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    IEC 62321-6-2015 Determination of certain substances in electrotechnical products - Part 6 Polybrominated biphenyls and polybrominated diphenyl ethers in polyme.pdf

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    IEC 62321-6-2015 Determination of certain substances in electrotechnical products - Part 6 Polybrominated biphenyls and polybrominated diphenyl ethers in polyme.pdf

    1、 IEC 62321-6 Edition 1.0 2015-06 INTERNATIONAL STANDARD NORME INTERNATIONALE Determination of certain substances in electrotechnical products Part 6: Polybrominated biphenyls and polybrominated diphenyl ethers in polymers by gas chromatographymass spectrometry (GC-MS) Dtermination de certaines subst

    2、ances dans les produits lectrotechniques Partie 6: Diphnyles polybroms et diphnylthers polybroms dans des polymres par chromatographie en phase gazeusespectromtrie de masse (GC-MS) IEC 62321-6:2015-06(en-fr) colour inside THIS PUBLICATION IS COPYRIGHT PROTECTED Copyright 2015 IEC, Geneva, Switzerlan

    3、d All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means, electronic or mechanical, including photocopying and microfilm, without permission in writing from either IEC or IECs member National Committee in the country of

    4、the requester. If you have any questions about IEC copyright or have an enquiry about obtaining additional rights to this publication, please contact the address below or your local IEC member National Committee for further information. Droits de reproduction rservs. Sauf indication contraire, aucun

    5、e partie de cette publication ne peut tre reproduite ni utilise sous quelque forme que ce soit et par aucun procd, lectronique ou mcanique, y compris la photocopie et les microfilms, sans laccord crit de lIEC ou du Comit national de lIEC du pays du demandeur. Si vous avez des questions sur le copyri

    6、ght de lIEC ou si vous dsirez obtenir des droits supplmentaires sur cette publication, utilisez les coordonnes ci-aprs ou contactez le Comit national de lIEC de votre pays de rsidence. IEC Central Office Tel.: +41 22 919 02 11 3, rue de Varemb Fax: +41 22 919 03 00 CH-1211 Geneva 20 infoiec.ch Switz

    7、erland www.iec.ch About the IEC The International Electrotechnical Commission (IEC) is the leading global organization that prepares and publishes International Standards for all electrical, electronic and related technologies. About IEC publications The technical content of IEC publications is kept

    8、 under constant review by the IEC. Please make sure that you have the latest edition, a corrigenda or an amendment might have been published. IEC Catalogue - webstore.iec.ch/catalogue The stand-alone application for consulting the entire bibliographical information on IEC International Standards, Te

    9、chnical Specifications, Technical Reports and other documents. Available for PC, Mac OS, Android Tablets and iPad. IEC publications search - www.iec.ch/searchpub The advanced search enables to find IEC publications by a variety of criteria (reference number, text, technical committee,). It also give

    10、s information on projects, replaced and withdrawn publications. IEC Just Published - webstore.iec.ch/justpublished Stay up to date on all new IEC publications. Just Published details all new publications released. Available online and also once a month by email. Electropedia - www.electropedia.org T

    11、he worlds leading online dictionary of electronic and electrical terms containing more than 30 000 terms and definitions in English and French, with equivalent terms in 15 additional languages. Also known as the International Electrotechnical Vocabulary (IEV) online. IEC Glossary - std.iec.ch/glossa

    12、ry More than 60 000 electrotechnical terminology entries in English and French extracted from the Terms and Definitions clause of IEC publications issued since 2002. Some entries have been collected from earlier publications of IEC TC 37, 77, 86 and CISPR. IEC Customer Service Centre - webstore.iec.

