prEN IEC 62321-11:2022

Determination of certain substances in electrotechnical products - Part 11: Tris (2-chloroethyl) phosphate (TCEP) in plastics by gas chromatography-mass spectrometry (GC-MS) and liquid chromatography-mass spectrometry (LC-MS)

This part of IEC 62321 specifies two different techniques for the determination of TCEP tris(2-chloroethyl) phosphate (TCEP) in plastics, the GC-MS or LC-MS method; both of which are suitable for quantitative analysis. These two techniques have been evaluated for use with polyurethane, Polyvinyl chloride and polyethylene materials containing TCEP between 200 mg/kg to 2 000 mg/kg. Use of the methods escribed in International Standard for other polymers and concentration ranges has not been specifically evaluated. These test methods do not apply to plastics materials having a processing temperature higher than 230 ℃. NOTE TCEP starts thermal decomposition at approximately 230 ℃. Polymer types which have a processing temperature into shapes of plastics (e.g. pellets, moulded parts, or sheets etc.) not exceeding the decomposition temperature can contain TCEP. Py-TD-GC-MS is another technique, suitable for the screening of TCEP in plastics (See Annex A).

Določevanje posameznih snovi v elektrotehničnih izdelkih - 11. del: Določevanje ? tris (2-kloroetil) fosfata (TCEP) v plastiki ? polimernih materialih ? s plinsko kromatografijo-masno spektrometrijo (GC-MS) in tekočinsko kromatografijo-masno spektrometrijo (LC-MS)

Détermination de certaines substances dans les produits électrotechniques - Partie 11: Phosphate de tris(2-chloroéthyle) (TCEP) dans les plastiques par chromatographie en phase gazeuse-spectrométrie de masse (GC-MS) et chromatographie en phase liquide-spectrométrie de masse (LC-MS)

Določevanje posameznih snovi v elektrotehničnih izdelkih - 11. del: Določevanje ? tris (2-kloroetil) fosfata (TCEP) v polimernih materialih s plinsko kromatografijo-masno spektrometrijo (GC-MS) in tekočinsko kromatografijo-masno spektrometrijo (LC-MS)

General Information

• Status: Not Published
• Publication Date: 23-Jul-2023
• ICS: 13.020.01 - Environment and environmental protection in general
• ICS: 43.040.10 - Electrical and electronic equipment
• Technical Committee: CLC/TC 111X - Environment
• Drafting Committee: IEC/TC 111 - Environmental standardization for electrical and electronic products and systems
• Current Stage: 4060 - Enquiry results established and sent to TC, SR, BTTF - Enquiry
• Start Date: 25-Mar-2022
• Completion Date: 25-Mar-2022
• Ref Project: oSIST prEN IEC 62321-11:2022 - Determination of certain substances in electrotechnical products - Part 11: Tris (2-chloroethyl) phosphate (TCEP) in plastics by gas chromatography-mass spectrometry (GC-MS) and liquid chromatography-mass spectrometry (LC-MS)

Standards Content (Sample)

SLOVENSKI STANDARD
oSIST prEN IEC 62321-11:2022
01-marec-2022
Določevanje posameznih snovi v elektrotehničnih izdelkih - 11. del: Določevanje ?
tris (2-kloroetil) fosfata (TCEP) v polimernih materialih s plinsko kromatografijo-
masno spektrometrijo (GC-MS) in tekočinsko kromatografijo-masno
spektrometrijo (LC-MS)
Determination of certain substances in electrotechnical products - Part 11: Tris (2-
chloroethyl) phosphate (TCEP) in plastics by gas chromatography-mass spectrometry
(GC-MS) and liquid chromatography-mass spectrometry (LC-MS)
Določevanje posameznih snovi v elektrotehničnih izdelkih - 11. del: Določevanje ? tris (2-
kloroetil) fosfata (TCEP) v plastiki ? polimernih materialih ? s plinsko kromatografijo-
masno spektrometrijo (GC-MS) in tekočinsko kromatografijo-masno spektrometrijo (LC-
MS)
Ta slovenski standard je istoveten z: prEN IEC 62321-11:2022
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 62321-11:2022 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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oSIST prEN IEC 62321-11:2022

