SIST EN IEC 62321-9:2021

Determination of certain substances in electrotechnical products - Part 9: Hexabromocyclododecane in polymers by chromatography-mass spectrometry (GC-MS)

This part of IEC 62321 specifies two techniques for the determination of
hexabromocyclododecane (HBCDD) in polymers of electrotechnical products.
The gas chromatography-mass spectrometry (GC-MS) test method is described in the
normative part of this document. The GC-MS method is suitable for the determination of
hexabromocyclododecane (HBCDD).
A method using high-pressure liquid chromatography-mass spectrometry (HPLC-MS) is given
in informative Annex A.
These test methods have been evaluated for use with EPS (expanded polystyrene foam),
XPS (extruded polystyrene foam) and ABS (acrylonitrile butadiene styrene) within the
concentration ranges as specified in Table 1. The use of this method for other types of materials
or concentration ranges outside those specified below has not been evaluated.
This document has the status of a horizontal standard in accordance with IEC Guide 108.

Verfahren zur Bestimmung von bestimmten Substanzen in Produkten der Elektrotechnik – Teil 9: Hexabromcyclododecan in Polymeren durch Chromatographie-Massenspektrometrie (GC-MS)

Détermination de certaines substances dans les produits électrotechniques - Partie 9: Hexabromocyclododécane dans les polymères par chromatographie en phase gazeuse-spectrométrie de masse (GC-MS)

L'IEC 62321-9:2021 spécifie deux techniques pour la détermination de l’hexabromocyclododécane (HBCDD) dans les polymères des produits électrotechniques.
La méthode d’essai par chromatographie en phase gazeuse-spectrométrie de masse (GC-MS) est décrite dans la partie normative du présent document. La méthode GC-MS convient à la détermination de l’hexabromocyclododécane (HBCDD).
L’Annexe A informative spécifie une méthode utilisant la chromatographie en phase liquide sous haute pression-spectrométrie de masse (HPLC-MS).
Ces méthodes d’essai ont été évaluées pour une utilisation avec une mousse EPS (polystyrène expansé), XPS (polystyrène extrudé) et de l’ABS (acrylonitrile-butadiène-styrène) dans les plages de concentrations spécifiées. L’utilisation de ces méthodes pour d’autres types de matériaux ou des plages de concentrations en dehors de celles spécifiées ci-dessous n’a pas été évaluée.
Le présent document a le statut d'une norme horizontale conformément au Guide IEC 108.

Določevanje posameznih snovi v elektrotehničnih izdelkih - 9. del: Heksabromociklododekan v polimerih s plinskim kromatografom z masnim spektrometrom (GC-MS)

General Information

• Status: Published
• Publication Date: 14-Nov-2021
• ICS: 29.020 - Electrical engineering 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: 6060 - National Implementation/Publication (Adopted Project)
• Start Date: 22-Oct-2021
• Due Date: 27-Dec-2021
• Completion Date: 15-Nov-2021
• Ref Project: EN IEC 62321-9:2021 - Determination of certain substances in electrotechnical products - Part 9: Hexabromocyclododecane in polymers by chromatography-mass spectrometry (GC-MS)

Standards Content (Sample)

SLOVENSKI STANDARD
SIST EN IEC 62321-9:2021
01-december-2021
Določevanje posameznih snovi v elektrotehničnih izdelkih - 9. del:
Heksabromociklododekan v polimerih s plinskim kromatografom z masnim
spektrometrom (GC-MS)
Determination of certain substances in electrotechnical products - Part 9:
Hexabromocyclododecane in polymers by chromatography-mass spectrometry (GC-MS)
Ta slovenski standard je istoveten z: EN IEC 62321-9:2021
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
SIST EN IEC 62321-9:2021 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST EN IEC 62321-9:2021


