SIST EN 62321-6:2015
(Main)Determination of certain substances in electrotechnical products - Part 6: Polybrominated biphenyls and polybrominated diphenyl ethers in polymers by gas chromatography-mass spectrometry (GC-MS) - Ion Attachment Mass Spectrometry (IAMS) and High Pressure Liquid Chromatography - Ultra Violet detection (HPLC-UV) (IEC 62321-6:2015)
Determination of certain substances in electrotechnical products - Part 6: Polybrominated biphenyls and polybrominated diphenyl ethers in polymers by gas chromatography-mass spectrometry (GC-MS) - Ion Attachment Mass Spectrometry (IAMS) and High Pressure Liquid Chromatography - Ultra Violet detection (HPLC-UV) (IEC 62321-6:2015)
This Part of IEC 62321 specifies one normative and two informative techniques for the
determination of polybrominated biphenyls (PBB) and diphenyl ethers (PBDE) in polymers of
electrotechnical products.
The gas chromatography–mass spectrometry (GC-MS) test method is suitable for the
determination of monobrominated to decabrominated biphenyls (PBB) and monobrominated to
decabrominated diphenyl ethers (PBDE).
Annexes A and C contain methods using ion attachment mass spectrometry (IAMS) coupled
with direct injection probe (DIP) and high-pressure liquid chromatography coupled to photo
diode array ultra violet detector (HPLC-PDA/UV). These techniques have utility as fast,
qualitative or semi-quantitative type methods but are subject to limitations including
interferences or the number or type of PBB and PBDE compounds within their scope.
The ion attachment mass spectrometry (IAMS) technique is limited to the determination of
decabromo biphenyl and technical mixtures of decabromodiphenyl ether, octabromodiphenyl
ether, and pentabromo diphenyl ether flame retardant compounds. The determination of other
PBBs or PBDEs by this method has not been evaluated.
The high-pressure liquid chromatography technique is limited to the determination of technical
mixtures of decabromodiphenyl ether, octabromo diphenyl ether, decabromo biphenyl and
octabromo biphenyl technical flame retardants. The determination of other PBBs or PBDEs by
this method has not been evaluated.
These test methods have been evaluated for use with PS-HI (polystyrene, high-impact) and
PC/ABS (a blend of polycarbonate and acrylonitrile butadiene styrene) containing individual
PBDEs between 20 mg/kg to 2 000 mg/kg and total PBDEs between 1 300 mg/kg to 5 000
mg/kg as depicted in this standard including in Annex F. The use of these methods for other
polymer types, PBBs or other PBDE compounds or concentration ranges other than those
specified above has not been specifically evaluated.
Verfahren zur Bestimmung von bestimmten Substanzen in Produkten der Elektrotechnik - Teil 6: Polybromierte Biphenyl- und Diphenylether in Polymeren durch Gaschromatographie-Massenspektrometrie (GC-MS) (IEC 62321-6:2015)
Détermination de certaines substances dans les produits électrotechniques - Partie 6: Diphényles polybromés et diphényléthers polybromés dans des polymères par chromatographie en phase gazeuse, Spectrométrie de masse (GC-MS) - Spectrométrie de masse à ions attachés (IAMS) et chromatographie liquide à haute pression - Détection des ultraviolets (HPLC-UV) (IEC 62321-6:2015)
L'IEC 62321-6:2015 spécifie une technique normative et deux techniques informatives de détermination de diphényles polybromés (PBB) et de diphényléthers polybromés (PBDE) dans des polymères de produits électrotechniques. Les méthodes de test sont:
- La méthode d'essai de chromatographie en phase gazeuse - spectrométrie de masse (GC-MS);
- La technique de la spectrométrie de masse à ions attachés (IAMS) et
- La technique de la chromatographie liquide à haute pression. La première édition de l'IEC 62321:2008 était une norme "autonome" qui incluait une introduction, une vue d'ensemble des méthodes d'essai, la préparation mécanique des échantillons et différents articles relatifs à des méthodes d'essai. Cette première édition de l'IEC 62321-6 remplace en partie l'IEC 62321:2008, formant une révision structurelle et remplaçant en général l'Annexe A.
Določevanje posameznih substanc v elektrotehniških izdelkih - 6. del: Določevanje polibromiranih bifenilov in polibromiranih difeniletrov v polimerih s plinsko kromatografijo-masno spektrometrijo (GC-MS) - Masna spektrometrija s pripenjanjem iona (IAMS) in tekočinska kromatografija visoke ločljivosti z UV-detekcijo (HPLC-UV) (IEC 62321-6:2015)
Ta del standarda IEC 62321 določa eno normativno in dve informativni tehniki za določanje polibromiranih bifenilov (PBB) in difenil etrov (PBDE) v polimerih elektrotehničnih izdelkov.
