1、 IEC 62321-8 Edition 1.0 2017-03 INTERNATIONAL STANDARD NORME INTERNATIONALE Determination of certain substances in electrotechnical products Part 8: Phthalates in polymers by gas chromatography-mass spectrometry (GC-MS), gas chromatography-mass spectrometry using a pyrolyzer/thermal desorption acce
2、ssory (Py/TD-GC-MS) Dtermination de certaines substances dans les produits lectrotechniques Partie 8: Analyse des phtalates dans les polymres par chromatographie en phase gazeuse-spectromtrie de masse (GC-MS), chromatographie en phase gazeuse-spectromtrie de masse par pyrolyse/thermodsorption (Py/TD
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20、 vous dsirez nous donner des commentaires sur cette publication ou si vous avez des questions contactez-nous: csciec.ch. IEC 62321-8 Edition 1.0 2017-03 INTERNATIONAL STANDARD NORME INTERNATIONALE Determination of certain substances in electrotechnical products Part 8: Phthalates in polymers by gas
21、chromatography-mass spectrometry (GC-MS), gas chromatography-mass spectrometry using a pyrolyzer/thermal desorption accessory (Py/TD-GC-MS) Dtermination de certaines substances dans les produits lectrotechniques Partie 8: Analyse des phtalates dans les polymres par chromatographie en phase gazeuse-s
22、pectromtrie de masse (GC-MS), chromatographie en phase gazeuse-spectromtrie de masse par pyrolyse/thermodsorption (Py/TD-GC-MS) INTERNATIONAL ELECTROTECHNICAL COMMISSION COMMISSION ELECTROTECHNIQUE INTERNATIONALE ICS 31.020; 71.040.50 ISBN 978-2-8322-4144-8 Registered trademark of the International
23、Electrotechnical Commission Marque dpose de la Commission Electrotechnique Internationale Warning! Make sure that you obtained this publication from an authorized distributor. Attention! Veuillez vous assurer que vous avez obtenu cette publication via un distributeur agr. 2 IEC 62321-8:2017 IEC 2017
24、 CONTENTS FOREWORD . 6 INTRODUCTION . 8 1 Scope 9 2 Normative references 9 3 Terms, definitions and abbreviated terms 10 3.1 Terms and definitions 10 3.2 Abbreviated terms . 10 4 Principle 11 5 Reagents and materials . 11 5.1 GC-MS method . 11 5.2 Py/TD-GC-MS method 12 6 Apparatus 12 6.1 GC-MS metho
25、d . 12 6.2 Py/TD-GC-MS method 13 7 Sampling . 14 7.1 General . 14 7.2 GC-MS method . 14 7.3 Py/TD-GC-MS method 14 8 Procedure 14 8.1 General instructions for the analysis . 14 8.1.1 Overview . 14 8.1.2 GC-MS method 14 8.1.3 Py/TD-GC-MS method . 14 8.2 Sample preparation . 15 8.2.1 GC-MS method 15 8.
26、2.2 Py/TD-GC-MS method . 16 8.3 Instrumental parameters . 16 8.3.1 GC-MS method 16 8.3.2 Py/TD-GC-MS method . 18 8.4 Calibrants . 18 8.5 Calibration 19 8.5.1 GC-MS method 19 8.5.2 Py/TD-GC-MS method . 20 9 Calculation of phthalate concentration . 21 9.1 GC-MS method . 21 9.2 Py/TD-GC-MS method 22 10
27、 Precision . 23 10.1 GC-MS method . 23 10.1.1 Threshold judgement . 23 10.1.2 Repeatability and reproducibility 24 10.2 Py/TD-GC-MS method 25 10.2.1 Screening judgement . 25 10.2.2 Repeatability and reproducibility 26 11 Quality assurance and control . 27 11.1 General . 27 IEC 62321-8:2017 IEC 2017
28、3 11.2 GC-MS method . 27 11.2.1 Performance 27 11.2.2 Limit of detection (LOD) or method detection limit (MDL) and limit of quantification (LOQ) 28 11.3 Py/TD-GC-MS method 29 11.3.1 Sensitivity 29 11.3.2 Blank test 29 11.3.3 Limit of detection (LOD) or method detection limit (MDL) and limit of quant
29、ification (LOQ) 29 12 Test report . 30 Annex A (informative) Determination of phthalates in polymers by ion attachment mass spectrometry (IAMS) 31 A.1 Principle . 31 A.2 Reagents and materials 31 A.3 Apparatus . 31 A.4 Sampling. 32 A.5 Procedure . 32 A.5.1 General instructions for the analysis 32 A.
