DIN EN ISO 8292-1-2010 Animal and vegetable fats and oils - Determination of solid fat content by pulsed NMR - Part 1 Direct method (ISO 8292-1 2008) German version EN ISO 8292-1 2.pdf

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1、August 2010 Translation by DIN-Sprachendienst.English price group 14No 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

2、 67.200.10!$j8“1712921www.din.deDDIN EN ISO 8292-1Animal and vegetable fats and oils Determination of solid fat content by pulsed NMR Part 1: Direct method (ISO 8292-1:2008)English translation of DIN EN ISO 8292-1:2010-08Tierische und pflanzliche Fette und le Bestimmung des Festanteils von Fett durc

3、h das Verfahren mit gepulster magnetischerKernresonanz Teil 1: Direktes Verfahren (ISO 8292-1:2008)Englische bersetzung von DIN EN ISO 8292-1:2010-08Corps gras dorigines animale et vgtale Dtermination de la teneur en corps gras solides par RMN pulse Partie 1: Mthode directe (ISO 8292-1:2008)Traducti

4、on anglaise de DIN EN ISO 8292-1:2010-08DIN EN ISO 8292:1995-07www.beuth.deIn case of doubt, the German-language original shall be considered authoritative.Document comprises 34 pagesSupersedes08.10 DIN EN ISO 8292-1:2010-08 2 A comma is used as the decimal marker. National foreword This standard ha

5、s been prepared by Technical Committee ISO/TC 34 “Food products” (Secretariat: AFNOR, France), Subcommittee SC 11 “Animal and vegetable fats and oils” (Secretariat: BSI, United Kingdom) in collaboration with Technical Committee CEN/TC 307 “Oilseeds, vegetable and animal fats and oils and their by-pr

6、oducts Methods of sampling and analysis” (Secretariat: AFNOR, France). The responsible German bodies involved in its preparation were the Normenausschuss Lebensmittel und landwirtschaftliche Produkte (Food and Agricultural Products Standards Committee) and the Deutsche Gesellschaft fr Fettwissenscha

7、ft DGF (German Fat Research Society), Joint Committee NA 057-05-05 AA Analytik von Fetten, len, Fettprodukten, verwandten Stoffen und Rohstoffen. DIN EN ISO 8292 consists of the following parts, under the general title Animal and vegetable fats and oils Determination of solid fat content by pulsed N

8、MR: Part 1: Direct method Part 2: Indirect method 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 ISO 5555 ISO 5725-1 DIN ISO 5725-1 ISO 5725-2 DIN ISO 5725-2 ISO 8292-2 DIN EN ISO 8292-2 Amendments Th

9、is standard differs from DIN EN ISO 8292:1995-07 as follows: a) The standard has been divided into two parts: Part 1 specifying a direct method and Part 2 specifying an indirect method for the determination of the solid fat content. b) The scope now specifies a direct method for the determination of

10、 the solid fat content in animal and vegetable fats and oils using low-resolution pulsed nuclear magnetic resonance (NMR) spectrometry. c) The definition of “solid fat content” (3.1) has been revised and further terms and definitions have been included. d) Clause 4 “Symbols and abbreviations” has be

11、en added. e) Clause 5 “Principle” (former clause 4) has been given in more detail. f) The former clause 5 “Materials” has been deleted. g) Requirements for the measuring instruments to be used have been revised. h) Clause 8 “Procedure” (former clause 9) has been revised, e.g.: The former subclause 9

12、.1 “Thermal pretreatment” has been replaced by subclause 8.1 “Measurement protocol and test sample”. Subclause 8.2 “Oven, water baths and temperature-controlled blocks” has been added. DIN EN ISO 8292-1:2010-08 3 Subclause 8.3 “Determination of the conversion factor (where necessary)” has been added

13、. Subclause 8.4 “NMR spectrometer” has been added. i) Clause 9 “Expression of results” has been extended. j) Clause 11 “Test report” lists all points that are to be included in the test report. k) Annex A (informative) “Results of interlaboratory tests” has been added. l) Annex B (informative) “Theo

