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
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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
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