the Codex Alimentarius), acceptable limits for the peroxide values are often specified. Due to anomalies in the reproducibility of the results, it was noticed that there are slight differences between the standard

36、ized methods. A very important point is the dependence of the result on the amount of sample used for the determination. As the determination of the peroxide value (PV) is a highly empirical procedure, ISO/TC 34/SC 11 has decided to fix the sample mass at 5 g for PV greater than 1, and at 10 g for P

37、V less than or equal to 1, and to limit the applicability of this method to animal and vegetable fats and oils with peroxide values from 0 meq to 30 meq of active oxygen per kilogram. The user of this document should be aware that the results obtained can be slightly lower than with previous standar

38、ds.DIN EN ISO 3960:2017-05 EN ISO 3960:2017 (E)5 1 ScopeThis document specifies a method for the iodometric determination of the peroxide value of animal and vegetable fats and oils with a visual endpoint detection. The peroxide value is a measure of the amount of oxygen chemically bound to an oil o

39、r fat as peroxides, particularly hydroperoxides.The method is applicable to all animal and vegetable fats and oils, fatty acids and their mixtures with peroxide values from 0 meq to 30 meq (milliequivalents) of active oxygen per kilogram. It is also applicable to margarines and fat spreads with vary

40、ing water content. The method is not suitable for milk fats and is not applicable to lecithins.It is to be noted that the peroxide value is a dynamic parameter, whose value is dependent upon the history of the sample. Furthermore, the determination of the peroxide value is a highly empirical procedu

41、re and the value obtained depends on the sample mass. It is stressed that, due to the prescribed sample mass, the peroxide values obtained can be slightly lower than those obtained with a lower sample mass.Milk and milk products (or fat coming from milk and milk products) are excluded from the scope

42、 of this document.NOTE 1 A preferred method for the iodometric determination of the peroxide value for milk fats is specified in ISO 3976.NOTE 2 A method for the potentiometric determination of the peroxide value is given in ISO 27107.2 Normative referencesThe following documents are referred to in

43、the text in such a way that some or all of their content constitutes requirements 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 661, Animal and vegetable fats and oi

44、ls Preparation of test sample3 Terms and definitionsFor the purposes of this document, the following terms and definitions apply.ISO and IEC maintain terminological databases for use in standardization at the following addresses: IEC Electropedia: available at h t t p :/ www .electropedia .org/ ISO

45、Online browsing platform: available at h t t p s :/ www .iso .org/ obp/ DIN EN ISO 3960:2017-05 EN ISO 3960:2017 (E) 6 3.1peroxide valuePVquantity of those substances in the sample, expressed in terms of active oxygen, that oxidize potassium iodide under the conditions specified in this documentNote

46、 1 to entry: The peroxide value is usually expressed in milliequivalents (meq) of active oxygen per kilogram of oil, but it may also be expressed (in SI units) as millimoles (mmol) of active oxygen per kilogram of oil. The value expressed in millimoles of active oxygen per kilogram is half of that e

47、xpressed in milliequivalents of active oxygen per kilogram. Multiplication of the peroxide value (meq of active oxygen per kilogram) by the equivalent mass of oxygen (equalling 8) gives the milligrams of active oxygen per kilogram of oil.4 PrincipleThe test sample is dissolved in isooctane and glaci

48、al acetic acid, and potassium iodide is added. The iodine liberated by the peroxides is determined iodometrically (visually) with a starch indicator and a sodium thiosulfate standard solution. The endpoint of the titration is determined iodometrically (visually).5 ReagentsWARNING Attention is drawn to the national regulations that specify the handling of hazardous substances and users obligations thereunder. Technical, organ