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oSIST prEN IEC 62321-11:2022
111/641/CDV

COMMITTEE DRAFT FOR VOTE (CDV)

PROJECT NUMBER:
IEC 62321-11 ED1
DATE OF CIRCULATION: CLOSING DATE FOR VOTING:
2021-12-31 2022-03-25
SUPERSEDES DOCUMENTS:
111/557/CD, 111/613/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 11: Tris (2-chloroethyl)
phosphate (TCEP) in plastics by gas chromatography-mass spectrometry (GC-MS) and liquid
chromatography-mass spectrometry (LC-MS)

PROPOSED STABILITY DATE: 2025

NOTE FROM TC/SC OFFICERS:

1
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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2 DETERMINATION OF CERTAIN SUBSTANCES
3 IN ELECTROTECHNICAL PRODUCTS –
4
5 Part 11: Tris(2-chloroethyl) phosphate (TCEP) in plastics by gas
6 chromatography-mass spectrometry (GC-MS) and liquid chromatography-mass
7 spectrometry (LC-MS)
8
9

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10 CONTENTS
11 FOREWORD . 5
12 INTRODUCTION . 7
13 1. Scope . 8
14 2. Normative references . 8
15 3. Terms, definitions and abbreviations . 8
16 3.1. Terms and definitions . 8
17 3.1.1. Screening . 8
18 3.1.2. Plastic, noun . 9
19 3.1.3. Polymer . 9
20 3.2. Abbreviations . 9
21 4. Principle . 10
22 5. Reagents and materials . 10
23 6. Apparatus . 11
24 6.1. GC-MS Method . 11
25 6.2. LC-MS Method . 11
26 7. Sampling. 12
27 8. Procedure . 12
28 8.1. General instructions for the analysis. 12
29 8.2. Sample preparation . 12
30 8.2.1. GC-MS Method . 12
31 8.2.2. LC-MS Method . 14
32 8.3. Instrumental parameters . 15
33 8.3.1. GC-MS Method . 15
34 Table 1 – Measurement condition of GC-MS . 15
35 Table 2 – Reference masses for the quantification of TCEP . 16
36 8.3.2. LC-MS Method . 16
37 Table 3 – Measurement condition of LC-MS . 16
38 8.4. Calibrants. 17
39 8.5. Calibration. 17
40 8.5.1. General . 17
41 8.5.2. TCEP and surrogate (100 μg/ml) stock solution. 17
42 8.5.3. Internal standard solution (100 μg/ml of anthracene-d ) . 17
10
43 8.5.4. Standard solutions . 18
44 Table 4 – Calibration standard solution of TCEP with internal standard – Estimated TCEP
45 sample solution concentration 0,1 µg/ml and higher . 18
46 Table 5 – Calibration standard solution of TCEP with internal standard – Estimated TCEP
47 sample solution concentration lover than 0.1 µg/ml . 18
48 9. Calculation of TCEP concentration . 19
49 10. Precision . 21
50 10.1. GC-MS Method . 21
51 Table 6 – IIS 11 repeatability and reproducibility. 21
52 10.2. LC-MS Method . 21
53 Table 7 – IIS 11 repeatability and reproducibility. 22

