BS EN 62321-6-2015 Determination of certain substances in electrotechnical products Polybrominated biphenyls and polybrominated diphenyl ethers in polymers by gas chromatography-ma.pdf

1、BSI Standards PublicationDetermination of certain substances in electrotechnicalproductsPart 6: Polybrominated biphenyls and polybrominated diphenyl ethers in polymers by gas chromatographymass spectrometry (GC-MS)BS EN 62321-6:2015EUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN 62321-6August 2015

2、ICS 13.020; 43.040.10 Supersedes EN 62321:2009 (partially) English VersionDetermination of certain substances in electrotechnical products- Part 6: Polybrominated biphenyls and polybrominated diphenyl ethers in polymers by gas chromatography-mass spectrometry(GC-MS)(IEC 62321-6:2015)Dtermination de

3、certaines substances dans les produitslectrotechniques - Partie 6: Diphnyles polybroms etdiphnylthers polybroms dans des polymres parchromatographie en phase gazeuse-spectromtrie de masse (GC-MS)(IEC 62321-6:2015)Verfahren zur Bestimmung von bestimmten Substanzen in Produkten der Elektrotechnik - Te

4、il 6: PolybromierteBiphenyl- und Diphenylether in Polymeren durchGaschromatographie-Massenspektrometrie (GC-MS)(IEC 62321-6:2015)This European Standard was approved by CENELEC on 2015-07-10. CENELEC members are bound to comply with the CEN/CENELECInternal Regulations which stipulate the conditions f

5、or 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 to the CEN-CENELEC Management Centre or to any CENELEC member.This European Standard exists in t

6、hree official versions (English, French, German). A version in any other language made by translation under the responsibility of a CENELEC member into its own language and notified to the CEN-CENELEC Management Centre has the same status as the official versions.CENELEC members are the national ele

7、ctrotechnical committees of Austria, Belgium, Bulgaria, Croatia, Cyprus, the Czech Republic,Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia,Lithuania, Luxembourg, Malta, the Netherlands, Norway, Poland, Portugal, Rom

8、ania, Slovakia, Slovenia, Spain, Sweden, Switzerland,Turkey and the United Kingdom.European Committee for Electrotechnical StandardizationComit Europen de Normalisation ElectrotechniqueEuropisches Komitee fr Elektrotechnische NormungCEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels 20

9、15 CENELEC All rights of exploitation in any form and by any means reserved worldwide for CENELEC Members.Ref. No. EN 62321-6:2015 EBS EN 62321-6:2015BS EN 62321-6:2015 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of EN 62321-6:2015. It is identical to IEC 62321-6:

10、2015. Together with BS EN 62321-1:2013, BS EN 62321-2:2014, BS EN 62321-3-1:2014, BS EN 62321-3-2:2014, BS EN 62321-4:2014, BS EN 62321-5:2014, BS EN 62321-7-1, BS EN 62321-7-2 and BS EN 62321-8 it supersedes BS EN 62321:2009, which will be withdrawn upon publication of all parts of the BS EN 62321

11、series.The UK participation in its preparation was entrusted to Technical Committee GEL/111, Electrotechnical environment committee.A list of organizations represented on this committee can be obtained on request to its secretary.This publication does not purport to include all the necessary provisi

12、ons of a contract. Users are responsible for its correct application. The British Standards Institution 2015. Published by BSI Standards Limited 2015ISBN 978 0 580 74396 2ICS 13.020.01; 43.040.10Compliance with a British Standard cannot confer immunity from legal obligations.This British Standard wa

13、s published under the authority of the Standards Policy and Strategy Committee on 31 October 2015.Amendments/corrigenda issued since publicationDate Text affectedEUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 62321-6 August 2015 ICS 13.020; 43.040.10 Supersedes EN 62321:2009 (partially) Englis

14、h Version Determination of certain substances in electrotechnical products - Part 6: Polybrominated biphenyls and polybrominated diphenyl ethers in polymers by gas chromatography-mass spectrometry (GC-MS) (IEC 62321-6:2015) Dtermination de certaines substances dans les produits lectrotechniques - Pa

15、rtie 6: Diphnyles polybroms et diphnylthers polybroms dans des polymres par chromatographie en phase gazeuse-spectromtrie de masse (GC-MS) (IEC 62321-6:2015) Verfahren zur Bestimmung von bestimmten Substanzen in Produkten der Elektrotechnik - Teil 6: Polybromierte Biphenyl- und Diphenylether in Poly

16、meren durch Gaschromatographie-Massenspektrometrie (GC-MS) (IEC 62321-6:2015) This European Standard was approved by CENELEC on 2015-07-10. CENELEC members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of a n

17、ational 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 CENELEC member. This European Standard exists in three official versions (English, French, German)

18、. A version in any other language made by translation under the responsibility of a CENELEC member into its own language and notified to the CEN-CENELEC Management Centre has the same status as the official versions. CENELEC members are the national electrotechnical committees of Austria, Belgium, B

19、ulgaria, Croatia, Cyprus, the Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, the Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Swit

20、zerland, Turkey and the United Kingdom. European Committee for Electrotechnical Standardization Comit Europen de Normalisation Electrotechnique Europisches Komitee fr Elektrotechnische Normung CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels 2015 CENELEC All rights of exploitation in

