kSIST fprEN IEC 62321-12:2023

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 crtaines substances dans les produits électroniques - Partie 12: Détermination simultanmée - Biphéyles polybromés, diphényléthers polybromés et phtalates dans les polymères par chromatographie en phase gazeuse-spectronmétrie 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

• Status: Not Published
• Public Enquiry End Date: 30-Mar-2022
• ICS: 01.110 - Technical product documentation
• ICS: 13.020.01 - Environment and environmental protection in general
• ICS: 29.020 - Electrical engineering in general
• ICS: 29.100.01 - Components for electrical equipment in general
• ICS: 31.020 - Electronic components in general
• ICS: 71.040.50 - Physicochemical methods of analysis
• Technical Committee: ITIV - Electronics assembly technology and Environmental standardization
• Current Stage: 5020 - Formal vote (FV) (Adopted Project)
• Start Date: 17-Jan-2023
• Due Date: 07-Mar-2023
• Completion Date: 19-Apr-2023
• Ref Project: EN IEC 62321-12:2023 - 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

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.

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oSIST prEN IEC 62321-12:2022

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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.

Copyright © 2021 International Electrotechnical Commission, IEC. All rights reserved. It is permitted to download this

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.

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3
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11
12
13 INTERNATIONAL ELECTROTECHNICAL COMMISSION
14 ____________
15
16 DETERMINATION OF CERTAIN SUBSTANCES IN ELECTROTECHNICAL
17 PRODUCTS –
18
19 Part 12: Simultaneous determination – polybrominated biphenyls,
20 polybrominated diphenyl ethers and phthalates in polymers by gas
21 chromatography-mass spectrometry
22

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IEC CDV 62321-12  IEC:2021 – 3 –
23 CONTENTS
24
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
10
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

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69 Annex E (informative)  Statistics results of the international interlaboratory study 12
70 (IIS12) . 35
71
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
100
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
111
112

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IEC CDV 62321-12  IEC:2021 – 5 –
113 INTERNATIONAL ELECTROTECHNICAL COMMISSION
114 ____________
115 DETERMINATION OF CERTAIN SUBSTANCES IN ELECTROTECHNICAL
116 PRODUCTS –
117
118 Part 12: Simultaneous determination– polybrominated biphenyls,
119 polybrominated diphenyl ethers and phthalates in polymers by gas
120 chromatography-mass spectrometry
121
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 Standards, Technical Specifications, Technical Reports,
127 Publicly Available Specifications (PAS) and Guides (hereafter referred to as “IEC Publication(s)”). Their
128 preparation is entrusted to technical committees; any IEC National Committee interested in the subject dealt with
129 may participate in this preparatory work. International, governmental and non-governmental organizations liaising
130 with the IEC also participate in this preparation. IEC collaborates closely with the International Organization for
131 Standardization (ISO) in accordance with conditions determined by agreement between the two organizations.
132 2) The formal decisions or agreements of IEC on technical matters express, as nearly as possible, an international
133 consensus of opinion on the relevant subjects since each technical committee has representation from all
134 interested IEC National Committees.
135 3) IEC Publications have the form of recommendations for international use and are accepted by IEC National
136 Committees in that sense. While all reasonable efforts are made to ensure that the technical content of IEC
137 Publications is accurate, IEC cannot be held responsible for the way in which they are used or for any
138 misinterpretation by any end user.
139 4) In order to promote international uniformity, IEC National Committees undertake to apply IEC Publications
140 transparently to the maximum extent possible in their national and regional publications. Any divergence between
141 any IEC Publication and the corresponding national or regional publication shall be clearly indicated in the latter.
142 5) IEC itself does not provide any attestation of conformity. Independent certification bodies provide conformity
143 assessment services and, in some areas, access to IEC marks of conformity. IEC is not responsible for any
144 services carried out by independent certification bodies.
145 6) All users should ensure that they have the latest edition of this publication.
146 7) No liability shall attach to IEC or its directors, employees, servants or agents including individual experts and
147 members of its technical committees and IEC National Committees for any personal injury, property damage or
148 other damage of any nature whatsoever, whether direct or indirect, or for costs (including legal fees) and
149 expenses arising out of the publication, use of, or reliance upon, this IEC Publication or any other IEC Publications.
150 8) Attention is drawn to the Normative references cited in this publication. Use of the referenced publications is
151 indispensable for the correct application of this publication.
152 9) Attention is drawn to the possibility that some of the elements of this IEC Publication may be the subject of patent
153 rights. IEC shall not be held responsible for identifying any or all such patent rights.
154 International Standard IEC 62321-12 has been prepared by IEC technical committee 111:
155 Environmental standardization for electrical and electronic products and systems.
156 The text of this International Standard is based on the following documents:
FDIS Report on voting
XX/XX/FDIS XX/XX/RVD
157
158 Full information on the voting for the approval of this International Standard can be found in the
159 report on voting indicated in the above table.
160 This document has been drafted in accordance with the ISO/IEC Directives, Part 2.
161 The committee has decided that the contents of this document will remain unchanged until the
162 stability date indicated on the IEC website under "http://webstore.iec.ch" in the data related to
163 the specific document. At this date, the document will be

