prEN IEC 62321-13:2025
(Main)Determination of certain substances in electrotechnical products - Part 13: Bisphenol a in plastics by liquid chromatography-diode array detection (LC-DAD), liquid chromatography-mass spectrometry (LC-MS) and liquid chromatography-tandem mass spectrometry (LC-MS/MS)
Determination of certain substances in electrotechnical products - Part 13: Bisphenol a in plastics by liquid chromatography-diode array detection (LC-DAD), liquid chromatography-mass spectrometry (LC-MS) and liquid chromatography-tandem mass spectrometry (LC-MS/MS)
Détermination de certaines substances dans les produits électrotechniques - Partie 13: Bisphénol a dans les plastiques par chromatographie en phase liquide avec détection à barrettes de diodes (LC-DAD), par chromatographie en phase liquide avec spectrométrie de masse (LC-MS) et par chromatographie en phase liquide avec spectrométrie de masse en tandem (LC-MS/MS)
Določevanje posameznih snovi v elektrotehničnih izdelkih - 13. del: Določevanje bisfenola A v plastiki s tekočinsko kromatografijo - določevanje s serijo diod (LC-DAD), tekočinsko kromatografijo - masno spektrometrijo (LC-MS) in tekočinsko kromatografijo - tandemsko masno spektrometrijo (LC-MS/MS)
General Information
Standards Content (Sample)
SLOVENSKI STANDARD
01-april-2025
Določevanje posameznih snovi v elektrotehničnih izdelkih - 13. del: Določevanje
bisfenola A v plastiki s tekočinsko kromatografijo - določevanje s serijo diod (LC-
DAD), tekočinsko kromatografijo - masno spektrometrijo (LC-MS) in tekočinsko
kromatografijo - tandemsko masno spektrometrijo (LC-MS/MS)
Determination of certain substances in electrotechnical products - Part 13: Bisphenol A
in plastics by liquid chromatography-diode array detection (LC-DAD), liquid
chromatography-mass spectrometry (LC-MS) and liquid chromatography-tandem mass
spectrometry (LC-MS/MS)
Détermination de certaines substances dans les produits électrotechniques - Partie 13:
Bisphénol A dans les plastiques par chromatographie en phase liquide avec détection à
barrettes de diodes (LC-DAD), par chromatographie en phase liquide avec spectrométrie
de masse (LC-MS) et par chromatographie en phase liquide avec spectrométrie de
masse en tandem (LC-MS/MS)
Ta slovenski standard je istoveten z: prEN IEC 62321-13:2025
ICS:
13.020.01 Okolje in varstvo okolja na Environment and
splošno environmental protection in
general
43.040.10 Električna in elektronska Electrical and electronic
oprema equipment
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
111/799/CDV
COMMITTEE DRAFT FOR VOTE (CDV)
PROJECT NUMBER:
IEC 62321-13 ED1
DATE OF CIRCULATION: CLOSING DATE FOR VOTING:
2025-01-17 2025-04-11
SUPERSEDES DOCUMENTS:
111/685/CD, 111/790/CC
IEC TC 111 : ENVIRONMENTAL STANDARDIZATION FOR ELECTRICAL AND ELECTRONIC PRODUCTS AND SYSTEMS
SECRETARIAT: SECRETARY:
Italy Mr Alfonso Sturchio
OF INTEREST TO THE FOLLOWING COMMITTEES: HORIZONTAL FUNCTION(S):
TC 2,TC 9,TC 18,TC 20,TC 21,TC 23,TC 34,SC 34D,TC
TC 111 Horizontal Basic Environment - Assessment
59,TC 62,SC 65B,TC 80,TC 82,TC 88,TC 91,TC 100,TC
121,TC 124,TC 125
ASPECTS CONCERNED:
Environment
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.
Recipients of this document are invited to submit, with their comments, notification of any relevant “In Some Countries”
clauses to be included should this proposal proceed. Recipients are reminded that the CDV stage is the final stage for
submitting ISC clauses. (SEE AC/22/2007 OR NEW GUIDANCE DOC).
