EN ISO 13884-2005 en Animal and vegetable fats and oils Determination of isolated trans isomers by infrared spectrometry《动物和植物脂肪和油 用红外光谱测定法测定孤立的反式异构体 ISO 13884-2003》.pdf

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1、BRITISH STANDARDBS EN ISO 13884:2005Incorporating Amendment No. 1 to BS ISO 13884:2003 (renumbers BS ISO as BS EN ISO 13884:2005)Animal and vegetable fats and oils Determination of isolated trans isomers by infrared spectrometry The European Standard EN ISO 13884:2005 has the status of a British Sta

2、ndardICS 67.200.10g49g50g3g38g50g51g60g44g49g42g3g58g44g55g43g50g56g55g3g37g54g44g3g51g40g53g48g44g54g54g44g50g49g3g40g59g38g40g51g55g3g36g54g3g51g40g53g48g44g55g55g40g39g3g37g60g3g38g50g51g60g53g44g42g43g55g3g47g36g58BS EN ISO 13884:2005This British Standard was published under the authority of the

3、 Standards Policy and Strategy Committee on 17 July 2003 BSI 2006ISBN 0 580 42272 0National forewordThis British Standard is the official English language version of EN ISO 13884:2005. It is identical with ISO 13884:2003.The UK participation in its preparation was entrusted to Technical Committee AW

4、/307, Oil seeds animal and vegetable fats and oils, which has the responsibility to: A list of organizations represented on this committee can be obtained on request to its secretary.Cross-referencesThe British Standards which implement international or European publications referred to in this docu

5、ment may be found in the BSI Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Search” facility of the BSI Electronic Catalogue or of British Standards Online.This publication does not purport to include all the necessary provisions of a contract.

6、Users are responsible for its correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. aid enquirers to understand the text; present to the responsible international/European committee any enquiries on the interpretation, or proposals for cha

7、nge, and keep UK interests informed; monitor related international and European developments and promulgate them in the UK.Summary of pagesThis document comprises a front cover, an inside front cover, the EN ISO title page, the EN ISO foreword page, the ISO title page, pages ii and iii, a blank page

8、, pages 1 to 9 and a back cover.The BSI copyright notice displayed in this document indicates when the document was last issued.Amendments issued since publicationAmd. No. Date Comments15855 31 August 2006 Renumbers BS ISO 13884:2003 as BS EN ISO 13884:2005EUROPEAN STANDARDNORME EUROPENNEEUROPISCHE

9、NORMEN ISO 13884August 2005ICS 67.200.10English VersionAnimal and vegetable fats and oils Determination of isolatedtrans isomers by infrared spectrometry (ISO 13884:2003)Corps gras dorigines animale et vgtale Dtermination,par spectromtrie infrarouge, des isomres trans isols(ISO 13884:2003)Tierische

10、und pflanzliche Fette und le isolierter trans-Isomere durch Infarot-Spektrometrie (ISO 13884:2003)This European Standard was approved by CEN on 28 July 2005.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this EuropeanStandard the s

11、tatus of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such nationalstandards may be obtained on application to the Central Secretariat or to any CEN member.This European Standard exists in three official versions (English, French, German). A

12、version in any other language made by translationunder the responsibility of a CEN member into its own language and notified to the Central Secretariat has the same status as the officialversions.CEN members are the national standards bodies of Austria, Belgium, Cyprus, Czech Republic, Denmark, Esto

13、nia, Finland, France,Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Slovakia,Slovenia, Spain, Sweden, Switzerland and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMIT EUROPEN DE NORMALISATIONEUROPISCHES KOMITE

14、E FR NORMUNGManagement Centre: rue de Stassart, 36 B-1050 Brussels 2005 CEN All rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN ISO 13884:2005: EBestimmungForewordThe text of ISO 13884:2003 has been prepared by Technical Committee ISO/TC 34,

15、 Agricultural food products, of the International Organization for Standardization (ISO) and has been taken over as EN ISO 13884:2005 by 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 he