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164 • reconfirmed,
165 • withdrawn,
166 • replaced by a revised edition, or
167 • amended.
168 The National Committees are requested to note that for this document the stability date
169 is 20XX.
170 THIS TEXT IS INCLUDED FOR THE INFORMATION OF THE NATIONAL COMMITTEES AND WILL BE DELETED
171 AT THE PUBLICATION STAGE.
172

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IEC CDV 62321-12  IEC:2021 – 7 –
173 INTRODUCTION
174 The widespread use of electrotechnical products has drawn increased attention to their impact
175 on the environment. In many countries all over the world this has resulted in the adaptation of
176 regulations affecting wastes, substances and energy use of electrotechnical products.
177 The use of certain substances (e.g. lead (Pb), cadmium (Cd), polybrominated diphenyl ethers
178 (PBDEs) and specific phthalates) in electrotechnical products is a source of concern in current
179 and proposed regional legislation.
180 The purpose of the IEC 62321 series is therefore to provide test methods that will allow the
181 electrotechnical industry to determine the levels of certain substances of concern in
182 electrotechnical products on a consistent global basis.
183 This first edition of IEC 62321-12 introduces a new part in the IEC 62321 series.
184 WARNING – Persons using this document should be familiar with normal laboratory practice.
185 This document does not purport to address all of the safety problems, if any, associated with
186 its use. It is the responsibility of the user to establish appropriate safety and health practices
187 and to ensure compliance with any national regulatory conditions.

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188 DETERMINATION OF CERTAIN SUBSTANCES IN ELECTROTECHNICAL
189 PRODUCTS –
190
191 Part 12: Simultaneous determination – polybrominated biphenyls,
192 polybrominated diphenyl ethers and phthalates in polymers by gas
193 chromatography-mass spectrometry
194
195
196 1. Scope
197 This part of IEC 62321 specifies one normative extraction and measurement technique for
198 simultaneous determination of polybrominated biphenyls, polybrominated diphenyl ethers, and
199 four phthalates (di-isobutyl phthalate (DIBP), di-n-butyl phthalate (DBP), benzylbutyl phthalate
200 (BBP), di-(2-ethylhexyl) phthalate (DEHP)) in polymers of electrotechnical products.
201 Ultrasonic-assisted extraction is described for simultaneous extraction for sample preparation
202 in this document.
203 Gas chromatography-mass spectrometry (GC-MS) is considered the normative technique for
204 measurement of simultaneous determination of the analytes in range of 25 mg/kg to 2 000
205 mg/kg.
206 This test method has been evaluated by the test of PP, PVC, ABS, ACM, PS, PU and PE
207 materials.
208 2. Normative references
209 The following documents are referred to in the text in such a way that some or all of their content
210 constitutes requirements of this document. For dated references, only the edition cited applies.
211 For undated references, the latest edition of the referenced document (including any
212 amendments) applies.
213 IEC 62321-1, Determination of certain substances in electrotechnical products – Part 1:
214 Introduction and overview
215 IEC 62321-2, Determination of certain substances in electrotechnical products – Part 2:
216 Disassembly, disjointment and mechanical sample preparation
217 3. Terms, definitions and abbreviated terms
218 3.1 Terms and definitions
219 For the purposes of this document, the following terms and definitions apply.
220 ISO and IEC maintain terminological databases for use in standardization at the following
221 addresses:
222 • IEC Electropedia: available at http://www.electropedia.org/
223 • ISO Online browsing platform: available at http://www.iso.org/obp
224 3.1.1 Simultaneous determination
225 Use the same analysis and detection procedure to determine different classes of analytes. The
226 same analysis and detection procedure includes (but not limited to): pretreatment, extraction,
227 cleaning-up and detection.
228 [Defined by referring to ISO 21470: 2020]