TITLE:
Determination of certain substances in electrotechnical products – Part 13: Bisphenol A in plastics by
liquid chromatography-diode array detection (LC-DAD), liquid chromatography-mass spectrometry (LC-
MS) and liquid chromatography-tandem mass spectrometry (LC-MS/MS)
PROPOSED STABILITY DATE: 2029
NOTE FROM TC/SC OFFICERS:
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.
111/799/CDV -2- IEC CDV 62321-13 © IEC 2025
1 CONTENTS
2 FOREWORD . 3
3 INTRODUCTION . 5
4 1 Scope . 6
5 2 Normative references . 6
6 3 Definitions. 6
7 3.1 Terms and definitions . 6
8 3.2 Abbreviations . 6
9 4 Principle . 7
10 5 Reagents and materials . 7
11 6 Apparatus . 8
12 7 Sampling. 8
13 8 Procedure . 8
14 8.1 General instructions for the analysis. 8
15 8.2 Sample preparation . 9
16 8.2.1 Stock solution . 9
17 8.2.2 Extraction . 9
18 8.3 Instrumental parameters . 9
19 8.3.1 Stationary phase . 9
20 8.3.2 Liquid (mobile) phase . 9
21 8.4 Calibrants. 9
22 8.5 Calibration. 10
23 8.5.1 General . 10
24 8.5.2 Standard solutions . 10
25 9 Calculation of BPA concentration . 11
26 9.1 General . 11
27 9.2 Calculation . 11
28 10 Precision data . 12
29 10.1 LC-DAD Method . 12
30 10.2 LC-MS Method . 13
31 10.3 LC-MS/MS Method . 15
32 11 Quality assurance and quality control . 16
33 11.1 Performance . 16
34 11.2 Internal control samples and blanks . 17
35 11.3 Method detection limit and reporting limit . 17
36 12 Test report . 18
37 Annex A (informative) Conditions of each instrument . 19
38 Annex B (informative) Examples of chromatograms at suggested conditions . 22
39 Annex C (informative) Results of preliminary international Interlaboratory study (Pre-IIS 13)24
40 Annex D (informative) Results of International Interlaboratory study (IIS 13) . 27
111/799/CDV -3- IEC CDV 62321-13 © IEC 2025
42 INTERNATIONAL ELECTROTECHNICAL COMMISSION
43 ____________
45 DETERMINATION OF CERTAIN SUBSTANCES
46 IN ELECTROTECHNICAL PRODUCTS –
48 Part 13: Bisphenol A in plastics by liquid chromatography-diode array detector
49 (LC-DAD), liquid chromatography-mass spectrometry (LC-MS) and liquid
50 chromatography-tandem mass spectrometry (LC/MS-MS)
52 FOREWORD
53 1) The International Electrotechnical Commission (IEC) is a worldwide organization for standardization comprising all national
54 electrotechnical committees (IEC National Committees). The object of IEC is to promote international co-operation on all
55 questions concerning standardization in the electrical and electronic fields. To this end and in addition to other activities,
56 IEC publishes International Standards, Technical Specifications, Technical Reports, Publicly Available Specifications (PAS)
57 and Guides (hereafter referred to as “IEC Publication(s)”). Their preparation is entrusted to technical committees; any IEC
58 National Committee interested in the subject dealt with may participate in this preparatory work. International, governmental
59 and non-governmental organizations liaising with the IEC also participate in this preparation. IEC collaborates closely with
60 the International Organization for Standardization (ISO) in accordance with conditions determined by agreement between
61 the two organizations.
62 2) The formal decisions or agreements of IEC on technical matters express, as nearly as possible, an international consensus
63 of opinion on the relevant subjects since each technical committee has representation from all interested IEC National
64 Committees.
65 3) IEC Publications have the form of recommendations for international use and are accepted by IEC National Committees in
66 that sense. While all reasonable efforts are made to ensure that the technical content of IEC Publications is accurate, IEC
67 cannot be held responsible for the way in which they are used or for any misinterpretation by any end user.