EUROPEAN STANDARD EN IEC 62321-9

NORME EUROPÉENNE

EUROPÄISCHE NORM
October 2021
ICS 13.020.01; 43.040.10

English Version
Determination of certain substances in electrotechnical products
- Part 9: Hexabromocyclododecane in polymers by
chromatography-mass spectrometry (GC-MS)
(IEC 62321-9:2021)
Détermination de certaines substances dans les produits Verfahren zur Bestimmung von bestimmten Substanzen in
électrotechniques - Partie 9: Hexabromocyclododécane Produkten der Elektrotechnik - Teil 9:
dans les polymères par chromatographie en phase Hexabromcyclododecan in Polymeren durch
gazeuse-spectrométrie de masse (GC-MS) Chromatographie-Massenspektrometrie (GC-MS)
(IEC 62321-9:2021) (IEC 62321-9:2021)
This European Standard was approved by CENELEC on 2021-10-04. CENELEC members are bound to comply with the CEN/CENELEC
Internal Regulations which stipulate the conditions for giving this European Standard the status of a national standard without any alteration.
Up-to-date lists and bibliographical references concerning such national standards may be obtained on application to the CEN-CENELEC
Management Centre or to any CENELEC member.
This European Standard exists in three official versions (English, French, German). A version in any other language made by translation
under the responsibility of a CENELEC member into its own language and notified to the CEN-CENELEC Management Centre has the
same status as the official versions.
CENELEC members are the national electrotechnical committees of Austria, Belgium, Bulgaria, Croatia, Cyprus, the Czech Republic,
Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, the
Netherlands, Norway, Poland, Portugal, Republic of North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland,
Turkey and the United Kingdom.


European Committee for Electrotechnical Standardization
Comité Européen de Normalisation Electrotechnique
Europäisches Komitee für Elektrotechnische Normung
CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels
© 2021 CENELEC All rights of exploitation in any form and by any means reserved worldwide for CENELEC Members.
 Ref. No. EN IEC 62321-9:2021 E

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SIST EN IEC 62321-9:2021
EN IEC 62321-9:2021 (E)
European foreword
The text of document 111/620/FDIS, future edition 1 of IEC 62321-9, prepared by IEC/TC 111
“Environmental standardization for electrical and electronic products and systems” was submitted to
the IEC-CENELEC parallel vote and approved by CENELEC as EN IEC 62321-9:2021.
The following dates are fixed:
• latest date by which the document has to be implemented at national (dop) 2022–07–04
level by publication of an identical national standard or by endorsement
• latest date by which the national standards conflicting with the (dow) 2024–10–04
document have to be withdrawn
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. CENELEC shall not be held responsible for identifying any or all such patent rights.
Any feedback and questions on this document should be directed to the users’ national committee. A
complete listing of these bodies can be found on the CENELEC website.
Endorsement notice
The text of the International Standard IEC 62321-9:2021 was approved by CENELEC as a European
Standard without any modification.
In the official version, for Bibliography, the following notes have to be added for the standards
indicated:
IEC 62321-2 NOTE Harmonized as EN 62321-2
IEC 62321-3-1 NOTE Harmonized as EN 62321-3-1
ISO 3696 NOTE Harmonized as EN ISO 3696
ISO 5667-1 NOTE Harmonized as EN ISO 5667-1
2

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SIST EN IEC 62321-9:2021
EN IEC 62321-9:2021 (E)
Annex ZA
(normative)

Normative references to international publications
with their corresponding European publications
The following documents are referred to in the text in such a way that some or all of their content
constitutes requirements of this document. For dated references, only the edition cited applies. For
undated references, the latest edition of the referenced document (including any amendments)
applies.
NOTE 1 Where an International Publication has been modified by common modifications, indicated by (mod), the
relevant EN/HD applies.
NOTE 2 Up-to-date information on the latest versions of the European Standards listed in this annex is available
here: www.cenelec.eu.
Publication Year Title EN/HD Year
IEC 62321-1 2013 Determination of certain substances in EN 62321-1 2013
electrotechnical products - Part 1:
Introduction and overview