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54
11. Quality assurance and control . 22
55 11.1. General . 22
56 11.2. GC-MS Method . 22
57 11.2.1. Performance . 22
58 11.2.2. Method detection limit and reporting limit . 23
59 11.3. LC-MS Method . 24
60 11.3.1. Performance . 24
61 11.3.2. Method detection limit and reporting limit . 24
62 12. Test report . 25
63 Annex A . 26
64 A.1 Principle . 26
65 A.2 Reagents and materials . 27
66 A.3 Apparatus . 27
67 A.4 Sampling . 28
68 A.5 Procedure . 28
69 A.5.1 General instructions for the analysis . 28
70 A.5.2 Sample preparation . 28
71 A.5.3 Instrumental parameters . 29
72 Table A.1 – Measurement condition of Py/TD-GC-MS . 29
73 A.5.4 Calibration . 29
74 A.6 Calculation of TCEP concentration . 31
75 A.6.1 General . 31
76 A.6.2 Determination of RF of DEHP . 31
77 A.6.3 Calculation . 31
78 Annex B . 33
79 Figure B.1 – Gas Chromatogram of TCEP, TCEP-d12 and anthracene-d10. . 33
80 Figure B.2 – Mass spectrum of TCEP by GC-MS. . 33
81 Annex C . 34
82 Figure C.1 – Liquid chromatogram of TCEP and TCEP-d . . 34
12
83 Figure C.2 – Mass spectrum of TCEP by LC-MS. . 35
84 Figure C.3 – Mass spectrum of TCEP-d by LC-MS. . 35
12
85 Annex D . 36
86 36
87 Bibliography . 37
88
89

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90 INTERNATIONAL ELECTROTECHNICAL COMMISSION
91 ____________
92 DETERMINATION OF CERTAIN SUBSTANCES
93 IN ELECTROTECHNICAL PRODUCTS –
94
95 Part 11: Tris(2-chloroethyl) phosphate (TCEP) in plastics by gas
96 chromatography-mass spectrometry (GC-MS) and liquid chromatography-mass
97 spectrometry (LC-MS)
98
99 FOREWORD
100 1) The International Electrotechnical Commission (IEC) is a worldwide organization for standardization comprising all national
101 electrotechnical committees (IEC National Committees). The object of IEC is to promote international co-operation on all
102 questions concerning standardization in the electrical and electronic fields. To this end and in addition to other activities,
103 IEC publishes International Standards, Technical Specifications, Technical Reports, Publicly Available Specifications (PAS)
104 and Guides (hereafter referred to as “IEC Publication(s)”). Their preparation is entrusted to technical committees; any IEC
105 National Committee interested in the subject dealt with may participate in this preparatory work. International, governmental
106 and non-governmental organizations liaising with the IEC also participate in this preparation. IEC collaborates closely with
107 the International Organization for Standardization (ISO) in accordance with conditions determined by agreement between
108 the two organizations.
109 2) The formal decisions or agreements of IEC on technical matters express, as nearly as possible, an international consensus
110 of opinion on the relevant subjects since each technical committee has representation from all interested IEC National
111 Committees.
112 3) IEC Publications have the form of recommendations for international use and are accepted by IEC National Committees in
113 that sense. While all reasonable efforts are made to ensure that the technical content of IEC Publications is accurate, IEC
114 cannot be held responsible for the way in which they are used or for any misinterpretation by any end user.
115 4) In order to promote international uniformity, IEC National Committees undertake to apply IEC Publications transparently to
116 the maximum extent possible in their national and regional publications. Any divergence between any IEC Publication and
117 the corresponding national or regional publication shall be clearly indicated in the latter.
118 5) IEC itself does not provide any attestation of conformity. Independent certification bodies provide conformity assessment
119 services and, in some areas, access to IEC marks of conformity. IEC is not responsible for any services carried out by
120 independent certification bodies.
121 6) All users should ensure that they have the latest edition of this publication.
122 7) No liability shall attach to IEC or its directors, employees, servants or agents including individual experts and members of
123 its technical committees and IEC National Committees for any personal injury, property damage or other damage of any
124 nature whatsoever, whether direct or indirect, or for costs (including legal fees) and expenses arising out of the publication,
125 use of, or reliance upon, this IEC Publication or any other IEC Publications.
126 8) Attention is drawn to the Normative references cited in this publication. Use of the referenced publications is indispensable
127 for the correct application of this publication.
128 9) Attention is drawn to the possibility that some of the elements of this IEC Publication may be the subject of patent rights.
129 IEC shall not be held responsible for identifying any or all such patent rights.
130 International Standard IEC 62321-11 has been prepared by IEC technical committee 111: Environmental
131 standardization for electrical and electronic products and systems.
132 The text of this International Standard is based on the following documents:
FDIS Report on voting
XX/XX/FDIS XX/XX/RVD
133
134 Full information on the voting for the approval of this International Standard can be found in the report
135 on voting indicated in the above table.
136 This document has been drafted in accordance with the ISO/IEC Directives, Part 2.