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229 3.1.2 Ultrasonic-assisted extraction
230 An extraction technique using ultrasonic waves to accelerate the speed of extracting
231 substances in the sample matrix (the extractant does not dissolve the sample matrix) so as to
232 improve the extraction efficiency, e.g., in an ultrasonic bath.
233 [Defined by referring to Method EPA 3550C: 2007]
234 3.1.3 Calibrant
235 Calibration standard
236 Substance in solid, liquid or gas form with known and stable concentration(s) of the analyte(s)
237 of interest used to establish instrument response (calibration curve) with respect to analyte(s)
238 concentration(s).
239 [SOURCE: IEC 62321-8: 2017, 3.1.3]
240 3.1.4 Technical mixture
241 Commercial product manufactured for industrial use whose purity is not as clearly defined as
242 an individual high purity calibration standard.
243 [SOURCE: IEC 62321-6: 2015, 3.1.2]
244 3.2 Abbreviated terms
245 BBP Benzyl butyl phthalate
246 BDE Brominated diphenyl ether
247 BSA Bis(trimethylsilyl)acetamide
248 BSTFA N,O-Bis(trimethylsilyl)trifluoroacetamide
249 CCC Continuing calibration check standard
250 DBOFB (4, 4’-dibromooctafluorobiphenyl) (n)
251 DBP Di-n-butyl phthalate
252 Deca-BB Decabromobiphenyl
253 Deca-BDE Decabromodiphenyl ether
254 DEHP Di-(2-ethylhexyl) phthalate
255 DIBP Di-isobutyl phthalate
256 DMDCS Dimethyldichlorosilane
257 EI Electron ionization
258 EPA U.S. Environmental Protection Agency
259 GC-MS Gas chromatography-mass spectrometry
260 IS Internal standard
261 IUPAC International Union of Pure and Applied Chemistry
262 LOD Limit of detection
263 LOQ Limit of quantification
264 MDL Method detection limit