    13、ch/csc If you wish to give us your feedback on this publication or need further assistance, please contact the Customer Service Centre: csciec.ch. A propos de lIEC La Commission Electrotechnique Internationale (IEC) est la premire organisation mondiale qui labore et publie des Normes internationales

    14、 pour tout ce qui a trait llectricit, llectronique et aux technologies apparentes. A propos des publications IEC Le contenu technique des publications IEC est constamment revu. Veuillez vous assurer que vous possdez ldition la plus rcente, un corrigendum ou amendement peut avoir t publi. Catalogue I

    15、EC - webstore.iec.ch/catalogue Application autonome pour consulter tous les renseignements bibliographiques sur les Normes internationales, Spcifications techniques, Rapports techniques et autres documents de lIEC. Disponible pour PC, Mac OS, tablettes Android et iPad. Recherche de publications IEC

    16、- www.iec.ch/searchpub La recherche avance permet de trouver des publications IEC en utilisant diffrents critres (numro de rfrence, texte, comit dtudes,). Elle donne aussi des informations sur les projets et les publications remplaces ou retires. IEC Just Published - webstore.iec.ch/justpublished Re

    17、stez inform sur les nouvelles publications IEC. Just Published dtaille les nouvelles publications parues. Disponible en ligne et aussi une fois par mois par email. Electropedia - www.electropedia.org Le premier dictionnaire en ligne de termes lectroniques et lectriques. Il contient plus de 30 000 te

    18、rmes et dfinitions en anglais et en franais, ainsi que les termes quivalents dans 15 langues additionnelles. Egalement appel Vocabulaire Electrotechnique International (IEV) en ligne. Glossaire IEC - std.iec.ch/glossary Plus de 60 000 entres terminologiques lectrotechniques, en anglais et en franais

    19、, extraites des articles Termes et Dfinitions des publications IEC parues depuis 2002. Plus certaines entres antrieures extraites des publications des CE 37, 77, 86 et CISPR de lIEC. Service Clients - webstore.iec.ch/csc Si vous dsirez nous donner des commentaires sur cette publication ou si vous av

    20、ez des questions contactez-nous: csciec.ch. IEC 62321-6 Edition 1.0 2015-06 INTERNATIONAL STANDARD NORME INTERNATIONALE Determination of certain substances in electrotechnical products Part 6: Polybrominated biphenyls and polybrominated diphenyl ethers in polymers by gas chromatographymass spectrome

    21、try (GC-MS) Dtermination de certaines substances dans les produits lectrotechniques Partie 6: Diphnyles polybroms et diphnylthers polybroms dans des polymres par chromatographie en phase gazeusespectromtrie de masse (GC-MS) INTERNATIONAL ELECTROTECHNICAL COMMISSION COMMISSION ELECTROTECHNIQUE INTERN

    22、ATIONALE ICS 13.020; 43.040.10 ISBN 978-2-8322-2689-6 Registered trademark of the International Electrotechnical Commission Marque dpose de la Commission Electrotechnique Internationale Warning! Make sure that you obtained this publication from an authorized distributor. Attention! Veuillez vous ass

    23、urer que vous avez obtenu cette publication via un distributeur agr. colour inside 2 IEC 62321-6:2015 IEC 2015 CONTENTS FOREWORD . 6 INTRODUCTION . 8 1 Scope 9 2 Normative references. 9 3 Terms, definitions and abbreviations 10 3.1 Terms and definitions 10 3.2 Abbreviations 10 4 Principle 11 5 Reage

    24、nts and materials . 11 6 Apparatus 11 7 Sampling . 12 8 Procedure . 12 8.1 General instructions for the analysis 12 8.2 Sample preparation . 12 8.2.1 Stock solution 12 8.2.2 Pre-extraction of the Soxhlet extractors 13 8.2.3 Extraction 13 8.2.4 Alternative extraction procedures for soluble polymers 1

    25、3 8.2.5 Addition of the internal standard (IS) 14 8.3 Instrumental parameters 14 8.4 Calibrants . 16 8.5 Calibration 17 8.5.1 General . 17 8.5.2 PBB (1 g/ml for each congener), PBDE (1 g/ml for each congener) and surrogate standard (1 g/ml) stock solution 18 8.5.3 Standard solutions . 18 9 Calculati

    26、on of PBB and PBDE concentration 19 9.1 General . 19 9.2 Calculation 19 10 Precision . 21 10.1 Threshold judgement . 21 10.2 Repeatability and reproducibility 22 11 Quality assurance and control 22 11.1 Resolution. 22 11.2 Performance . 23 11.3 Limit of detection (LOD) or method detection limit (MDL