30、5.2 Sample preparation . 32 A.5.3 Instrumental parameters 33 A.5.4 Calibrants 34 A.5.5 Calibration . 34 A.6 Calculation of phthalates concentration . 35 A.7 Quality assurance and control . 35 A.7.1 General . 35 A.7.2 Sensitivity 35 A.7.3 Recovery . 35 A.7.4 Blank test 36 A.7.5 Limit of detection (LO
31、D) or method detection limit (MDL) and limit of quantification (LOQ) 37 A.8 Test report 37 Annex B (informative) Determination of phthalates in polymers by liquid chromatography-mass spectrometry(LC-MS) 38 B.1 Principle . 38 B.2 Reagents and materials 38 B.3 Apparatus . 38 B.4 Sampling. 39 B.5 Proce
32、dure . 39 B.5.1 General instructions for the analysis 39 B.5.2 Sample preparation . 39 B.5.3 Instrumental parameters 40 B.5.4 Calibrants 42 B.5.5 Calibration . 42 B.6 Calculation of phthalates concentration . 43 B.7 Quality assurance and control . 44 B.7.1 General . 44 B.7.2 Performance 44 B.7.3 Lim
33、it of detection (LOD) or method detection limit (MDL) and limit of quantification (LOQ) 44 B.8 Test report 45 4 IEC 62321-8:2017 IEC 2017 Annex C (informative) Examples of chromatograms at suggested conditions . 46 C.1 GC-MS method . 46 C.2 Py/TD-GC-MS method 47 C.3 LC-MS method 47 C.4 IAMS method 4
34、8 Annex D (informative) Verification of the EGA thermal desorption zone . 51 Annex E (informative) Example of IAMS and Py/TD-GC-MS instruments 52 Annex F (informative) Example of false positive detection of phthalates . 54 Annex G (informative) Examples of sample preparation for quantitative analysi
35、s of phthalates by GC-MS 55 G.1 General . 55 G.2 Soxhlet extraction of phthalates using proper organic solvents . 55 Annex H (informative) Extraction of phthalates by dissolution in THF using sonication and precipitation of polymer matrix . 58 Annex I (informative) Commercially available reference m
36、aterials considered suitable for GC-MS and Py/TD-GC-MS. 60 I.1 GC-MS 60 I.2 Py/TD-GC-MS . 60 Annex J (informative) Commercially available capillary columns considered suitable for GC-MS and Py-GC-MS 62 Annex K (informative) Labware cleaning procedure for phthalate testing 63 K.1 With the use of a fu
37、rnace (non-volumetric glassware only) 63 K.2 Without the use of a furnace (glassware and plastic-ware) 63 K.3 Estimation of cleanness of the inner areas of volumetric glassware 64 Annex L (informative) Results of international inter-laboratory study 5 . 65 Annex M (informative) Sample analysis seque
38、nce 70 M.1 GC-MS 70 Annex N (informative) Flow chart . 71 Bibliography 72 Figure C.1 Total ion current chromatogram of each phthalate (10 g/ml, 1 l, splitless) . 46 Figure C.2 Extracted ion chromatogram of DINP (10 g/ml, 1 l, splitless) . 46 Figure C.3 Extracted ion chromatogram of DIDP (10 g/ml, 1
39、l, splitless) . 47 Figure C.4 Total ion current chromatogram of 100 g/ml of phthalate mixture by Py/TD-GC-MS . 47 Figure C.5 Total ion current chromatogram of 5 g/ml of phthalate mixture by LC-MS 48 Figure C.6 Mass spectrum of each phthalate by IAMS . 49 Figure C.7 Total ion current chromatogram of