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137
The committee has decided that the contents of this document will remain unchanged until the stability
138 date indicated on the IEC website under "http://webstore.iec.ch" in the data related to the specific
139 document. At this date, the document will be
140 – reconfirmed,
141 – withdrawn,
142 – replaced by a revised edition, or
143 – amended.
144 The National Committees are requested to note that for this document the stability date is 20XX.
145 THIS TEXT IS INCLUDED FOR THE INFORMATION OF THE NATIONAL COMMITTEES AND WILL BE DELETED AT THE
146 PUBLICATION STAGE.
147

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148 INTRODUCTION
149 The widespread use of electrotechnical products has drawn increased attention to their impact on the
150 environment. In many countries this has resulted in the adoption of regulations affecting wastes,
151 substances and energy use of electrotechnical products.
152 The use of certain substances (e.g. lead (Pb), cadmium (Cd) and polybrominated diphenyl ethers
153 (PBDEs)) in electrotechnical products is a source of concern in current and proposed regional legislation.
154 The purpose of the IEC 62321 series is therefore to provide test methods that will allow the
155 electrotechnical industry to determine the levels of certain substances of concern in electrotechnical
156 products on a consistent global basis.
157 This first edition of IEC 62321-11 introduces a new subject covering Tris(2-chloroethyl) phosphate
158 (TCEP) in the IEC 62321 series.
159 TCEP is a halogenated phosphorus-based flame retardant that is disclosable as a Substance of Very
160 High Concern (SVHC) as it is classified as toxic to reproduction category 2 (R60) and was included in
161 the candidate list for authorisation on 13 January 2010, following ECHA’s decision ED/68/2009 and in
162 regulation (EC) No 1907/2006 ANNEX XVI.
163 TCEP is used as a flame retardant in plastics such as polyester and polyurethane foam, and as a
164 plasticizer in Polyvinyl chloride. Additionally, TCEP is used as an alternative for brominated flame
165 retardants that have been restricted. No applicable testing standard exists for TCEP analysis in plastics.
166 As a result, analysis criteria have been established by IEC/TC 111/JWG 14 joint-development with
167 ISO/TC 61/SC 5 as ISO/IEC double logo International Standard; to provide a test method that will allow
168 industry to determine the levels of TCEP in plastics.
169 WARNING — Persons using this International Standard should be familiar with normal
170 laboratory practice. This International Standard does not purport to address all of the safety
171 problems, if any, associated with its use. It is the responsibility of the user to establish
172 appropriate safety and health practices and to ensure compliance with any national regulatory
173 conditions.