68 4) In order to promote international uniformity, IEC National Committees undertake to apply IEC Publications transparently to
69 the maximum extent possible in their national and regional publications. Any divergence between any IEC Publication and
70 the corresponding national or regional publication shall be clearly indicated in the latter.
71 5) IEC itself does not provide any attestation of conformity. Independent certification bodies provide conformity assessment
72 services and, in some areas, access to IEC marks of conformity. IEC is not responsible for any services carried out by
73 independent certification bodies.
74 6) All users should ensure that they have the latest edition of this publication.
75 7) No liability shall attach to IEC or its directors, employees, servants or agents including individual experts and members of
76 its technical committees and IEC National Committees for any personal injury, property damage or other damage of any
77 nature whatsoever, whether direct or indirect, or for costs (including legal fees) and expenses arising out of the publication,
78 use of, or reliance upon, this IEC Publication or any other IEC Publications.
79 8) Attention is drawn to the Normative references cited in this publication. Use of the referenced publications is indispensable
80 for the correct application of this publication.
81 9) Attention is drawn to the possibility that some of the elements of this IEC Publication may be the subject of patent rights.
82 IEC shall not be held responsible for identifying any or all such patent rights.
83 IEC 62321 has been prepared by technical committee 111: ENVIRONMENTAL STANDARDIZATION
84 FOR ELECTRICAL AND ELECTRONIC PRODUCTS AND SYSTEMS. It is an International Standard.
85 The text of this International Standard is based on the following documents:
FDIS Report on voting
XX/XX/FDIS XX/XX/RVD
87 Full information on the voting for its approval can be found in the report on voting indicated in the above
88 table.
89 The language used for the development of this International Standard is English.
111/799/CDV -4- IEC CDV 62321-13 © IEC 2025
90 This document was drafted in accordance with ISO/IEC Directives, Part 2, and developed in accordance
91 with ISO/IEC Directives, Part 1 and ISO/IEC Directives, IEC Supplement, available at
92 www.iec.ch/members_experts/refdocs. The main document types developed by IEC are described in
93 greater detail at www.iec.ch/standardsdev/publications.
94 The committee has decided that the contents of this document will remain unchanged until the stability
95 date indicated on the IEC website under "http://webstore.iec.ch" in the data related to the specific
96 document. At this date, the document will be
97 • reconfirmed,
98 • withdrawn,
99 • replaced by a revised edition, or
100 • amended.
111/799/CDV -5- IEC CDV 62321-13 © IEC 2025
101 INTRODUCTION
102 The widespread use of electrotechnical products has drawn increased attention to their impact on the
103 environment. In many countries this has resulted in the adaptation of regulations affecting waste,
104 substances and energy use of electrotechnical products.
105 The use of certain substances (e.g. lead (Pb), cadmium (Cd), mercury (Hg) and polybrominated diphenyl
106 ethers (PBDEs)), phthalates in electronical products is a source of concern in current and proposed
107 regional legislation.
108 The purpose of the IEC 62321 series is therefore to provide test methods that will allow the
109 electrotechnical industry to determine the levels of certain substances of concern in electrotechnical
110 products on a consistent global basis.
111 This first edition of IEC 62321-13 introduces a new subject covering Bisphenol A in the IEC 62321 series.
112 WARNING — Persons using this International Standard should be familiar with normal laboratory
113 practice. This standard does not purport to address all of the safety problems, if any, associated
114 with its use. It is the responsibility of the user to establish appropriate safety and health practices
115 and to ensure compliance with any national regulatory conditions.
