BS EN 62321-8:2017
$215.11
Determination of certain substances in electrotechnical products – Phthalates in polymers by gas chromatography-mass spectrometry (GC-MS), gas chromatography-mass spectrometry using a pyrolyzer/thermal desorption accessory (Py/TD-GC-MS)
| Published By | Publication Date | Number of Pages |
| BSI | 2017 | 80 |
This part of IEC 62321 specifies two normative and two informative techniques for the determination of di-isobutyl phthalate (DIBP), di-n-butyl phthalate (DBP), benzylbutyl phthalate (BBP), di-(2-ethylhexyl) phthalate (DEHP), di-n-octyl phthalate (DNOP), di-isononyl phthalate (DINP) and di-iso-decyl phthalate (DIDP) in polymers of electrotechnical products.
Gas chromatography-mass spectrometry (GC-MS) and gas chromatography-mass spectrometry (Py/TD-GC-MS) techniques are described in the normative part of this document.
The GC-MS method is considered the referee technique for the quantitative determination of DIBP, DBP, BBP, DEHP, DNOP, DINP and DIDP in the range of 50 mg/kg to 2 000 mg/kg.
The GC-MS coupled with a pyrolyzer/thermal desorption (TD) accessory is suitable for screening and semi-quantitative analysis of DIBP, DBP, BBP, DEHP, DNOP, DINP, and DIDP in polymers that are used as parts of the electrotechnical products in the range of 100 mg/kg to 2 000 mg/kg.
The IAMS technique is suitable for screening and semi-quantitative analysis of DIBP, DBP, BBP, DEHP, DNOP, DINP, and DIDP. Determination of DBP and DIBP, DEHP and DNOP by IAMS has not been established due to peak and mass spectral resolution limitations.
The LC-MS technique is limited to the determination of of BBP, DEHP, DNOP, DINP, and DIDP. Determination of DBP and DIBP by LC-MS has not been established due to peak and mass spectral resolution limitations.
A flow chart depicting how the normative Py/TD-GC-MS and GC-MS methods and informative methods using ion attachment mass spectrometry (IAMS) coupled with direct injection probe (DIP) and liquid chromatography-mass spectrometry (LC-MS) can be used are provided in annexes of this document.
These four test methods have been evaluated by the test of PE (polyethylene) and PVC (polyvinyl chloride) materials containing individual phthalates between ~450 mg/kg to 30 000 mg/kg as depicted in the normative and informative parts of this document. The use of the four methods described in this document for other polymer types, phthalate compounds or concentration ranges other than those specified above has not been specifically evaluated.
PDF Catalog
| PDF Pages | PDF Title |
|---|---|
| 2 | National foreword |
| 7 | English CONTENTS |
| 11 | FOREWORD |
| 13 | INTRODUCTION |
| 14 | 1 Scope 2 Normative references |
| 15 | 3 Terms, definitions and abbreviated terms 3.1 Terms and definitions 3.2 Abbreviated terms |
| 16 | 4 Principle 5 Reagents and materials 5.1 GC-MS method |
| 17 | 5.2 Py/TD-GC-MS method 6 Apparatus 6.1 GC-MS method |
| 18 | 6.2 Py/TD-GC-MS method |
| 19 | 7 Sampling 7.1 General 7.2 GC-MS method 7.3 Py/TD-GC-MS method 8 Procedure 8.1 General instructions for the analysis 8.1.1 Overview 8.1.2 GC-MS method 8.1.3 Py/TD-GC-MS method |
| 20 | 8.2 Sample preparation 8.2.1 GC-MS method |
| 21 | 8.2.2 Py/TD-GC-MS method 8.3 Instrumental parameters 8.3.1 GC-MS method |
| 22 | Tables Table 1 – Measurement condition of GC-MS Table 2 – Reference masses for the quantification of each phthalate |
| 23 | 8.3.2 Py/TD-GC-MS method 8.4 Calibrants Table 3 – Measurement condition of Py/TD-GC-MS |
| 24 | 8.5 Calibration 8.5.1 GC-MS method Table 4 – Calibration standard solution of phthalates |
| 25 | 8.5.2 Py/TD-GC-MS method |
| 26 | 9 Calculation of phthalate concentration 9.1 GC-MS method |
| 27 | 9.2 Py/TD-GC-MS method |
| 28 | 10 Precision 10.1 GC-MS method 10.1.1 Threshold judgement Table 5 – IIS5 Threshold judgement |
| 29 | 10.1.2 Repeatability and reproducibility Table 6 – IIS5 Repeatability and reproducibility |
| 30 | 10.2 Py/TD-GC-MS method 10.2.1 Screening judgement Table 7 – IIS5 screening and threshold judgement |
| 31 | 10.2.2 Repeatability and reproducibility Table 8 – IIS5 Repeatability and reproducibility |
| 32 | 11 Quality assurance and control 11.1 General 11.2 GC-MS method 11.2.1 Performance |
| 33 | 11.2.2 Limit of detection (LOD) or method detection limit (MDL) and limit of quantification (LOQ) |
| 34 | 11.3 Py/TD-GC-MS method 11.3.1 Sensitivity 11.3.2 Blank test 11.3.3 Limit of detection (LOD) or method detection limit (MDL) and limit of quantification (LOQ) |
| 35 | 12 Test report |
| 36 | Annex A (informative)Determination of phthalates in polymers byion attachment mass spectrometry (IAMS) A.1 Principle A.2 Reagents and materials A.3 Apparatus |
| 37 | A.4 Sampling A.5 Procedure A.5.1 General instructions for the analysis A.5.2 Sample preparation |
| 38 | A.5.3 Instrumental parameters |
| 39 | A.5.4 Calibrants A.5.5 Calibration Table A.1 – Measurement condition of IAMS |
| 40 | A.6 Calculation of phthalates concentration A.7 Quality assurance and control A.7.1 General A.7.2 Sensitivity A.7.3 Recovery |