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174 DETERMINATION OF CERTAIN SUBSTANCES
175 IN ELECTROTECHNICAL PRODUCTS –
176
177 Part 11: Tris(2-chloroethyl) phosphate (TCEP) in plastics by gas
178 chromatography-mass spectrometry (GC-MS) and liquid chromatography-mass
179 spectrometry (LC-MS)
180
181 1. Scope
182 This part of IEC 62321 specifies two different techniques for the determination of TCEP tris(2-chloroethyl)
183 phosphate (TCEP) in plastics, the GC-MS or LC-MS method; both of which are suitable for quantitative
184 analysis.
185 These two techniques have been evaluated for use with polyurethane, Polyvinyl chloride and
186 polyethylene materials containing TCEP between 200 mg/kg to 2 000 mg/kg. Use of the methods
187 described in International Standard for other polymers and concentration ranges has not been
188 specifically evaluated.
189 These test methods do not apply to plastics materials having a processing temperature higher than
190 230 ℃.
191 NOTE TCEP starts thermal decomposition at approximately 230 ℃. Polymer types which have a processing temperature into
192 shapes of plastics (e.g. pellets, moulded parts, or sheets etc.) not exceeding the decomposition temperature can contain TCEP.
193 Py-TD-GC-MS is another technique, suitable for the screening of TCEP in plastics (See Annex A).
194 2. Normative references
195 The following referenced documents are indispensable for the application of this document. For dated
196 references, only the edition cited applies. For undated references, the latest edition of the referenced
197 document (including any amendments) applies.
198
199 IEC 62321-1:2013, Determination of certain substances in electrotechnical products – Part 1:
200 Introduction and overview
201 IEC 62321-2:2013, Determination of certain substances in electrotechnical products – Part 2:
202 Disassembly, disjointment and mechanical sample preparation
203 ISO 472:2013, Plastics – Vocabulary
204 ISO 1043-1:2011, Plastics – Symbols and abbreviated terms – Part 1: Basic polymers and their special
205 characteristics
206 ISO 1382:2012, Rubber-Vocabulary
207
208 3. Terms, definitions and abbreviations
209 3.1. Terms and definitions
210 For the purposes of this document, the following terms and definitions apply.
211 ISO and IEC maintain terminological databases for use in standardization at the following addresses:
212 • IEC Electropedia: available at http://www.electropedia.org/
213 • ISO Online browsing platform: available at http://www.iso.org/obp
214 3.1.1. Screening
215 Analytical procedure to determine the presence or absence of substances in the representative part or
216 section of a product, relative to the value or values chosen as the criterion for presence, absence or

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217
further testing.
218 Note to entry: If the screening method produces values that are not conclusive, then additional analysis or other follow-up
219 actions may be necessary to make a final presence/absence decision.
220 [SOURCE: IEC 62321-1:2013, 3.1.10]
221 3.1.2. Plastic, noun
222 Material which contains as an essential ingredient a high polymer and which, at some stage in its processing into
223 finished products, can be shaped by flow
224 Note 1 to entry Elastomeric materials, which are also shaped by flow, are not considered to be plastics.
225 Note 2 to entry In some countries, particularly the United Kingdom, the term “plastics” is used as the singular form as well as the plural form.
226 [SOURCE: ISO 472:2013, 2.702]
227 3.1.3. Polymer
228 substance composed of molecules characterized by the multiple repetition of one or more species of atoms or
229 groups of atoms (constitutional units) linked to each other in amounts sufficient to provide a set of properties that
230 do not vary markedly with the addition or removal of one or a few of the constitutional units. [SOURCE: ISO
231 1382:2012, 2.341]
232 3.2. Abbreviations
233 ACN       Acetonitrile
234 API-ES Atmospheric pressure ionization – electrostatic
235 BSA       N,O-Bis(trimethylsilyl)acetamide
236 BSTFA N,O-Bis(trimethylsilyl)trifluoroacetamide
237 CCC Continuing calibration check standard
238 CRM  Certified reference material
239 D Dilution factor
240 DEHP Di-(2-ethylhexyl) phthalate
241 DIP       Direct injection probe
242 DMDCS Dimethyldichlorosilane
243 EI Electron ionization
244 GC-MS Gas chromatography – mass spectrometry
245 HPLC High-performance liquid chromatography
246 ID Internal diameter
247 IS Internal standard
248 LC-MS Liquid chromatography – mass spectrometry
249 LOD  Limit of detection
250 LOQ  Limit of quantification
251 MDL  Method detection limit
252 MS Mass spectrometry
253 NS Neck size
254 PBB Polybrominated biphenyl
255 PBDE Polybrominated diphenyl ether
256 PS Polystyrene
257 PTFE      Polytetrafluoroethylene
258 PUR Polyurethane