16、ld 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 February 2006, and conflicting national standards shall be withdrawn at the latest by February 2006. According to the CEN/CENELEC Inter

17、nal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Nether

18、lands, Norway, Poland, Portugal, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. Endorsement notice The text of ISO 13884:2003 has been approved by CEN as EN ISO 13884:2005 without any modifications. EN ISO 13884:2005Reference numberISO 13884:2003(E)OSI 3002INTERNATIONAL STANDARD

19、ISO13884First edition2003-07-01Animal and vegetable fats and oils Determination of isolated trans isomers by infrared spectrometry Corps gras dorigines animale et vgtale Dtermination, par spectromtrie infrarouge, des isomres trans isols 3002 yluJ 71 ISB EN ISO 13884:2005DPlcsid Fremia ihTs PDF file

20、may ctnoian emdebt dedyfepcaes. In ccaocnadrw eith Aebods licensilop gnic,y this file mairp eb ynted iv roweb detu slahl ton ide ebtlnu deess the typefaces whice era hml era deddebicsnede to i dnanstlaled t noeh computfrep reormign tide ehtin.g In wodlnidaot gnhis file, trapise atpecc tiereht nser e

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23、o sswrehise specified, on trap fo this lbupictaion maeb y cudorperro de tuilizi den yna form ro na ybm ynae,s lecetrinoc ro mecinahcal, inclidung tohpcoiypodna gn micrfoilm, wittuoh repmissii non writign from ietI rehSa Ot tsserdda eh ebolw or ISOs memreb i ydobn the cnuotrfo y ttseuqer ehe.r ISO ci

24、rypothg fofice saCe tsopale 65 eneG 1121-HC 02 avleT. 4 + 10 947 22 1 11 xaF0 947 22 14 + 9 74 E-mail coirypthgiso.o grWe bwww.is.o groPulbisdehi n Switlrez dnaii ISO 3002 Allr ihgtsser edrve 3002 yluJ 71 ISBiiiForeword ISO (the International Organization for Standardization) is a worldwide federati

25、on 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

26、. 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 w

27、ith 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 appr

28、oval 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 13884 was prepared by Technical Commit

29、tee ISO/TC 34, Food products, Subcommittee SC 11, Animal and vegetable fats and oils. EN ISO 13884:2005blankINTENRATIONAL TSANDADR Animal and vegetable fats and oils Determination of isolated trans isomers by infrared spectrometry 1 Scope This International Standard specifies a method for the accura

30、te determination of isolated trans bonds in natural or processed long-chain fatty acids, fatty acid esters and triglycerides with trans isomer levels W 5 %. The method is not applicable, or is applicable only with specific precautions, to fats and oils containing high levels (over 5 %) of conjugated

31、 unsaturation (e.g. tung oil), materials containing functional groups which modify the intensity of the C-H deformation about the trans double bond e.g. castor oil containing ricinoleic acid or its geometrical isomer, ricinelaidic acid (12-hydroxy-9-octadecenoic acid), mixed triglycerides having lon

32、g- and short-chain moieties (such as diacetostearin), or in general, any materials containing constituents which have functional groups which give rise to specific absorption bands at or sufficiently close to interfere with the 966 cm1band of the C-H deformation of the isolated trans double bond. NO

33、TE Dienes, such as cis-trans and trans-trans dienes, can affect the calibration. For accurate determinations on materials with trans levels below 5 %, a standardized capillary GLC method is recommended (for example, see ISO 15304). 2 Normative references The following referenced documents are indisp

34、ensable 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 661, Animal and vegetable fats and oils Preparation of test sample ISO 5509, Animal and ve

35、getable fats and oils Preparation of methyl esters of fatty acids 3 Terms and definitions For the purposes of this document, the following terms and definitions apply. 3.1 percentage of trans fatty acids % trans quantity of those substances in the sample, expressed in terms of the mass equivalent of

36、 methyl elaidate, divided by the sample mass expressed in grams per 10 ml of solvent EN ISO 13884:200514 Principle In most naturally occurring vegetable fats and oils, unsaturated constituents contain only isolated (i.e. non-conjugated) double bonds in the cis configuration. These cis bonds may be i