    27、) and limit of quantification (LOQ) 24 12 Test report. 25 Annex A (informative) Determination of PBB and PBDE in polymers by ion attachment mass spectrometry (IAMS) 26 A.1 Principle . 26 A.2 Reagents and materials . 26 A.3 Apparatus . 26 A.4 Sampling. 27 A.4.1 General . 27 A.4.2 Qualitative stage 27

    28、 IEC 62321-6:2015 IEC 2015 3 A.4.3 Semi-quantitative stage 27 A.5 Procedure . 27 A.5.1 General instructions for the analysis . 27 A.5.2 Sample preparation 27 A.5.3 Instrumental parameters. 28 A.5.4 Calibrants 29 A.5.5 Calibration . 29 A.6 Calculation of PBB and PBDE concentration 30 A.6.1 General .

    29、30 A.6.2 Calculation . 31 A.6.3 Judgement of ambiguous spectrum 32 A.7 Precision . 34 A.7.1 Threshold judgement 34 A.7.2 Repeatability and reproducibility . 34 A.8 Quality assurance and control . 35 A.8.1 Sensitivity 35 A.8.2 Recovery . 35 A.8.3 Blank test 36 A.8.4 Limits of detection (LOD) and limi

    30、ts of quantification (LOQ) 36 A.9 Test report 36 Annex B (informative) Diagram of an IAMS instrument 37 Annex C (informative) Determination of PBB and PBDE in polymers by high-pressure liquid chromatography Ultra violet detection (HPLC-UV) . 38 C.1 Principle . 38 C.2 Reagents and materials . 38 C.3

    31、Apparatus . 38 C.4 Sampling. 39 C.5 Procedure . 39 C.5.1 General instructions for the analysis . 39 C.5.2 Sample preparation 39 C.5.3 Instrumental parameters. 40 C.5.4 Calibrants 40 C.6 Calibration 41 C.6.1 General . 41 C.6.2 Standard solutions . 41 C.7 Calculation of PBB and PBDE concentration 42 C

    32、.7.1 General . 42 C.7.2 Calculation . 42 C.8 Precision . 43 C.8.1 Threshold judgement 43 C.8.2 Repeatability and reproducibility . 43 C.9 Quality assurance and control . 44 C.9.1 Standards spike recovery . 44 C.9.2 Internal control samples and blanks 44 C.9.3 Limits of detection (LOD) and limits of

    33、quantification (LOQ) 45 C.10 Test report 45 Annex D (informative) Examples of chromatograms at suggested conditions . 46 D.1 GC-MS method . 46 D.2 IAMS method 48 4 IEC 62321-6:2015 IEC 2015 D.3 HPLC-UV method 52 Annex E (informative) Example applicability of the IAMS, HPLC and GC-MS test methods . 5

    34、3 Annex F (informative) Results of international interlaboratory study 4B (IIS4B) . 54 Bibliography . 57 Figure A.1 Mass spectra of Deca BB and TBBA obtained in scan mode and profile mode 33 Figure A.2 Identification of Tetra-BDE and Penta-BDE by isotope pattern recognition 33 Figure B.1 Diagram of

    35、an IAMS instrument . 37 Figure D.1 Total ion chromatogram of PBDE mixture, BDE-1 to BDE-206 (5 g/ml), BDE-209 (50 g/ml) 47 Figure D.2 Total ion chromatogram of PBB mixture (3,5 g/ml) . 47 Figure D.3 Total ion chromatogram of PBB and PBDE mixtures (BDE-1 to BDE-206 5 g/ml, BDE-209 50 g/ml, PBBs 3,5 g

    36、/ml) . 48 Figure D.4 Mass spectrum of each PBDE congener by IAMS-1 (TriBDE to HexaBDE) . 49 Figure D.5 Mass spectrum of each PBDE congener by IAMS-2 (HeptaBDE to DecaBDE) 49 Figure D.6 Mass spectra of technical OctaBDE(a) as mixture 50 Figure D.7 Temperature-programmed chromatography of each PBDE co

