EN IEC 62321-12:2023
(Main)Determination of certain substances in electrotechnical products - Part 12: Simultaneous determination - Polybrominated biphenyls, polybrominated diphenyl ethers and phthalates in polymers by gas chromatography-mass spectrometry
Determination of certain substances in electrotechnical products - Part 12: Simultaneous determination - Polybrominated biphenyls, polybrominated diphenyl ethers and phthalates in polymers by gas chromatography-mass spectrometry
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.
Verfahren zur Bestimmung von bestimmten Substanzen in Produkten der Elektrotechnik - Teil 12: Gleichzeitige Bestimmung - Polybromierte Biphenyle, polybromierte Diphenylether und Phthalate in Polymeren durch Gaschromatographie-Massenspektrometrie
Détermination de certaines substances dans les produits électroniques - Partie 12: Détermination simultanée - Biphényles polybromés, diphényléthers polybromés et phtalates dans les polymères par chromatographie en phase gazeuse-spectrométrie de masse
IEC 62321-12:2023 spécifie une méthode d’essai de référence pour le dosage simultané des polybromobiphényles, des polybromodiphényléthers et de quatre phtalates: phtalate de di-isobutyle (DIBP), phtalate de di-n-butyle (DBP), phtalate de benzylbutyle (BBP), phtalate de bis (2-éthylhexyle) (DEHP) dans les polymères de produits électrotechniques. La technique d’extraction décrite dans le présent document est l’extraction assistée par ultrasons utilisée pour l’extraction simultanée pour la préparation des échantillons. La chromatographie en phase gazeuse-spectrométrie de masse (CG-SM) est considérée comme la technique de référence pour la mesure de la détermination simultanée des analytes dans la gamme de 25 mg/kg à 2 000 mg/kg. La méthode d’essai utilisant l’extraction assistée par ultrasons suivie d’une détection GC-MS a été évaluée par les essais de polypropylène (PP), de polychlorure de vinyle (PVC), d’acrylonitrile butadiène styrène (ABS), de caoutchouc acrylate (ACM), de polystyrène (PS), de polyuréthane (PU) et de polyéthylène (PE). Le présent document a le statut de publication horizontale conformément au Guide CEI 108
Določevanje posameznih snovi v elektrotehničnih izdelkih - 12. del: Sočasno določevanje polibromiranih bifenilov, polibromiranih difenil etrov in ftalatov v polimerih s plinsko kromatografijo-masno spektrometrijo
General Information
Standards Content (Sample)
SLOVENSKI STANDARD
oSIST prEN IEC 62321-12:2022
01-marec-2022
Določevanje posameznih snovi v elektrotehničnih izdelkih - 12. del: Sočasno
določevanje polibromiranih bifenilov, polibromiranih difenil etrov in ftalatov v
polimerih s plinsko kromatografijo-masno spektrometrijo
Determination of certain substances in electrotechnical products - Part 12: Simultaneous
determination - Polybrominated biphenyls, polybrominated diphenyl ethers and
phthalates in polymers by gas chromatography-mass spectrometry
Ta slovenski standard je istoveten z: prEN IEC 62321-12:2022
ICS:
29.020 Elektrotehnika na splošno Electrical engineering in
general
31.020 Elektronske komponente na Electronic components in
splošno general
71.040.50 Fizikalnokemijske analitske Physicochemical methods of
metode analysis
oSIST prEN IEC 62321-12:2022 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
oSIST prEN IEC 62321-12:2022
oSIST prEN IEC 62321-12:2022
111/645/CDV
COMMITTEE DRAFT FOR VOTE (CDV)
PROJECT NUMBER:
IEC 62321-12 ED1
DATE OF CIRCULATION: CLOSING DATE FOR VOTING:
2022-01-07 2022-04-01
SUPERSEDES DOCUMENTS:
111/543/CD, 111/566/CC
IEC TC 111 : ENVIRONMENTAL STANDARDIZATION FOR ELECTRICAL AND ELECTRONIC PRODUCTS AND SYSTEMS
SECRETARIAT: SECRETARY:
Italy Mr Marco Iadevaia
OF INTEREST TO THE FOLLOWING COMMITTEES: PROPOSED HORIZONTAL STANDARD:
Other TC/SCs are requested to indicate their interest, if
any, in this CDV to the secretary.