3

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IEC 62321-9

®


Edition 1.0 2021-08




INTERNATIONAL



STANDARD




NORME


INTERNATIONALE




HORIZONTAL PUBLICATION

PUBLICATION HORIZONTALE




Determination of certain substances in electrotechnical products –

Part 9: Hexabromocyclododecane in polymers by gas chromatography-mass

spectrometry (GC‑MS)



Détermination de certaines substances dans les produits électrotechniques –

Partie 9: Hexabromocyclododécane dans les polymères par chromatographie


en phase gazeuse-spectrométrie de masse (GC‑MS)













INTERNATIONAL

ELECTROTECHNICAL

COMMISSION


COMMISSION

ELECTROTECHNIQUE


INTERNATIONALE




ICS 13.020.01; 43.040.10 ISBN 978-2-8322-9960-9




Warning! Make sure that you obtained this publication from an authorized distributor.

Attention! Veuillez vous assurer que vous avez obtenu cette publication via un distributeur agréé.

® Registered trademark of the International Electrotechnical Commission
Marque déposée de la Commission Electrotechnique Internationale

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CONTENTS
FOREWORD . 4
INTRODUCTION . 6
1 Scope . 7
2 Normative references . 7
3 Terms, definitions and abbreviated terms . 7
3.1 Terms and definitions . 7
3.2 Abbreviated terms . 8
4 Principle . 8
5 Reagents and materials . 8
6 Apparatus . 9
7 Sampling . 9
8 Procedure . 10
8.1 General instructions for the analysis . 10
8.2 Sample preparation . 10
8.2.1 Stock solution . 10
8.2.2 Pre-extraction of the Soxhlet extractors . 10
8.2.3 Soxhlet extraction . 10
8.2.4 Alternative extraction procedure for soluble polymers . 11
8.2.5 Addition of the internal standard (IS) . 11
8.3 Instrumental parameters . 11
8.4 Calibrants . 12
8.5 Calibration . 12
8.5.1 General . 12
8.5.2 Standard solutions . 12
9 Calculation of HBCDD concentration . 13
9.1 General . 13
9.2 Calculation . 13
10 Precision . 15
11 Quality assurance and quality control . 16
11.1 Performance . 16
11.2 Internal control samples and blanks . 17
11.3 Method detection limit (MDL) and reporting limit . 17
12 Test report . 18
Annex A (informative) Determination of HBCDD in polymers by high-pressure liquid
chromatography-mass spectrometry (HPLC-MS) . 19
A.1 Principle . 19
A.2 Reagents and materials . 19
A.3 Apparatus . 19
A.4 Sampling. 20
A.5 Procedure . 20
A.5.1 General instructions for the analysis . 20
A.5.2 Sample preparation . 20
A.5.3 Instrumental parameters . 21
A.5.4 Calibrants . 22
A.5.5 Calibration . 22

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A.6 Calculation of HBCDD concentration . 23
A.6.1 General . 23
A.6.2 Calculation . 23
A.7 Precision . 24
A.8 Quality assurance and quality control . 25
A.8.1 Performance . 25
A.8.2 Method detection limit (MDL) and reporting limit . 25
A.9 Test report . 26
Annex B (informative) Examples of chromatograms at suggested conditions . 27
Annex C (informative)  Results of international interlaboratory study (IIS 9) . 29
Bibliography . 31

Figure B.1 – Total ion chromatogram of HBCDD by GC‑MS analysis. 27
Figure B.2 – Mass spectrum of HBCDD by GC‑MS analysis . 27
Figure B.3 – Total ion chromatogram of HBCDD isomers (α-, β-, γ-HBCDD) by HPLC-
MS analysis . 28

Table 1 – Tested concentration ranges for HBCDD by GC‑MS in various materials . 7
Table 2 – Reference masses for the quantification of HBCDD . 12
Table 3 – Commercially available HBCDD reference materials considered suitable for
GC-MS analysis . 12
Table 4 – Calibration solutions of HBCDD . 13
Table 5 – IIS 9 repeatability and reproducibility . 16
Table A.1 – HPLC-MS liquid phase . 21
Table A.2 – Commercially available HBCDD reference materials considered suitable
for HPLC-MS analysis . 22
Table A.3 – Calibration solutions of HBCDD . 23
Table A.4 – IIS 9 repeatability and reproducibility . 25
Table C.1 – Mean results and recovery rates for HBCDD using GC‑MS . 29
Table C.2 – Statistical data for GC‑MS . 29
Table C.3 – Mean results and recovery rates for HBCDD using HPLC-MS . 29
Table C.4 – Statistical data for HPLC-MS . 30