111/799/CDV -6- IEC CDV 62321-13 © IEC 2025
116 DETERMINATION OF CERTAIN SUBSTANCES
117 IN ELECTROTECHNICAL PRODUCTS –
119 Part 13: Bisphenol A in plastics by liquid chromatography-diode array detector
120 (LC-DAD), liquid chromatography-mass spectrometry (LC-MS) and liquid
121 chromatography-tandem mass spectrometry (LC/MS-MS)
124 1 Scope
125 This International standard specifies three techniques for the determination of free Bisphenol A (BPA)
126 in plastics of electrotechnical products.
127 The liquid chromatography – diode array detector (LC-DAD) and liquid chromatography mass
128 spectrometry (LC-MS) and liquid chromatography tandem mass spectrometry (LC-MS/MS). These test
129 methods are described in the normative part of this standard. These test methods have been evaluated for
130 use with PC, PC/ABS, PP matrices containing free BPA between 20 mg/kg to 500 mg/kg as shown in the Pre-
131 IIS 13 results in Annex C and IIS 13 results in Annex D. The use of these methods for BPA concentration
132 ranges of plastics, other than those specified in Annex C, Annex D has not been evaluated.
133 2 Normative references
134 The following documents are referred to in the text in such a way that some or all of their content
135 constitutes requirements of this document. For dated references, only the edition cited applies. For
136 undated references, the latest edition of the referenced document (including any amendments) applies.
137 IEC 62321-1 – Determination of certain substances in electrotechnical products – Part 1: Introduction
138 and overview
139 IEC 62321-2 – Determination of certain substances in electrotechnical products – Part 2: Disassembly,
140 disjunction and mechanical sample preparation
141 ISO 3696:1987 – Water for analytical laboratory use – Specification and test
142 3 Definitions
143 3.1 Terms and definitions
144 For the purposes of this document, the terms and definitions provided in IEC 62321-1 and the following
145 terms and definitions apply.
146 ISO and IEC maintain terminological databases for use in standardization at the following addresses:
147 • IEC Electropedia: available at http://www.electropedia.org/
148 • ISO Online browsing platform: available at http://www.iso.org/obp
149 3.1.1 Free Bisphenol A
150 Refers to chemically unbound BPA, as present in material.
151 3.2 Abbreviations
152 For the purpose of this document, the following abbreviations apply.
ABS Acrylonitrile-butadiene-styrene
111/799/CDV -7- IEC CDV 62321-13 © IEC 2025
API-ES Atmospheric pressure ionization – Electrospray
BPA Bisphenol A
BPC Bisphenol C
CCC Continuing calibration check standard
CRM Certified reference material
IS Internal standard
LC Liquid chromatography
LC-DAD Liquid chromatography-diode array detector
LC-MS Liquid chromatography-mass spectrometry
LC-MS/MS Liquid chromatography-tandem mass spectrometry
MDL Method detection limit
PC Polycarbonate
PC/ABS Polycarbonate/ Acrylonitrile-butadiene-styrene
PP Polypropylene
PTFE Polytetrafluoroethylene
QC Quality control
RSD Relative standard deviation
TRM Traceable reference material
153 4 Principle
154 Free BPA is determined using ultrasonic extraction followed by high performance liquid chromatography
155 separation and tandem mass spectrometry and liquid chromatography-diode array detection. When
156 analysing free BPA in PC and type of epoxy resin samples, thermal stress to the sample should be
157 avoided during sample preparation (see section 7), as heat can affect the result.
158 5 Reagents and materials
159 The reagent chemicals used for the tests described in this standard shall have a minimum purity as
160 described in a) to i). This is intended to ensure the reagents are free from contamination and prevent
161 proliferation of blank values. There is a risk of elevated blank values due to the ubiquitous nature of
162 BPA (CAS #80-05-7). Laboratories should assure to verify the blank value of the test method especially
163 in case the calibration curve shows an offset.
164 a) Methanol (Purity LC grade or higher);
111/799/CDV -8- IEC CDV 62321-13 © IEC 2025
165 b) Tetrahydrofuran (Purity LC grade or higher);
166 c) Water (Purified water, quality of the mobile phase ingredients and solution or according to ISO
167 3696:1987, Grade 1);
168 d) Acetonitrile (Purity LC grade or higher);
169 e) Mixed solvent solution (1:1 Methanol and water),
170 - Add 500 ml methanol and 500 ml water to 1 l beaker and mix.