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259
PVC       Polyvinyl chloride
260 Py/TD-GC-MS Gas chromatography-mass spectrometry using a pyrolyzer/thermal desorption
261 accessory
262 QC  Quality control
263 RF Response factor
264 RRF Relative response factor
265 RSD Relative standard deviation
266 SIM  Single (or “selected”) ion monitoring
267 TCEP      Tris(2-chloroethyl) phosphate, (CAS Number: 115-96-8)
268 TD        Thermal desorption
269 THF Tetrahydrofuran
270 TICS Tentatively identified compounds
271
272 4. Principle
273 The samples are dissolved by THF using ultra-sonication, or extracted using Soxhlet. The matrix polymer of
274 dissolved sample is separated by precipitation with non-solvent, methanol.
275 TCEP in the sample solution is determined quantitatively and qualitatively using GC-MS or LC-MS. It is possible
276 to analyze high concentrations by diluting the sample solution.
277
278 5. Reagents and materials
279 All chemicals are tested for contamination and blank values prior to application.
280 a) TCEP (tris(2-chloroethyl) phosphate): CAS No. 115-96-8 (purity of greater than a mass fraction of
281 98 %)
282 b) THF (GC grade or higher, higher than 99,9 %)
283 c) n-Hexane (GC grade or higher, higher than 98,5 %)
284 d) Methanol (GC grade or higher, higher than 99,9 %)
285 e) Mixed solvent (THF mixed with methanol, the ratio of THF/methanol is 1/4)
286 f) Helium (purity of greater than 99,999 %)
287 g) Calibrants; reference materials of TCEP (purity of greater than 98 %)
288 h) Surrogate and internal standards:
289 - Surrogate standard used to monitor analytes recovery according to 8.2.1.1 and 8.2.2.1,
290 for example TCEP-d ;
12
291 - Internal standard used to correct injection errors, according to 8.2.1.1 and 8.2.2.1,
292 for example anthracene d-
10
293 The standards are acceptable when using a quadruple-type mass spectrometer. A high-resolution mass
294 spectrometer will require the use of other suitable standard substances having a mass and elution time
295 similar to that of the analyte.
296

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297 6. Apparatus
298 6.1. GC-MS Method
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) Cryogenic grinding mill with liquid N2 cooling;
302 c) Ultrasonic bath;
303 d) 1 ml, 5 ml, 10 ml, 50 ml, 100 ml volumetric flasks;
304 e) Soxhlet extractors:
305 - 30 ml soxhlet extractors;
306 - 250 ml round-bottomed flask;
307 - Ground-in stopper NS 29/32;
308 - Dimroth condenser NS 29/32;
309 - Boiling stones (e.g. glass pearls or Raschig rings);
310 f) Extraction thimble (cellulose 30 ml, ID 22 mm, height 80 mm);
311 g) Glass wool (for extraction thimble);
312 h) Heating jackets;
313 i) Funnels;
314 j) Aluminium foil;
315 k) Cork rings;
316 l) 0,45 ㎛ PTFE filter;
317 m) Microlitre syringe or automatic pipettes;
318 n) Pasteur pipettes;
319 o) 2 ml sample vials and a screw cap with PTFE gasket or, depending on the analytical system, a
320 comparable sample receptacle;
321 p) Mini-shaker (also known as vortexer or vortex mixer)
322 q) Deactivated injector liner (for GC-MS)
323 r) Gas chromatograph - mass spectrometer, split/splitless inlet and a programmable temperature-
324 controlled oven. The mass spectrometer shall be able to perform selected ion monitoring (SIM) and
325 total ion current (“full scan”). The ionization box shall be treated for chemical stability, and controlled
326 at 230 ℃. Kinetic energy of 70 eV shall be applied in electron ionization (EI) mode.
327 NOTE The use of an auto-sampler is recommended to ensure repeatability.
328 s) Capillary column
329 t) 50 ml am
...