21、 any form and by any means reserved worldwide for CENELEC Members. Ref. No. EN 62321-6:2015 E BS EN 62321-6:2015EN 62321-6:2015 2 European foreword The text of document 111/368/FDIS, future edition 1 of IEC 62321-6, prepared by IEC/TC 111 “Environmental standardization for electrical and electronic

22、products and systems“ was submitted to the IEC-CENELEC parallel vote and approved by CENELEC as EN 62321-6:2015. The following dates are fixed: latest date by which the document has to be implemented at national level by publication of an identical national standard or by endorsement (dop) 2016-04-1

23、0 latest date by which the national standards conflicting with the document have to be withdrawn (dow) 2018-07-10 This document supersedes EN 62321:2009 (partially). Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CENELEC and/or C

24、EN shall not be held responsible for identifying any or all such patent rights. Endorsement notice The text of the International Standard IEC 62321-6.2015 was approved by CENELEC as a European Standard without any modification. BS EN 62321-6:2015EN 62321-6:2015 3 Annex ZA (normative) Normative refer

25、ences to international publications with their corresponding European publications The following documents, in whole or in part, are normatively referenced in this document and are indispensable for its application. For dated references, only the edition cited applies. For undated references, the la

26、test edition of the referenced document (including any amendments) applies. NOTE 1 When an International Publication has been modified by common modifications, indicated by (mod), the relevant EN/HD applies. NOTE 2 Up-to-date information on the latest versions of the European Standards listed in thi

27、s annex is available here: www.cenelec.eu Publication Year Title EN/HD Year IEC 62321 2008 Electrotechnical products - Determination of levels of six regulated substances (lead, mercury, cadmium, hexavalent chromium, polybrominated biphenyls, polybrominated diphenyl ethers) EN 62321 2009 IEC 62321-1

28、 2013 Determination of certain substances in electrotechnical products - Part 1: Introduction and overview EN 62321-1 2013 IEC 62321-2 2013 Determination of certain substances in electrotechnical products - Part 2: Disassembly, disjunction and mechanical sample preparation EN 62321-2 2014 BS EN 6232

29、1-6:2015EN 62321-6:2015 2 European foreword The text of document 111/368/FDIS, future edition 1 of IEC 62321-6, prepared by IEC/TC 111 “Environmental standardization for electrical and electronic products and systems“ was submitted to the IEC-CENELEC parallel vote and approved by CENELEC as EN 62321

30、-6:2015. The following dates are fixed: latest date by which the document has to be implemented at national level by publication of an identical national standard or by endorsement (dop) 2016-04-10 latest date by which the national standards conflicting with the document have to be withdrawn (dow) 2

31、018-07-10 This document supersedes EN 62321:2009 (partially). Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CENELEC and/or CEN shall not be held responsible for identifying any or all such patent rights. Endorsement notice The t

32、ext of the International Standard IEC 62321-6.2015 was approved by CENELEC as a European Standard without any modification. BS EN 62321-6:2015EN 62321-6:2015 3 Annex ZA (normative) Normative references to international publications with their corresponding European publications The following documen

33、ts, in whole or in part, 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. NOTE 1 When an International

34、 Publication has been modified by common modifications, indicated by (mod), the relevant EN/HD applies. NOTE 2 Up-to-date information on the latest versions of the European Standards listed in this annex is available here: www.cenelec.eu Publication Year Title EN/HD Year IEC 62321 2008 Electrotechni

35、cal products - Determination of levels of six regulated substances (lead, mercury, cadmium, hexavalent chromium, polybrominated biphenyls, polybrominated diphenyl ethers) EN 62321 2009 IEC 62321-1 2013 Determination of certain substances in electrotechnical products - Part 1: Introduction and overvi

36、ew EN 62321-1 2013 IEC 62321-2 2013 Determination of certain substances in electrotechnical products - Part 2: Disassembly, disjunction and mechanical sample preparation EN 62321-2 2014 BS EN 62321-6:2015 2 IEC 62321-6:2015 IEC 2015 CONTENTS FOREWORD . 6 INTRODUCTION . 8 1 Scope 9 2 Normative refere

37、nces. 9 3 Terms, definitions and abbreviations 10 3.1 Terms and definitions 10 3.2 Abbreviations 10 4 Principle 11 5 Reagents 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-

38、extraction of the Soxhlet extractors 13 8.2.3 Extraction 13 8.2.4 Alternative extraction procedures for soluble polymers 13 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), P

39、BDE (1 g/ml for each congener) and surrogate standard (1 g/ml) stock solution 18 8.5.3 Standard solutions . 18 9 Calculation 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 assur

40、ance and control 22 11.1 Resolution. 22 11.2 Performance . 23 11.3 Limit of detection (LOD) or method detection limit (MDL) 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 Princi

41、ple . 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 BS EN 62321-6:2015IEC 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.

42、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 . 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

43、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 limits 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 p

44、olymers by high-pressure liquid chromatography Ultra violet detection (HPLC-UV) . 38 C.1 Principle . 38 C.2 Reagents and materials . 38 C.3 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. 4

45、0 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.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

46、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 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 4

47、8 BS EN 62321-6:2015 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 Reagents and materials . 11 6 Apparatus 11 7 Sampling . 12 8 Proced

48、ure . 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 13 8.2.5 Addition of the internal standard (IS) 14 8.3 Instrume

49、ntal 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 Calculation 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 detec