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INTERNATIONAL ELECTROTECHNICAL COMMISSION
____________

DETERMINATION OF CERTAIN SUBSTANCES
IN ELECTROTECHNICAL PRODUCTS –

Part 9: Hexabromocyclododecane in polymers
by gas chromatography-mass spectrometry (GC‑MS)

FOREWORD
1) The International Electrotechnical Commission (IEC) is a worldwide organization for standardization comprising
all national electrotechnical committees (IEC National Committees). The object of IEC is to promote international
co-operation on all questions concerning standardization in the electrical and electronic fields. To this end and
in addition to other activities, IEC publishes International Standards, Technical Specifications, Technical Reports,
Publicly Available Specifications (PAS) and Guides (hereafter referred to as “IEC Publication(s)”). Their
preparation is entrusted to technical committees; any IEC National Committee interested in the subject dealt with
may participate in this preparatory work. International, governmental and non-governmental organizations liaising
with the IEC also participate in this preparation. IEC collaborates closely with the International Organization for
Standardization (ISO) in accordance with conditions determined by agreement between the two organizations.
2) The formal decisions or agreements of IEC on technical matters express, as nearly as possible, an international
consensus of opinion on the relevant subjects since each technical committee has representation from all
interested IEC National Committees.
3) IEC Publications have the form of recommendations for international use and are accepted by IEC National
Committees in that sense. While all reasonable efforts are made to ensure that the technical content of IEC
Publications is accurate, IEC cannot be held responsible for the way in which they are used or for any
misinterpretation by any end user.
4) In order to promote international uniformity, IEC National Committees undertake to apply IEC Publications
transparently to the maximum extent possible in their national and regional publications. Any divergence between
any IEC Publication and the corresponding national or regional publication shall be clearly indicated in the latter.
5) IEC itself does not provide any attestation of conformity. Independent certification bodies provide conformity
assessment services and, in some areas, access to IEC marks of conformity. IEC is not responsible for any
services carried out by independent certification bodies.
6) All users should ensure that they have the latest edition of this publication.
7) No liability shall attach to IEC or its directors, employees, servants or agents including individual experts and
members of its technical committees and IEC National Committees for any personal injury, property damage or
other damage of any nature whatsoever, whether direct or indirect, or for costs (including legal fees) and
expenses arising out of the publication, use of, or reliance upon, this IEC Publication or any other IEC
Publications.
8) Attention is drawn to the Normative references cited in this publication. Use of the referenced publications is
indispensable for the correct application of this publication.
9) Attention is drawn to the possibility that some of the elements of this IEC Publication may be the subject of patent
rights. IEC shall not be held responsible for identifying any or all such patent rights.
IEC 62321-9 has been prepared by IEC technical committee 111: Environmental
standardization for electrical and electronic products and systems. It is an International
Standard.
The text of this International Standard is based on the following documents:
FDIS Report on voting
111/620/FDIS 111/631/RVD

Full information on the voting for its approval can be found in the report on voting indicated in
the above table.
The language used for the development of this International Standard is English.

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SIST EN IEC 62321-9:2021
IEC 62321-9:2021 © IEC 2021 – 5 –
This document was drafted in accordance with ISO/IEC Directives, Part 2, and developed in
accordance with ISO/IEC Directives, Part 1 and ISO/IEC Directives, IEC Supplement, available
at www.iec.ch/members_experts/refdocs. The main document types developed by IEC are
described in greater detail at www.iec.ch/standardsdev/publications.
A list of all parts in the IEC 62321 series, published under the general title Determination of
certain substances in electrotechnical products, can be found on the IEC website
The committee has decided that the contents of this document will remain unchanged until the
stability date indicated on the IEC website under webstore.iec.ch in the data related to the
specific document. At this date, the document will be
• reconfirmed,
• withdrawn,
• replaced by a revised edition, or
• amended.