| 41 | A.7.4 Blank test Table A.2 – Certified value of constituent phthalates in KRISS CRM 113-03-006 |
| 42 | A.7.5 Limit of detection (LOD) or method detection limit (MDL) and limit of quantification (LOQ) A.8 Test report |
| 43 | Annex B (informative)Determination of phthalates in polymers by liquid chromatography-mass spectrometry(LC-MS) B.1 Principle B.2 Reagents and materials B.3 Apparatus |
| 44 | B.4 Sampling B.5 Procedure B.5.1 General instructions for the analysis B.5.2 Sample preparation |
| 45 | B.5.3 Instrumental parameters |
| 47 | B.5.4 Calibrants B.5.5 Calibration Table B.1 – Measurement condition of LC-MS |
| 48 | B.6 Calculation of phthalates concentration Table B.2 – Standard stock solution concentrations |
| 49 | B.7 Quality assurance and control B.7.1 General B.7.2 Performance B.7.3 Limit of detection (LOD) or method detection limit (MDL) and limit of quantification (LOQ) |
| 50 | B.8 Test report |
| 51 | Annex C (informative)Examples of chromatograms at suggested conditions C.1 GC-MS method Figures Figure C.1 – Total ion current chromatogram of each phthalate (10 µg/ml, 1 µl, splitless) Figure C.2 – Extracted ion chromatogram of DINP (10 µg/ml, 1 µl, splitless) |
| 52 | C.2 Py/TD-GC-MS method C.3 LC-MS method Figure C.3 – Extracted ion chromatogram of DIDP (10 µg/ml, 1 µl, splitless) Figure C.4 – Total ion current chromatogram of 100 µg/mlof phthalate mixture by Py/TD-GC-MS |
| 53 | C.4 IAMS method Figure C.5 – Total ion current chromatogram of 5 µg/ml of phthalate mixture by LC-MS |
| 54 | Figure C.6 – Mass spectrum of each phthalate by IAMS |
| 55 | Figure C.7 – Total ion current chromatogram of each absolute amount (0,08 µg) of phthalate mixture by IAMS 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 µg) |
| 56 | Annex D (informative)Verification of the EGA thermal desorption zone Figure D.1 – Example of EGA thermogram of a PVC sample containing phthalates |
| 57 | Annex E (informative)Example of IAMS and Py/TD-GC-MS instruments Figure E.1 – Example of IAMS instrument |
| 58 | Figure E.2 – Example of Py/TD-GC-MS instrument |
| 59 | Annex F (informative)Example of false positive detection of phthalates Figure F.1 – Typical laboratory wares made of plastic materialsthat may cause phthalate contamination Figure F.2 – Example of a chromatogram of a blank solvent (THF)in a plastic bottle showing DEHP contamination. |
| 60 | Annex G (informative)Examples of sample preparation for quantitative analysis of phthalates by GC-MS G.1 General G.2 Soxhlet extraction of phthalates using proper organic solvents |
| 61 | Table G.1 – Recovery ratios of phthalates according to different Soxhlet extraction times (extracting solvent: n-hexane) |
| 62 | Figure G.1 – Recovery ratios of Di-(2-ethylhexyl) phthalateusing Soxhlet extraction with different organic solvents Figure G.2 – Comparison of recovery ratios of phthalatesusing different extracting conditions |
| 63 | Annex H (informative)Extraction of phthalates by dissolution in THF using sonicationand precipitation of polymer matrix Table H.1 – Comparison of the efficiency of the sample preparation method of dissolution in THF using sonication and precipitation of polymeric matrix with that of Soxhlet extraction for soluble sample |
| 64 | 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 Soxhlet extraction for insoluble samples |
| 65 | Annex I (informative)Commercially available reference materials consideredsuitable for GC-MS and Py/TD-GC-MS I.1 GC-MS I.2 Py/TD-GC-MS Table I.1 – Example list of commercially available reference solutionsconsidered suitable for GC-MS |
| 66 | Figure I.1 – Sample preparation of reference materials Table I.2 – Example list of commercially available reference materials considered suitable for Py/TD-GC-MS |
| 67 | Annex J (informative)Commercially available capillary columns considered suitable for GC-MS and Py-GC-MS Table J.1 – Example list of commercially available capillary columnsconsidered suitable for GC-MS and Py-GC-MS analysis |
| 68 | Annex K (informative)Labware cleaning procedure for phthalate testing K.1 With the use of a furnace (non-volumetric glassware only) K.2 Without the use of a furnace (glassware and plastic-ware) |
| 69 | K.3 Estimation of cleanness of the inner areas of volumetric glassware |
| 70 | Annex L (informative)Results of international inter-laboratory study 5 Table L.1 – Statistical data for Py/TD-GC-MS |
| 72 | Table L.2 – Statistical data for GC-MS |
| 73 | Table L.3 – Statistical data for IAMS |
| 74 | Table L.4 – Statistical Data For LC-MS |
| 75 | Annex M (informative)Sample analysis sequence M.1 GC-MS Table M.1 – Sample analysis sequence for GC-MS analysis Table M.2 – Sample analysis sequence for Py/TD-GC-MS analysis |
| 76 | Annex N (informative)Flow chart Figure N.1 – Flow chart for screening step and quantitative step |
| 77 | Bibliography |
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