37、somerized to the trans configuration during extraction and processing procedures, due to oxidation, conversion during heating, and/or partial hydrogenation. Animal and marine fats and oils may contain measurable amounts of naturally occurring trans isomers. Isolated trans bonds in long-chain fatty a

38、cids, fatty acid esters and triglycerides may be measured by infrared (IR) spectrometry. An absorption band with a maximum at 966 cm1(10,3 m), arising from a C-H deformation about a trans double bond, is exhibited in the spectra of all compounds containing an isolated trans group. This band is not o

39、bserved in the spectra of the corresponding cis and saturated compounds. Measurement of the intensity of this absorption band under analytically controlled conditions is the basis for a quantitative method for the determination of the isolated trans isomer content. For higher accuracy, common interf

40、ering absorptions associated with the glycerol backbone of triglycerides and the carboxyl groups of fatty acids must be eliminated by conversion of these samples to their methyl esters prior to analysis. 5 Reagents Use only reagents of recognized analytical grade, unless otherwise specified. 5.1 Car

41、bon disulfide (CS2), dry. WARNING Prolonged breathing of carbon disulfide vapours is dangerous. This solvent should be handled only under conditions that provide adequate ventilation, preferably under a fume hood. 5.2 Primary standards: methyl elaidate and methyl oleate, with a purity of 99 %1). 6 A

42、pparatus 6.1 Infrared spectrometer (FT-IR or dispersive), capable of making measurements at 4 cm1resolution in the spectral range covering 1 050 cm1to 900 cm1. The data-handling capability of the instrument should allow conversion of spectra to absorbance, scale expansion of the x- and y-axes, and r

43、eadout of wave numbers to the nearest 1 cm1and of absorbance to the nearest 0,001 AU. FT-IR spectrometers should use TGS or DTGS detectors, or ensure linearity. 6.2 Infrared liquid sampling cells, with NaCl or KBr windows and a fixed optical path length of 1 mm. For use in null-type instruments, pai

44、rs of cells matched to within 0,01 AU are required. In split-beam type instruments with both cells filled with the solvent (5.1), electronic balance of the two beams to within these limits should be attained. 6.3 Volumetric flasks, class A, of capacities 10 ml, 25 ml and 50 ml. 6.4 Pipettes, class A

45、, of capacities 1 ml, 3 ml, 4 ml, 5 ml, 7 ml and 9 ml. 6.5 Disposable Pasteur pipettes, for filling infrared cells with the test sample. 6.6 Analytical balance, with a 60 g capacity, capable of weighing 0,2 g to an accuracy of 0,000 1 g. 1) These are available from Nu-Check-Prep, Inc., Elysian, MN,

46、USA. This information is given for the convenience of users of this International Standard and does not constitute an endorsement by ISO of these products. Equivalent products may be used if they can be shown to lead to the same results. EN ISO 13884:20052 7 Sampling Sampling is not part of the meth

47、od given in this International Standard. A recommended sampling method is given in ISO 5555. It is important that the laboratory receive a sample that is truly representative and has not been damaged or changed during transport and storage. 8 Preparation of test sample Prepare the test samples in ac

48、cordance with ISO 661. Laboratory samples of solid fats shall be completely melted on a steam bath at a temperature not more than 10 C above the melting point of the sample. The melted laboratory sample should be completely mixed before taking the test sample. Samples that appear cloudy because of t

49、he presence of water should be treated with anhydrous sodium sulfate and filtered before taking the test sample. 9 Procedure 9.1 Preparation of standards 9.1.1 Stocks solutions Weigh, to the nearest 0,000 1 g, 0,5 g 0,01 g of methyl elaidate (5.2) into a 25 ml volumetric flask (6.3). Dilute to volume with solvent (5.1), stopper and mix well. Prepare a second solution of methyl oleate (5.2) in exactly the same manner. These stock solutions have a concentration of 0,020 g/ml. Prepare a 0,002 0 g/ml stock solution