    37、ngener in the quantitative analysis of the reference material (ERM EC-590) 51 Figure D.8 Chromatogram and UV spectrum of DecaBDE . 52 Figure D.9 Chromatogram and UV spectrum of decaBB 52 Figure D.10 Chromatogram and UV Spectrum of OctaBDE 52 Figure D.11 Chromatogram and UV spectrum of octaBB . 52 Fi

    38、gure E.1 Flow chart, example applicability of the IAMS, HPLC and GC-MS test methods . 53 Table 1 Matrix spiking solution . 13 Table 2 Reference masses for the quantification of PBBs . 15 Table 3 Reference masses for the quantification of PBDEs . 16 Table 4 Example list of commercially available cali

    39、bration congeners considered suitable for this analysis 17 Table 5 Calibration solutions of PBBs and PBDEs 18 Table 6 IIS4B threshold judgement . 21 Table 7 IIS4B repeatability and reproducibility 22 Table 8 Example calculation . 23 Table A.1 Measurement condition of IAMS . 28 Table A.2 Example list

    40、 of commercially available calibrant reference materials considered suitable for this analysis 29 Table A.3 Example PBDE response factor standards (i.e. BDE-WD (Wellington), solution/ mixture of polybrominated diphenyl ether congeners(PBDE) . 29 Table A.4 Calibrant amounts 30 Table A.5 Response fact

    41、or of each PBDE congener a32 Table A.6 IIS4B threshold judgement 34 Table A.7 IIS4B repeatability and reproducibility . 35 IEC 62321-6:2015 IEC 2015 5 Table C.1 Example list of commercially available technical calibration mixtures considered suitable for this analysis 41 Table C.2 Standard stock sol

    42、ution concentrations (mg/100 ml) 41 Table C.3 IIS4B threshold judgement . 43 Table C.4 IIS4B Repeatability and reproducibility 44 Table D.1 PBB and PBDE congeners in the mixture 46 Table F.1 Statistical Data for GC-MS 54 Table F.2 Statistical data for IAMS . 55 Table F.3 Statistical data for HPLC-UV

    43、 . 56 6 IEC 62321-6:2015 IEC 2015 INTERNATIONAL ELECTROTECHNICAL COMMISSION _ DETERMINATION OF CERTAIN SUBSTANCES IN ELECTROTECHNICAL PRODUCTS Part 6: Polybrominated biphenyls and polybrominated diphenyl ethers in polymers by gas chromatographymass spectrometry (GC-MS) FOREWORD 1) The International

    44、Electrotechnical Commission (IEC) is a worldwide organization for standardization comprising all national electrotechnical committees (IEC National Committees). The object of IEC is to promote international co-operation on all questions concerning standardization in the electrical and electronic fie

    45、lds. To this end and in addition to other activities, IEC publishes International Standards, Technical Specifications, Technical Reports, Publicly Available Specifications (PAS) and Guides (hereafter referred to as “IEC Publication(s)”). Their preparation is entrusted to technical committees; any IE

    46、C National Committee interested in the subject dealt with may participate in this preparatory work. International, governmental and non- governmental organizations liaising with the IEC also participate in this preparation. IEC collaborates closely with the International Organization for Standardiza

    47、tion (ISO) in accordance with conditions determined by agreement between the two organizations. 2) The formal decisions or agreements of IEC on technical matters express, as nearly as possible, an international consensus of opinion on the relevant subjects since each technical committee has represen

    48、tation from all interested IEC National Committees. 3) IEC Publications have the form of recommendations for international use and are accepted by IEC National Committees in that sense. While all reasonable efforts are made to ensure that the technical content of IEC Publications is accurate, IEC ca

    49、nnot be held responsible for the way in which they are used or for any misinterpretation by any end user. 4) In order to promote international uniformity, IEC National Committees undertake to apply IEC Publications transparently to the maximum extent possible in their national and regional publications. Any divergence between any IEC Publication


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