FUNCTIONS CONCERNED:
EMC ENVIRONMENT QUALITY ASSURANCE SAFETY
SUBMITTED FOR CENELEC PARALLEL VOTING NOT SUBMITTED FOR CENELEC PARALLEL VOTING
Attention IEC-CENELEC parallel voting
The attention of IEC National Committees, members of
CENELEC, is drawn to the fact that this Committee Draft
for Vote (CDV) is submitted for parallel voting.
The CENELEC members are invited to vote through the
CENELEC online voting system.
This document is still under study and subject to change. It should not be used for reference purposes.
Recipients of this document are invited to submit, with their comments, notification of any relevant patent rights of
which they are aware and to provide supporting documentation.
TITLE:
Determination of certain substances in electrotechnical products - Part 12: Simultaneous
determination – Polybrominated biphenyls, polybrominated diphenyl ethers and phthalates in
polymers by gas chromatography-mass spectrometry
PROPOSED STABILITY DATE: 2027
NOTE FROM TC/SC OFFICERS:
This CDV was submitted based on the agreement of the 33rd WG3 meeting in September 2021.
electronic file, to make a copy and to print out the content for the sole purpose of preparing National Committee positions.
You may not copy or "mirror" the file or printed version of the document, or any part of it, for any other purpose without
permission in writing from IEC.
oSIST prEN IEC 62321-12:2022
– 2 – IEC CDV 62321-12 IEC:2021
13 INTERNATIONAL ELECTROTECHNICAL COMMISSION
14 ____________
16 DETERMINATION OF CERTAIN SUBSTANCES IN ELECTROTECHNICAL
17 PRODUCTS –
19 Part 12: Simultaneous determination – polybrominated biphenyls,
20 polybrominated diphenyl ethers and phthalates in polymers by gas
21 chromatography-mass spectrometry
oSIST prEN IEC 62321-12:2022
IEC CDV 62321-12 IEC:2021 – 3 –
23 CONTENTS
25 FOREWORD . 5
26 INTRODUCTION . 7
27 1 Scope . 8
28 2 Normative references . 8
29 3 Terms, definitions and abbreviated terms . 8
30 3.1 Terms and definitions. 8
31 3.1.1 Simultaneous determination . 8
32 3.1.2 Ultrasonic-assisted extraction . 8
33 3.1.3 Calibrant . 9
34 3.1.4 Technical mixture . 9
35 3.2 Abbreviated terms . 9
36 4 Principle . 10
37 5 Reagents and materials . 10
38 6 Equipment, apparatus and tools . 10
39 7 Sampling . 11
40 8 Procedure . 11
41 8.1 General instructions for the analysis . 11
42 8.2 Sample preparation . 11
43 8.2.1 Stock solution . 11
44 8.2.2 Extraction . 12
45 8.2.3 Addition of the internal standard (IS) . 13
46 8.3 Instrumental parameters . 13
47 8.4 Calibrants . 14
48 8.5 Calibration . 15
49 8.5.1 General . 15
50 8.5.2 Mixing stock solutions for PBB (10 μg/ml for each congener), PBDE (10
51 μg/ml for each congener), phthalate (10 μg/ml for each analyte) and
52 surrogate standard (10 μg/ml). . 15
53 8.5.3 Internal standard solution (100 μg/ml of CB209, anthracene-d ) . 15
54 8.5.4 Standard solutions . 16
55 9 Calculation of analyte concentration . 17
56 9.1 General . 17
57 9.2 Calculation . 17
58 10 Precision . 19
59 11 Quality assurance and control . 20
60 11.1 Resolution . 20
61 11.2 Performance . 20
62 11.3 Limit of detection (LOD) or method detection limit (MDL) and limit of
63 quantification (LOQ) . 22
64 12 Test report . 23
65 Annex A (informative) Example for extraction efficiency in different extractants . 24
66 Annex B (informative) Example for extraction efficiency in different cycles . 25
67 Annex C (informative) Examples of chromatograms at suggested conditions . 26
68 Annex D (informative) Examples of mass spectrograms at suggested conditions . 27