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265 PBB Polybrominated biphenyl
266 PBDE Polybrominated diphenyl ether
267 PTFE Polytetrafluoroethylene
268 PTV Programmed temperature vaporising
269 QC Quality control
270 RSD Relative standard deviation
271 SIM Selected ion monitoring
272 TICS Tentatively identified compounds
273 4. Principle
274 Different classes of analytes, ie., PBBs, PBDEs, BBP, DBP, DEHP, and DIBP, in polymers are
275 simultaneously ultrasonic assisted extracted and determined qualitatively and quantitatively by
276 gas chromatography-mass spectrometry (GC-MS) using full scan mode and (or) single (or
277 “selected”) ion monitoring (SIM) mode.
278 5. Reagents and materials
279 All reagents chemicals shall be tested for contamination and blank values prior to application
280 as follows:
281 a) n-hexane (GC grade or higher);
282 b) acetone (GC grade or higher);
283 c) acetone/n-hexane (1:1, v/v);
284 d) toluene (GC grade or higher);
285 e) helium (purity greater than a volume fraction of 99,999 %);
286 f) technical BDE-209 with BDE-209 ~ 96,9 % and BDE-206 ~ 1,5 % solution;
287 g) calibrants: refer to 8.4;
288 h) surrogate and internal standards
289 – surrogate standard used to monitor analyte recovery according to 8.2.1 a), 8.5.2 and 8.5.3,
290 e.g. DBOFB (4, 4’-dibromooctafluorobiphenyl) (n), dibutyl phthalate-3,4,5,6-d4 or di-(2-
291 ethylhexyl) phthalate-3,4,5,6-d .
4
292 – internal standard used to correct for injection errors, according to 8.2.1 b), 8.2.3 and 8.5.4,
293 e.g. anthracene-d or CB209 (2,2’,3,3’,4,4’,5,5’,6,6’-decachlorobiphenyl).
10
294 Deuterium substituted target analytes are recommended as surrogate and internal
295 standards.13C-labelled nonaBDE and 13C-labelled decaBDE are recommended for the high-
296 mass PBDEs. Other standards may be used as surrogate and internal standard, if they have
297 been validated to give acceptable blank, recoveries and precision of analysis.
298 6. Equipment, apparatus and tools
299 The following items shall be used for the analysis:
300 a) analytical balance capable of measuring accurately to 0,000 1 g;
301 b) 1 ml, 5 ml, 10 ml, 25 ml, 100 ml volumetric flasks;
302 c) ultrasonic bath (450 W, 40 kHz, Volume ~10 l, or equivalent.);

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303 NOTE 1 Much lower ultrasonic power and frequency, much larger bath volume can influence the extraction efficiency.
1
304 Validation of extraction efficiency can refer to Annex B.
305 d) glass centrifuge tube with a screw cap with polytetrafluoroethylene shim (for extraction, ~10
306 ml);
307 e) centrifuge (capacity not less than 5 000 r/min);
308 f) deactivated injector liner (for GC-MS);
309 g) aluminium foil;
310 NOTE 2 Brown or amber vessels as indicated in the text of the procedure can also be used.
311 h) microlitre syringe or automatic pipettes;
312 i) pasteur pipette;
313 j) 1,5 ml sample vials with 100 μl glass insert and a screw cap with polytetrafluoroethylene
314 (PTFE) gasket or, depending on the analytical system, a comparable sample receptacle. Brown
315 or amber vessels shall be used as indicated in the text of the procedure;
316 k) mini-shaker (also known as vortexer or vortex mixer);
317 l) a gas chromatograph with a capillary column coupled to a mass spectrometric detector
318 (electron ionization, EI) is used for the analysis. The mass spectrometric detector shall be able
319 to perform selective ion monitoring and has an upper mass range of at least 1 000 m/z. The
320 high-range mass is required to unambiguously identify deca-BDE and nona-BDE. The use of
321 an autosampler is strongly recommended to ensure repeatability;
322 m) a column length of approximately 15 m has sufficient separation efficiency for PBB, PBDE
323 and phthalate compounds (see 8.3 a)) for example of suitable column);
324 n) 0,45 μm PTFE filter membrane;
325 o) pre-cleaned filter paper, pre extracted using acetone/n-hexane (see 5 c)) as extractant
326 according 8.2.2 d) for 3 cycles and dried in the air.
327 7. Sampling
328 As described in IEC 62321-2, unless indicated otherwise (e.g. “… using a nipper.”), cryogenic
329 grinding with liquid nitrogen cooling is recommended. The samples shall be ground to pass
330 through a 500 μm sieve before extraction.
331 8. Procedure
332 8.1 General instructions for the analysis
333 The following general instructions shall be followed:
334 a) In order to reduce blank values, ensure the cleanliness of all glass equipment (excluding
335 volumetric flasks) and deactivate glass wool by subjecting it to 450 °C for at least 30 min. To
336 avoid decomposition and/or debromination of PBDEs by UV light during extraction and analysis,
337 glass equipment made from brown or amber glass shall be used.
338 NOTE If no brown or amber glass is available, aluminium foil can
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