171 f) 10 mM ammonium acetate buffer solution
172 - Add 0,771 g ammonium acetate in a 1 l beaker (6.h), dissolve with a little purified water (5.c), then
173 add 900 ml purified water. Transfer to 1 l volumetric flask and add 10 ml acetonitrile and dilute with
174 purified water to the marked line.
175 g) Calibrants, BPA (Purity of greater than a mass fraction of 99 %);
176 h) Internal standard used to correct for injection (e.g. BPA-d , BPA-d , BPC);
16 8
177 i) 0,04 % Phosphoric acid buffer solution
178 - Add about 0,471 ml 85 % Phosphoric acid in a 1 l volumetric flask (6.b) and dilute with purified
179 water to the marked line.
180 NOTE To prevent exothermal reaction fill volumetric flask to half of water and then add acid. Then fill to the mark with
181 purified water.
182 6 Apparatus
183 The following items shall be used for the analysis:
184 a) Analytical balance having an accuracy of 0,000 1 g;
185 b) 10 ml, 100 ml, 1 l volumetric flasks (glass);
186 c) Ultrasonic bath; with a minimum power of 200 W and a bath area of 706 cm , corresponding to 0,28
187 W/cm , without a basket and with an internal or external thermostat.
188 d) Pasteur pipette (glass);
189 e) 1,5 ml sample vials with 100 µl glass insert and a screw cap with polytetrafluoroethylene (PTFE)
190 gasket or, depending on the analytical system, a comparable sample receptacle;
191 f) 0,45 µm PTFE filter membrane;
192 g) Centrifuge; with over 3 000 r/min
193 h) 1 l beaker (glass)
194 i) Minimum 40 ml vial (glass)
195 7 Sampling
196 As described in IEC 62321-2 unless otherwise indicated, the following procedure shall be used.
197 Cut samples approximately to a size of 2 mm x 2 mm, and homogenise. Contact with possible sources
198 of BPA-contamination shall be avoided during sampling.
199 NOTE Heat can cause the formation of additional free BPA. Avoid using devices that generate heat (e.g. circular saw).
200 8 Procedure
201 8.1 General instructions for the analysis
202 The following general instructions shall be followed:
203 a) In order to reduce blank values, ensure the cleanliness of all glass and analytical equipment;
111/799/CDV -9- IEC CDV 62321-13 © IEC 2025
204 b) If the amount of BPA in the sample is considerably above the calibration range, it will be necessary
205 to carry out the analysis using an adjusted sample size or by repeating the analysis using an extract
206 that has been appropriately diluted prior to internal standard addition.
207 8.2 Sample preparation
208 8.2.1 Stock solution
209 a) Standard solution for calibration: Prepare a standard solution containing Bisphenol A 1 000 µg/ml in
210 Tetrahydrofuran (5.b).
211 b) Internal standard for LC-MS and LC-MS/MS: 4 µg/ml in Tetrahydrofuran (5.b) (e.g. BPC, BPA-d ,
212 BPA-d )
213 c) Internal standard for LC-DAD: 40 µg/ml in Tetrahydrofuran (5.b) (e.g. BPC)
214 d) Dilution solution: 10 ml of internal standard (8.2.1.b or 8.2.1.c) in 30 ml of mixed solvent (5.e)
215 8.2.2 Extraction
216 a) Weigh approximately 1 g of the sample and transfer it into a tared vial. Record the mass to the
217 nearest 0,01 g. Lower sample weights can be tested.