14、ry of the direct method” has been added. m) Annex C (informative) “Additional measurement protocols” has been added. n) The standard has been editorially revised. Previous editions DIN EN ISO 8292: 1995-07 National Annex NA (informative) Bibliography DIN EN ISO 661, Animal and vegetable fats and oil

15、s Preparation of test sample DIN EN ISO 5555, Animal and vegetable fats and oils Sampling DIN ISO 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 resul

16、ts Part 2: Basic method for the determination of repeatability and reproducibility of a standard measurement method DIN EN ISO 8292-2, Animal and vegetable fats and oils Determination of solid fat content by pulsed NMR Part 2: Indirect method DIN EN ISO 8292-1:2010-08 4 This page is intentionally bl

17、ank EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 8292-1 April 2010 ICS 67.200.10 Supersedes EN ISO 8292:1995English Version Animal and vegetable fats and oils - Determination of solid fat content by pulsed NMR - Part 1: Direct method (ISO 8292-1:2008) Corps gras dorigines animale et vgta

18、le - Dtermination de la teneur en corps gras solides par RMN pulse - Partie 1: Mthode directe (ISO 8292-1:2008) Tierische und pflanzliche Fette und le - Bestimmung des Festanteils von Fett durch das Verfahren mit gepulster magnetischer Kernresonanz - Teil 1: Direktes Verfahren (ISO 8292-1:2008) This

19、 European Standard was approved by CEN on 18 March 2010. 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 reference

20、s 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

21、 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, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy

22、, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: Avenue Marnix 17, B-1000

23、Brussels 2010 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 8292-1:2010: EContents EN ISO 8292-1:2010 (E) DIN EN ISO 8292-1:2010-08 2 Page Foreword3 1 Scope 4 2 Normative references 4 3 Terms and definitions .4 4 Symbols and

24、abbreviated terms 5 5 Principle6 6 Apparatus .6 7 Sampling.8 8 Procedure .8 8.1 Measurement protocol and test sample8 8.2 Oven, water baths and temperature-controlled blocks .10 8.3 Determination of the conversion factor (where necessary)10 8.4 NMR spectrometer.11 8.5 Filling the measurement tubes.1

25、1 8.6 Removing the thermal history11 8.7 Equilibrating at the initial temperature11 8.8 Crystallization and tempering 12 8.9 Measuring the SFC 12 8.10 Number of determinations 13 8.11 Cleaning the measurement tubes 13 9 Expression of results 13 10 Precision.14 10.1 Interlaboratory test 14 10.2 Repea

26、tability.14 10.3 Reproducibility.14 11 Test report 15 Annex A (informative) Results of interlaboratory tests.16 Annex B (informative) Theory of the direct method 26 Annex C (informative) Additional measurement protocols28 Bibliography 30 Foreword The text of ISO 8292-1:2008 has been prepared by Tech

27、nical Committee ISO/TC 34 “Food products” of the International Organization for Standardization (ISO) and has been taken over as EN ISO 8292-1:2010 by 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,

28、 either by publication of an identical text or by endorsement, at the latest by October 2010, and conflicting national standards shall be withdrawn at the latest by October 2010. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN

29、 and/or CENELEC shall not be held responsible for identifying any or all such patent rights. This document supersedes EN ISO 8292:1995. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Au

30、stria, Belgium, Bulgaria, Croatia, 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

31、. Endorsement notice The text of ISO 8292-1:2008 has been approved by CEN as a EN ISO 8292-1:2010 without any modification. Technical Committee CEN/TC 307 “Oilseeds, vegetable and animal fats and oils and their by-products EN ISO 8292-1:2010 (E) DIN EN ISO 8292-1:2010-08 3 1 Scope This part of ISO 8

32、292 specifies a direct method for the determination of solid fat content in animal and vegetable fats and oils (hereafter designated “fats”) using low-resolution pulsed nuclear magnetic resonance (NMR) spectrometry. Two alternative thermal pre-treatments are specified: one for general purpose fats n

33、ot exhibiting pronounced polymorphism and which stabilize mainly in the -polymorph; and one for fats similar to cocoa butter which exhibit pronounced polymorphism and stabilize in the -polymorph. Additional thermal pre-treatments, which may be more suitable for specific purposes, are given in an inf

