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BS EN IEC 62321-12:2023

BS EN IEC 62321-12:2023

$167.15

Determination of certain substances in electrotechnical products – Simultaneous determination. Polybrominated biphenyls, polybrominated diphenyl ethers and phthalates in polymers by gas chromatography-mass spectrometry

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BSI 2023 42
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IEC 62321-12:2023 specifies a reference test method for the simultaneous determination of polybrominated biphenyls, polybrominated diphenyl ethers, and four phthalates: di-isobutyl phthalate (DIBP), di-n-butyl phthalate (DBP), benzylbutyl phthalate (BBP), di-(2-ethylhexyl) phthalate (DEHP) in polymers of electrotechnical products. The extraction technique described in this document is the ultrasonic-assisted extraction used for simultaneous extraction for sample preparation. Gas chromatography-mass spectrometry (GC-MS) is considered as the reference technique for the measurement of the simultaneous determination of analytes in the range of 25 mg/kg to 2 000 mg/kg. The test method using ultrasonic-assisted extraction followed by GC-MS detection has been evaluated by the tests of polypropylene (PP), polyvinylchloride (PVC), acrylonitrile butadiene styrene (ABS), acrylate rubber (ACM), polystyrene (PS), polyurethane (PU) and polyethylene (PE) materials. This document has the status of a horizontal publication in accordance with IEC Guide 108.

PDF Catalog

PDF Pages PDF Title
2 undefined
5 Annex ZA (normative)Normative references to international publicationswith their corresponding European publications
6 English
CONTENTS
8 FOREWORD
10 INTRODUCTION
11 1 Scope
2 Normative references
3 Terms, definitions and abbreviated terms
3.1 Terms and definitions
12 3.2 Abbreviated terms
13 4 Principle
5 Reagents and materials
14 6 Equipment, apparatus and tools
7 Sampling
8 Procedure
8.1 General instructions for the analysis
15 8.2 Sample preparation
8.2.1 Stock solution
8.2.2 Extraction
Tables
Table 1 – Matrix spiking solution
16 8.2.3 Addition of the internal standard (IS)
8.3 Instrumental parameters
17 Table 2 – Reference for the quantification of PBBs
Table 3 –Reference for the quantification of PBDEs
Table 4 – Reference for the quantification of each phthalate
18 8.4 Calibrants
8.5 Calibration
8.5.1 General
Table 5 – Example of commercially available reference solutions
19 8.5.2 Mixing stock solutions for PBB (10 μg/ml for each congener), PBDE (10 μg/ml for each congener), phthalate (10 μg/ml for each analyte) and surrogate standard (10 μg/ml)
8.5.3 Internal standard solution (100 μg/ml of CB209, anthracene-d10)
8.5.4 Standard solutions
Table 6 – Examples of calibration ranges of PBBs, PBDEs and phthalates
20 9 Calculation of analyte concentration
9.1 General
9.2 Calculation
23 10 Precision
Table 7 – IIS12 repeatability and reproducibility
24 11 Quality assurance and control
11.1 Resolution
11.2 Performance
Table 8 – Example calculation
25 Table 9 – IIS12 mean, recovery and relative standard deviation
26 11.3 Limit of detection (LOD) or method detection limit (MDL) and limit of quantification (LOQ)
27 12 Test report
28 Annex A (informative) Example of extraction efficiency in different extractants
Figures
Figure A.1 – Extraction efficiency using detection response of the analytes in different extractants
29 Annex B (informative) Example of extraction efficiency in different cycles
Table B.1 – Extraction efficiency of the analytes in different cycles
30 Annex C (informative) Examples of chromatograms
Figure C.1 – Total ion current chromatogram of each analyte (1,5 µg/ml, 1 µl, splitless)
Figure C.2 – SIM ion chromatogram of PBBs, PBDEs and phthalate (1,5 µg/ml, 1 µl, splitless)
31 Annex D (informative) Examples of mass spectrograms
Figure D.1 – 2-Bromobiphenyl (Mono-BB)
Figure D.2 – 4-Bromodiphenyl ether (Mono-BDE)
32 Figure D.3 – 2,5-Dibromobiphenyl (Di-BB)
Figure D.4 – Di-isobutyl phthalate (DIBP)
Figure D.5 – Di-n-butyl phthalate (DBP)
33 Figure D.6 – 4,4’-Dibromobiphenyl ether (Di-BDE)
Figure D.7 – 2,4,6-Tribromobiphenyl (Tri-BB)
Figure D.8 – 3,3’,4-Tribromobiphenyl ether (Tri-BDE)
34 Figure D.9 – 2,2’,5,5’-Tetrabromobiphenyl (Tetra-BB)
Figure D.10 – Butyl benzyl phthalate (BBP)
Figure D.11 – 2,2’,4,5’,6-Pentabromobiphenyl (Penta-BB)
35 Figure D.12 – Di-(2-ethylhexyl) phthalate (DEHP)
Figure D.13 – 3,3’,4,4’-Tetrabromobiphenyl ether (Tetra-BDE)
Figure D.14 – 2,2’,4,4’,6,6’-Hexabromobiphenyl (Hexa-BB)
36 Figure D.15 – 2,2’,4,4’,6-Pentabromobiphenyl ether (Penta-BDE)
Figure D.16 – 2,2’,4,4’,5,6’-Hexabromodiphenyl ether (Hexa-BDE)
Figure D.17 – 2,2’,3,4,4’,5,5’-Heptabromobiphenyl (Hepta-BB)
37 Figure D.18 – 2,2’,3,4,4’,5,6-Heptabromodiphenyl ether (Hepta-BDE)
Figure D.19 – 2,2’,3,4,4’,5,5’,6’-Octabromodiphenyl ether (Octa-BDE)
Figure D.20 – Octabromobiphenyl, technology (hepta + octa + nona) (Octa-BB)
38 Figure D.21 – 2,2’,3,3’,4,4’,5,5’,6-Nonabromobiphenyl (Nona-BB)
Figure D.22 – 2,2’,3,3’,4,4’,5,5’,6-Nonabromodiphenyl ether (Nona-BDE)
Figure D.23 – Decabromobiphenyl (Deca-BB)
39 Figure D.24 – Decabromodiphenyl ether (Deca-BDE)
40 Annex E (informative) Statistics results of the international interlaboratory study 12 (IIS12)
41 Bibliography

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BS EN IEC 62321-12:2023
$167.15