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INTRODUCTION
The widespread use of electrotechnical products has drawn increased attention to their impact
on the environment. In many countries this has resulted in the adoption of regulations affecting
wastes, substances and energy use of electrotechnical products.
The use of certain substances (e.g. lead (Pb), cadmium (Cd) and polybrominated diphenyl
ethers (PBDEs) in electrotechnical products is a source of concern in current and proposed
regional legislation.
The purpose of this document is therefore to provide test methods that will allow the
electrotechnical industry to determine the levels of certain substances of concern in
electrotechnical products on a consistent global basis.
WARNING – Persons using this document should be familiar with normal laboratory
practice. This document does not purport to address all of the safety problems, if any,
associated with its use. It is the responsibility of the user to establish appropriate safety
and health practices and to ensure compliance with any national regulatory conditions.

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DETERMINATION OF CERTAIN SUBSTANCES
IN ELECTROTECHNICAL PRODUCTS –

Part 9: Hexabromocyclododecane in polymers
by gas chromatography-mass spectrometry (GC‑MS)



1 Scope
This part of IEC 62321 specifies two techniques for the determination of
hexabromocyclododecane (HBCDD) in polymers of electrotechnical products.
The gas chromatography-mass spectrometry (GC-MS) test method is described in the
normative part of this document. The GC-MS method is suitable for the determination of
hexabromocyclododecane (HBCDD).
A method using high-pressure liquid chromatography-mass spectrometry (HPLC-MS) is given
in informative Annex A.
These test methods have been evaluated for use with EPS (expanded polystyrene foam),
XPS (extruded polystyrene foam) and ABS (acrylonitrile butadiene styrene) within the
concentration ranges as specified in Table 1. The use of this method for other types of materials
or concentration ranges outside those specified below has not been evaluated.
Table 1 – Tested concentration ranges for HBCDD by GC‑MS in various materials
Substance or element HBCDD
Medium or material tested
Unit of
Parameter
measurement ABS
EPS/XPS
mg/kg
Concentration range tested 6 080 to 11 940 1 000 to 10 000

This document has the status of a horizontal standard in accordance with IEC Guide 108.
2 Normative references
The following documents are referred to in the text in such a way that some or all of their content
constitutes requirements of this document. For dated references, only the edition cited applies.
For undated references, the latest edition of the referenced document (including any
amendments) applies.
IEC 62321-1:2013, Determination of certain substances in electrotechnical products – Part 1:
Introduction and overview
3 Terms, definitions and abbreviated terms
3.1 Terms and definitions
For the purposes of this document, the terms and definitions given in IEC 62321-1 apply.
ISO and IEC maintain terminological databases for use in standardization at the following
addresses:

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• IEC Electropedia: available at http://www.electropedia.org/
• ISO Online browsing platform: available at http://www.iso.org/obp
3.2 Abbreviated terms
ABS acrylonitrile butadiene styrene
API-ES atmospheric pressure-electrospray
BFR brominated flame retardant
BSA N,O-Bis(trimethylsilyl)acetamide
BSTFA N,O-Bis(trimethylsilyl)trifluoroacetamide
CCC continuing calibration check
C-IC combustion-ion chromatography
EI electron ionization
EPS expanded polystyrene foam
HBCDD hexabromocyclododecane
HPLC-MS high-pressure liquid chromatography-mass spectrometry
ID internal diameter
IS internal standard
GC‑MS gas chromatography-mass spectrometry
LOD limit of detection
LOQ limit of quantification
MDL method detection limit
PTFE polytetrafluoroethylene
QC quality control
RSD relative standard deviation
SIM single (or "selected") ion monitoring
THF tetrahydrofuran
TIF tentatively identified compound
XPS extruded polystyrene foam
XRF X-ray fluorescence
UV ultraviolet
4 Principle
HBCDD is determined using ultrasonic or Soxhlet extraction followed by gas chromatography
separation and mass spectrometry determination. This technique is suitable to determinate total
HBCDD instead of separated HBCDD isomers.
NOTE The thermal stability of HBCDD is poor. The results can be influenced by the temperature testing conditions.
5 Reagents and materials
All reagent chemicals shall be tested for contamination and blank values prior to application.
a) toluene (guaranteed reagent, purity of greater than a volume fraction of 99 %);
b) tetrahydrofuran (THF) (guaranteed reagent, purity of greater than a volume fraction of 99 %);
c) acetonitrile (guaranteed reagent, purity of greater than a volume fraction of 99 %);
d) methanol (guaranteed reagent, purity of greater than a volume fraction of 99 %);