34、ormative annex. The direct method is easy to carry out and is reproducible, but is not as accurate as the indirect method due to the approximate method of calculation. NOTE An indirect method is specified in ISO 8292-2. 2 Normative references The following referenced documents are indispensable for

35、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 661, Animal and vegetable fats and oils Preparation of test sample ISO 8292-2, Animal and vegetable fa

36、ts and oils Determination of solid fat content by pulsed NMR Part 2: Indirect method 3 Terms and definitions For the purposes of this document, the following terms and definitions apply. 3.1 solid fat content SFC ratio as a percentage of the number of protons in the solid phase to the number of prot

37、ons in the solid and liquid phase at a specified temperature NOTE SFC expressed on this basis is taken to be numerically equivalent to the percentage mass fraction of fat in the solid state. No correction is made for the different densities of protons in the solid and liquid phases, because this wou

38、ld require exact knowledge of the composition of the solid and liquid phases of the fat blends at each temperature. Regardless of any other systematic errors, this means that SFC values obtained by this method are about 0,5 % to 1,0 % higher than the true solid fat percentage mass fraction. EN ISO 8

39、292-1:2010 (E) DIN EN ISO 8292-1:2010-08 4 3.2 liquid fat content percentage mass fraction of fat in the liquid state at a specified temperature NOTE The liquid fat content is equal to 100 wSFC, where wSFCis the solid fat content. 3.3 tempering thermal treatment of the fat, after crystallization and

40、 prior to equilibration at the measurement temperature, which consists of holding the fat at a specified temperature for a specified time to transform the fat to a desired polymorph, and/or to ensure that a desired phase equilibrium has been achieved and/or to ensure that crystallization is complete

41、 3.4 measurement temperature temperature at which the solid fat content is determined 3.5 repetition time interval between successive pulses 3.6 dead time time during which the instrument receiver is unable to record the decay signal NOTE Dead time is usually less than 10 s after the pulse. 3.7 meas

42、urement protocol complete description of the solid fat content determination specifying application, instrumental conditions, method, tempering, and whether measurements are in series or in parallel NOTE Measurement protocols are listed in Table 1 and Annex C. 4 Symbols and abbreviated terms f conve

43、rsion (extrapolation) factor to correct the NMR signal observed at 11 s to that at time zero npnumber of pulses S1magnetization decay signal measured at about 11 s S2magnetization decay signal measured at about 70 s SFC solid fat content SLmagnetization decay signal corresponding to the liquid phase

44、 SSmagnetization decay signal corresponding to the solid phase SS+Lmagnetization decay signals corresponding to both solid plus liquid phases treprepetition time wSFC,i“true” SFC (measured in accordance with ISO 8292-2) wSFC,TSFC at measurement temperature, T EN ISO 8292-1:2010 (E) DIN EN ISO 8292-1

45、:2010-08 5 5 Principle The sample is tempered to a stable state at a specific temperature and then heated to, and stabilized at, the measurement temperature. Unless otherwise specified, measurement temperatures can be any or all of: 0 C; 5 C; 10 C; 15 C; 20 C; 25 C; 27,5 C; 30 C; 32,5 C; 35 C; 37,5

46、C; 40 C; 45 C; 50 C; 55 C; 60 C. After electromagnetic equilibration in the static magnetic field of the NMR spectrometer and application of a 90 radio frequency pulse, the magnetization decay signals from the protons in the solid and liquid phases are recorded at about 11 s and about 70 s (or at ti

47、mes recommended by the spectrometer manufacturer, see 6.1). SFC is then calculated. Measurements may be made in series or in parallel. One tube is filled from each test sample when making measurements in series. After tempering as required and holding at 0 C, the measurement tube is moved to the fir

48、st measurement temperature, held for the specified time, the SFC measured, and then moved to the second measurement temperature, and so on. Thus, only one tube is required for all test samples, regardless of how many measurement temperatures are used. However, the SFC recorded at a given measurement

49、 temperature depends on the preceding measurement temperatures and times. As many measurement tubes are filled from each test sample as there are measurement temperatures when making measurements in parallel. After tempering as required and holding at 0 C, each measurement tube is moved more or less simultaneously to each required measurement temperature and held for the specified time before measuring the SFC. Although more tubes are required for measurement in parallel than with that in