218 b) Add 10 ml of IS solution (8.2.1.b or 8.2.1.c) to the vial;
219 c) Tightly cap the sample vial. Place it in an ultrasonic bath (6.c) and sonicate at 40 °C for 60 min.;
220 d) After the sample has extracted, allow the vial to cool to ambient temperature;
221 e) Accurately add 30 ml of mixed solvent (5.e) dropwise into the vial to precipitate the sample matrix;
222 f) Allow the resulting extracted solution to stand at room temperature for 30 min.;(When necessary use
223 centrifuge (6.g) for 10 min to precipitated the sample matrix down with 3 000 r/min)
224 g) Filter the sample solution through a 0,45 µm PTFE membrane (6.f) and transfer into a vial for LC
225 analysis.
226 8.3 Instrumental parameters
227 Different conditions might be necessary to optimize a specific LC system to achieve effective
228 determination of free BPA and meet the QC and MDL requirements. The following parameters have
229 been found suitable and are provided as an example:
230 NOTE Additional detailed instrument parameters are described in Annex A and Annex B
231 8.3.1 Stationary phase
232 a) C Column, 150 mm x 2,1 mm ID, 5 μm or equivalent;
233 b) C Column, 250 mm x 4,6 mm ID, 5 μm or equivalent.
234 8.3.2 Liquid (mobile) phase
235 Water (5.c) and Acetonitrile (5.d) are used as liquid phases.
236 8.4 Calibrants
237 Table 1 shows BPA reference materials suitable for this analysis.
238 Table 1 – Commercially available BPA reference material considered suitable for this analysis
Compound name CAS Number
BPA 80-05-7
BPA-d 96210-87-6
BPA-d 92739-58-7
111/799/CDV -10- IEC CDV 62321-13 © IEC 2025
BPC 79-97-0
239 8.5 Calibration
240 8.5.1 General
241 Wherever possible, the solvent used for the sample and standard solutions are to be the same to avoid
242 any potential solvent effects. A calibration curve shall be developed for quantitative analysis. At least
243 four calibration solutions shall be prepared. Quantification is made on the basis of the measurement of
244 the peak areas. The linear regression fit of each calibration curve is required to have a relative standard
245 deviation (RSD) of less than or equal to 15 % of the linear calibration function. If the RSD of 15% is
246 exceeded the calibration needs to be repeated.
247 8.5.2 Standard solutions
248 A standard stock solution of BPA (reference material Table 1.) is prepared by dissolving appropriate
249 amounts of BPA using the appropriate dilution solution 8.2.1.d to achieve a final BPA standard stock
250 solution concentration of 10 µg/ml. This standard stock solution can be diluted using the appropriate
251 dilution solution (8.2.1.d) to achieve final calibration solutions shown in Table 2 and 3. This procedure
252 ensures a constant IS concentration of 1 µg/ml (LC-MS or LC-MS/MS) or 10 µg/ml (LC-DAD),
253 respectively).
254 Table 2 – Preparation of low concentrations of Calibration standard solutions of BPA
Standard solution Final concentration of BPA Final concentration of internal
No. (µg/ml) standard (µg/ml)
1 0,01 1,0
2 0,02 1,0
3 0,05 1,0
4 0,1 1,0
5 0,2 1,0
255 Table 3 – Preparation of high concentrations of Calibration standard solutions of BPA
Standard solution Final concentration of BPA Final concentration of internal
No. (µg/ml) standard (µg/ml)
1 0,1 10
2 0,2 10
3 0,5 10
4 1,0 10
5 2,0 10
256 NOTE Concentration ranges of the calibration standard solutions can be adjusted depending on instrument performance.
111/799/CDV -11- IEC CDV 62321-13 © IEC 2025
257 The internal standard is used for the correction of the injection error. Therefore evaluation of the
258 response factor or ratio is carried out by A/A .
IS
259 To produce calibration straight lines, the response A/A is plotted against the concentration ratio C/C .
IS IS
260 A linear regression is carried out using the following Equation 1:
AC
=α× +β
(1)
AC
IS IS
261 Where
262 A is the peak area of BPA in the calibration solution;
263 A is the peak area of the internal standard;
IS
264 C is the concentration of BPA in the calibr
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.
Loading comments...