oSIST prEN IEC 62321-12:2022
– 4 – IEC CDV 62321-12 IEC:2021
69 Annex E (informative) Statistics results of the international interlaboratory study 12
70 (IIS12) . 35
72 Figure A.1 – Extraction efficiency of the analytes in different extractants . 24
73 Figure C.1 – Total ion current chromatogram of each analyte (1.5 µg/ml, 1 µl, splitless) . 26
74 Figure C.2 – SIM ion chromatogram of PBBs, PBDEs and phthalate (1.5 µg/ml, 1 µl,
75 splitless) . 26
76 Figure D.1 – 2-Bromobiphenyl (Mono-BB) . 27
77 Figure D.2 – 4-Bromodiphenyl ether (Mono-BDE) . 27
78 Figure D.3 – 2,5-Dibromobiphenyl (Di-BB) . 27
79 Figure D.4 – Di-isobutyl phthalate (DIBP) . 28
80 Figure D.5 – Di-n-butyl phthalate (DBP) . 28
81 Figure D.6 – 4,4’-Dibromobiphenyl ether (Di-BDE) . 28
82 Figure D.7 – 2,4,6-Tribromobiphenyl (Tri-BB) . 29
83 Figure D.8 – 3,3’,4-Tribromobiphenyl ether (Tri-BDE) . 29
84 Figure D.9 – 2,2’,5,5’-Tetrabromobiphenyl (Tetra-BB) . 29
85 Figure D.10 – Butyl benzyl phthalate (BBP) . 30
86 Figure D.11 – 2,2’,4,5’,6-Pentabromobiphenyl (Penta-BB) . 30
87 Figure D.12 – Di-(2-ethylhexyl) phthalate (DEHP) . 30
88 Figure D.13 – 3,3’,4,4’-Tetrabromobiphenyl ether (Tetra-BDE) . 31
89 Figure D.14 – 2,2’,4,4’,6,6’-Hexabromobiphenyl (Hexa-BB) . 31
90 Figure D.15 – 2,2’,4,4’,6-Pentabromobiphenyl ether (Penta-BDE) . 31
91 Figure D.16 – 2,2’,4,4’,5,6’-Hexabromodiphenyl ether (Hexa-BDE) . 32
92 Figure D.17 – 2,2’,3,4,4’,5,5’-Heptabromobiphenyl (Hepta-BB) . 32
93 Figure D.18 – 2,2’,3,4,4’,5,6-Heptabromodiphenyl ether (Hepta-BDE) . 32
94 Figure D.19 – 2,2’,3,4,4’,5,5’,6’-Octabromodiphenyl ether (Octa-BDE) . 33
95 Figure D.20 – Octabromobiphenyl,techn.(hepta+octa+nona) (Octa-BB) . 33
96 Figure D.21 – 2,2’,3,3’,4,4’,5,5’,6-Nonabromobiphenyl (Nona-BB) . 33
97 Figure D.22 – 2,2’,3,3’,4,4’,5,5’,6-Nonabromodiphenyl ether (Nona-BDE) . 34
98 Figure D.23 – Decabromobiphenyl (Deca-BB) . 34
99 Figure D.24 – Decabromodiphenyl ether (Deca-BDE) . 34
101 Table 1 – Matrix spiking solution . 12
102 Table 2 – Reference masses for the quantification of PBBs . 13
103 Table 3 –Reference masses for the quantification of PBDEs . 14
104 Table 4 –Reference masses for the quantification of each phthalate . 14
105 Table 5 –Example list of commercially available reference solutions . 14
106 Table 6 – Example of Calibration ranges of PBBs, PBDEs and phthalates . 16
107 Table 7 – IIS12 repeatability and reproducibility . 19
108 Table 8 – Example calculation . 20
109 Table 9 – IIS12 mean, recovery and relative standard deviation . 21
110 Table B.1 – Extraction efficiency of the analytes in different cycles . 25
oSIST prEN IEC 62321-12:2022
IEC CDV 62321-12 IEC:2021 – 5 –
113 INTERNATIONAL ELECTROTECHNICAL COMMISSION
114 ____________
115 DETERMINATION OF CERTAIN SUBSTANCES IN ELECTROTECHNICAL
116 PRODUCTS –
118 Part 12: Simultaneous determination– polybrominated biphenyls,
119 polybrominated diphenyl ethers and phthalates in polymers by gas
120 chromatography-mass spectrometry
122 FOREWORD
123 1) The International Electrotechnical Commission (IEC) is a worldwide organization for standardization comprising
124 all national electrotechnical committees (IEC National Committees). The object of IEC is to promote international
125 co-operation on all questions concerning standardization in the electrical and electronic fields. To this end and
126 in addition to other activities, IEC publishes International Stan
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