40、each absolute amount (0,08 g) of phthalate mixture by IAMS 50 Figure C.8 Total ion current chromatogram of approximately 0,3 mg of PVC which contains 300 mg/kg of each phthalate mixture by IAMS (Absolute amount: 0,09 g) . 50 Figure D.1 Example of EGA thermogram of a PVC sample containing phthalates
41、. 51 Figure E.1 Example of IAMS instrument . 52 Figure E.2 Example of Py/TD-GC-MS instrument . 53 Figure F.1 Typical laboratory wares made of plastic materials that may cause phthalate contamination 54 IEC 62321-8:2017 IEC 2017 5 Figure F.2 Example of a chromatogram of a blank solvent (THF) in a pla
42、stic bottle showing DEHP contamination. 54 Figure G.1 Recovery ratios of Di-(2-ethylhexyl) phthalate using Soxhlet extraction with different organic solvents . 57 Figure G.2 Comparison of recovery ratios of phthalates using different extracting conditions . 57 Figure I.1 Sample preparation of refere
43、nce materials . 61 Figure N.1 Flow chart for screening step and quantitative step 71 Table 1 Measurement condition of GC-MS . 17 Table 2 Reference masses for the quantification of each phthalate 17 Table 3 Measurement condition of Py/TD-GC-MS 18 Table 4 Calibration standard solution of phthalates 19
44、 Table 5 IIS5 Threshold judgement 23 Table 6 IIS5 Repeatability and reproducibility 24 Table 7 IIS5 screening and threshold judgement 25 Table 8 IIS5 Repeatability and reproducibility 26 Table A.1 Measurement condition of IAMS . 34 Table A.2 Certified value of constituent phthalates in KRISS CRM 113
45、-03-006 . 36 Table B.1 Measurement condition of LC-MS 42 Table B.2 Standard stock solution concentrations 43 Table G.1 Recovery ratios of phthalates according to different Soxhlet extraction times (extracting solvent: n-hexane) . 56 Table H.1 Comparison of the efficiency of the sample preparation me
46、thod of dissolution in THF using sonication and precipitation of polymeric matrix with that of Soxhlet extraction for soluble sample 58 Table H.2 Comparison of the efficiency of the sample preparation method of dissolution in THF using sonication and precipitation of polymeric matrix with that of So
47、xhlet extraction for insoluble samples . 59 Table I.1 Example list of commercially available reference solutions considered suitable for GC-MS . 60 Table I.2 Example list of commercially available reference materials considered suitable for Py/TD-GC-MS. 61 Table J.1 Example list of commercially avai
48、lable capillary columns considered suitable for GC-MS and Py-GC-MS analysis . 62 Table L.1 Statistical data for Py/TD-GC-MS . 65 Table L.2 Statistical data for GC-MS 67 Table L.3 Statistical data for IAMS . 68 Table L.4 Statistical Data For LC-MS . 69 Table M.1 Sample analysis sequence for GC-MS ana
49、lysis . 70 Table M.2 Sample analysis sequence for Py/TD-GC-MS analysis 70 6 IEC 62321-8:2017 IEC 2017 INTERNATIONAL ELECTROTECHNICAL COMMISSION _ DETERMINATION OF CERTAIN SUBSTANCES IN ELECTROTECHNICAL PRODUCTS Part 8: Phthalates in polymers by gas chromatography-mass spectrometry (GC-MS), gas chromatography-mass spectrometry using a pyrolyzer/thermal d
