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BS EN 62321-8:2017 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), 2017
- National foreword
- English [Go to Page]
- CONTENTS
- FOREWORD
- INTRODUCTION
- 1 Scope
- 2 Normative references
- 3 Terms, definitions and abbreviated terms [Go to Page]
- 3.1 Terms and definitions
- 3.2 Abbreviated terms
- 4 Principle
- 5 Reagents and materials [Go to Page]
- 5.1 GC-MS method
- 5.2 Py/TD-GC-MS method
- 6 Apparatus [Go to Page]
- 6.1 GC-MS method
- 6.2 Py/TD-GC-MS method
- 7 Sampling [Go to Page]
- 7.1 General
- 7.2 GC-MS method
- 7.3 Py/TD-GC-MS method
- 8 Procedure [Go to Page]
- 8.1 General instructions for the analysis [Go to Page]
- 8.1.1 Overview
- 8.1.2 GC-MS method
- 8.1.3 Py/TD-GC-MS method
- 8.2 Sample preparation [Go to Page]
- 8.2.1 GC-MS method
- 8.2.2 Py/TD-GC-MS method
- 8.3 Instrumental parameters [Go to Page]
- 8.3.1 GC-MS method
- Tables [Go to Page]
- Table 1 – Measurement condition of GC-MS
- Table 2 – Reference masses for the quantification of each phthalate [Go to Page]
- 8.3.2 Py/TD-GC-MS method
- 8.4 Calibrants
- Table 3 – Measurement condition of Py/TD-GC-MS
- 8.5 Calibration [Go to Page]
- 8.5.1 GC-MS method
- Table 4 – Calibration standard solution of phthalates [Go to Page]
- 8.5.2 Py/TD-GC-MS method
- 9 Calculation of phthalate concentration [Go to Page]
- 9.1 GC-MS method
- 9.2 Py/TD-GC-MS method
- 10 Precision [Go to Page]
- 10.1 GC-MS method [Go to Page]
- 10.1.1 Threshold judgement
- Table 5 – IIS5 Threshold judgement [Go to Page]
- 10.1.2 Repeatability and reproducibility
- Table 6 – IIS5 Repeatability and reproducibility
- 10.2 Py/TD-GC-MS method [Go to Page]
- 10.2.1 Screening judgement
- Table 7 – IIS5 screening and threshold judgement [Go to Page]
- 10.2.2 Repeatability and reproducibility
- Table 8 – IIS5 Repeatability and reproducibility
- 11 Quality assurance and control [Go to Page]
- 11.1 General
- 11.2 GC-MS method [Go to Page]
- 11.2.1 Performance
- 11.2.2 Limit of detection (LOD) or method detection limit (MDL) and limit of quantification (LOQ)
- 11.3 Py/TD-GC-MS method [Go to Page]
- 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)
- 12 Test report
- Annex A (informative)Determination of phthalates in polymers byion attachment mass spectrometry (IAMS) [Go to Page]
- A.1 Principle
- A.2 Reagents and materials
- A.3 Apparatus
- A.4 Sampling
- A.5 Procedure [Go to Page]
- A.5.1 General instructions for the analysis
- A.5.2 Sample preparation
- A.5.3 Instrumental parameters
- A.5.4 Calibrants
- A.5.5 Calibration
- Table A.1 – Measurement condition of IAMS
- A.6 Calculation of phthalates concentration
- A.7 Quality assurance and control [Go to Page]
- A.7.1 General
- A.7.2 Sensitivity
- A.7.3 Recovery
- A.7.4 Blank test
- Table A.2 – Certified value of constituent phthalates in KRISS CRM 113-03-006 [Go to Page]
- A.7.5 Limit of detection (LOD) or method detection limit (MDL) and limit of quantification (LOQ)
- A.8 Test report
- Annex B (informative)Determination of phthalates in polymers by liquid chromatography-mass spectrometry(LC-MS) [Go to Page]
- B.1 Principle
- B.2 Reagents and materials
- B.3 Apparatus
- B.4 Sampling
- B.5 Procedure [Go to Page]
- B.5.1 General instructions for the analysis
- B.5.2 Sample preparation
- B.5.3 Instrumental parameters
- B.5.4 Calibrants
- B.5.5 Calibration
- Table B.1 – Measurement condition of LC-MS
- B.6 Calculation of phthalates concentration
- Table B.2 – Standard stock solution concentrations
- B.7 Quality assurance and control [Go to Page]
- 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)
- B.8 Test report
- Annex C (informative)Examples of chromatograms at suggested conditions [Go to Page]
- C.1 GC-MS method
- Figures [Go to Page]
- 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)
- 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
- C.4 IAMS method
- Figure C.5 – Total ion current chromatogram of 5 µg/ml of phthalate mixture by LC-MS
- Figure C.6 – Mass spectrum of each phthalate by IAMS
- 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)
- Annex D (informative)Verification of the EGA thermal desorption zone [Go to Page]
- Figure D.1 – Example of EGA thermogram of a PVC sample containing phthalates
- Annex E (informative)Example of IAMS and Py/TD-GC-MS instruments [Go to Page]
- Figure E.1 – Example of IAMS instrument
- Figure E.2 – Example of Py/TD-GC-MS instrument
- Annex F (informative)Example of false positive detection of phthalates [Go to Page]
- 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.
- Annex G (informative)Examples of sample preparation for quantitative analysis of phthalates by GC-MS [Go to Page]
- G.1 General
- G.2 Soxhlet extraction of phthalates using proper organic solvents
- Table G.1 – Recovery ratios of phthalates according to different Soxhlet extraction times (extracting solvent: n-hexane)
- 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
- Annex H (informative)Extraction of phthalates by dissolution in THF using sonicationand precipitation of polymer matrix [Go to Page]
- 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
- 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
- Annex I (informative)Commercially available reference materials consideredsuitable for GC-MS and Py/TD-GC-MS [Go to Page]
- I.1 GC-MS
- I.2 Py/TD-GC-MS
- Table I.1 – Example list of commercially available reference solutionsconsidered suitable for GC-MS
- 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
- Annex J (informative)Commercially available capillary columns considered suitable for GC-MS and Py-GC-MS [Go to Page]
- Table J.1 – Example list of commercially available capillary columnsconsidered suitable for GC-MS and Py-GC-MS analysis
- Annex K (informative)Labware cleaning procedure for phthalate testing [Go to Page]
- K.1 With the use of a furnace (non-volumetric glassware only)
- K.2 Without the use of a furnace (glassware and plastic-ware)
- K.3 Estimation of cleanness of the inner areas of volumetric glassware
- Annex L (informative)Results of international inter-laboratory study 5 [Go to Page]
- Table L.1 – Statistical data for Py/TD-GC-MS
- Table L.2 – Statistical data for GC-MS
- Table L.3 – Statistical data for IAMS
- Table L.4 – Statistical Data For LC-MS
- Annex M (informative)Sample analysis sequence [Go to Page]
- 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
- Annex N (informative)Flow chart [Go to Page]
- Figure N.1 – Flow chart for screening step and quantitative step
- Bibliography [Go to Page]