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e) mixed solvent solution (tetrahydrofuran and acetonitrile or methanol),
– add 500 ml tetrahydrofuran and 1 000 ml acetonitrile or methanol to a 2 000 ml beaker
and mix;
f) calibrants hexabromocyclododecane (guaranteed reagent, purity of greater than a volume
fraction of 99 %): see 8.4;
g) helium (purity of greater than a volume fraction of 99,999 %);
h) internal standard used to correct for injection errors (e.g. CB 209 (2,2’,3,3’,4,4’,5,5’,6,6’-
decachlorobiphenyl)).
6 Apparatus
The following items shall be used for the analysis:
a) analytical balance capable of measuring accurately to 0,000 1 g;
b) 10 ml, 20 ml, 500 ml, 1 000 ml volumetric flasks;
c) Soxhlet device, Soxhlet extractor of 200 ml or suitable volume;
d) extraction thimble;
e) heating jackets;
f) funnel (non plastic);
g) aluminium foil;
h) ultrasonic bath;
i) Pasteur pipette;
j) glass wool;
k) 1,5 ml sample vials with 100 µl glass insert and a screw cap with polytetrafluoroethylene
(PTFE) gasket or, depending on the analytical system, a comparable sample receptacle;
l) a gas chromatograph with a capillary column coupled to a mass spectrometric detector
(electron ionization, EI). The mass spectrometric detector shall be able to perform selective
ion monitoring. The use of an autosampler is strongly recommended to ensure repeatability.
A column length of approximately 30 m is suitable for sufficient separation efficiency for
HBCDD;
m) rotary evaporator with water bath;
n) milling equipment;
o) 0,45 µm PTFE filter membrane.
p) No. 5A filter paper.
7 Sampling
As described in IEC 62321-2, unless indicated otherwise, the following procedure a) is
recommended.
a) Cut samples approximately to a size of 2 mm × 2 mm, and mix them well.
NOTE 1 When using the alternative ultrasonic dissolution procedure for polymers that are difficult to dissolve,
cryogenic grinding with liquid nitrogen cooling is necessary. The samples are ground to pass through a 500 µm
sieve.
NOTE 2 Contact with polymer material are avoided during sampling.

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8 Procedure
8.1 General instructions for the analysis
The following general instructions shall be followed:
In order to reduce blank values, ensure the cleanliness of all glass equipment (excluding
volumetric flasks) and deactivate the glass wool by subjecting it to 450 °C for at least 30 min.
To avoid decomposition and/or debromination of HBCDD by UV light during extraction and
analysis, glass equipment made from brown or amber glass shall be used.
NOTE If no brown or amber glass is available, aluminium foil can be used for protection from light.
If the amount of Br in the sample (determined by XRF, C-IC or other means) is considerably
above the 0,1 % range, it will be necessary to carry out the analysis using an adjusted sample
size or by repeating the analysis using an extract that has been appropriately diluted prior to
internal standard addition.
8.2 Sample preparation
8.2.1 Stock solution
a) Standard mixture solution: Prepare a standard mixture solution containing α, β, γ-HBCDD
in an organic solvent at a concentration of 10 µg/ml made from e
...