Preskusna metoda plinske kromatografije z masno spektrometrijo (GC-MS) je primerna za določanje monobromiranih do dekabromiranih bifenilov (PBB) in monobromiranih do dekabromiranih difenil etrov (PBDE).
Dodatka A in C vsebujeta metode, v katerih se uporablja masna spektrometrija s pripenjanjem iona (IAMS) in sonda direktnega vbrizgavanja (DIP) ter visokotlačna tekočinska kromatografija v povezavi z UV-detekcijo (HPLC-PDA/UV). Te tehnike so uporabne kot hitre, kakovostne in semi-kvantitativne metode, vendar so predmet omejitev, ki vključujejo motnje ali število oz. vrsto spojin PBB in PBDE v okviru njihovega področja. Tehnika masne spektrometrije s pripenjanjem iona (IAMS) je omejena na določanje dekabromobifenila in na ogenj odpornih tehničnih mešanic dekabromodifeniletra, oktabromodifeniletra in pentabromodifeniletra. Določevanje drugih substanc PBB ali PBDE s to metodo ni ocenjeno. Tehnika visokotlačne tekočinske kromatografije je omejena na določevanje na ogenj odpornih tehničnih mešanic dekabromodifeniletra, oktabromodifeniletra, dekabromobifenila in oktabromobifenila. Določevanje drugih substanc PBB ali PBDE s
to metodo ni ocenjeno. Te preskusne metode so bile ocenjene za uporabo s PS-HI (polistiren visoke udarne žilavosti) in PC/ABS (mešanico polikarbonata in akrilonitril butadien stirena), ki vsebujejo posamezne substance PDBE od 20 mg/kg do 2000 mg/kg in skupnih PDBE od 1 300 mg/kg do 5000 mg/kg, kot je opisano v tem standardu, vključno z Dodatkom F. Uporaba teh metod za druge vrste polimerov, spojin PBB ali drugih spojin PBDE ali koncentracij, razen zgoraj navedenih, ni bila posebej ovrednotena.
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
SIST EN 62321-6:2015
01-december-2015
1DGRPHãþD
SIST EN 62321:2009
'RORþHYDQMHSRVDPH]QLKVXEVWDQFYHOHNWURWHKQLãNLKL]GHONLKGHO 'RORþHYDQMH
SROLEURPLUDQLKELIHQLORYLQSROLEURPLUDQLKGLIHQLOHWURYYSROLPHULKVSOLQVNR
NURPDWRJUDILMRPDVQRVSHNWURPHWULMR *&06 0DVQDVSHNWURPHWULMDV
SULSHQMDQMHPLRQD ,$06 LQWHNRþLQVNDNURPDWRJUDILMDYLVRNHORþOMLYRVWL]89
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Determination of certain substances in electrotechnical products - Part 6: Polybrominated
biphenyls and polybrominated diphenyl ethers in polymers by gas chromatography-mass
spectrometry (GC-MS) - Ion Attachment Mass Spectrometry (IAMS) and High Pressure
Liquid Chromatography - Ultra Violet detection (HPLC-UV) (IEC 62321-6:2015)
Verfahren zur Bestimmung von bestimmten Substanzen in Produkten der Elektrotechnik
- Teil 6: Polybromierte Biphenyl- und Diphenylether in Polymeren durch
Gaschromatographie-Massenspektrometrie (GC-MS) (IEC 62321-6:2015)
Ta slovenski standard je istoveten z: EN 62321-6:2015
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 62321-6:2015 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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SIST EN 62321-6:2015
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SIST EN 62321-6:2015
EUROPEAN STANDARD EN 62321-6
NORME EUROPÉENNE
EUROPÄISCHE NORM
August 2015
ICS 13.020; 43.040.10 Supersedes EN 62321:2009 (partially)
English Version
Determination of certain substances in electrotechnical products
- Part 6: Polybrominated biphenyls and polybrominated diphenyl
ethers in polymers by gas chromatography-mass spectrometry
(GC-MS)
(IEC 62321-6:2015)
Détermination de certaines substances dans les produits Verfahren zur Bestimmung von bestimmten Substanzen in
électrotechniques - Partie 6: Diphényles polybromés et Produkten der Elektrotechnik - Teil 6: Polybromierte
diphényléthers polybromés dans des polymères par Biphenyl- und Diphenylether in Polymeren durch
chromatographie en phase gazeuse-spectrométrie de Gaschromatographie-Massenspektrometrie (GC-MS)
masse (GC-MS) (IEC 62321-6:2015)
(IEC 62321-6:2015)
This European Standard was approved by CENELEC on 2015-07-10. 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, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia,
Lithuania, Luxembourg, Malta, the Netherlands, Norway, Poland, Portugal, Romania, 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: Avenue Marnix 17, B-1000 Brussels
© 2015 CENELEC All rights of exploitation in any form and by any means reserved worldwide for CENELEC Members.
Ref. No. EN 62321-6:2015 E
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SIST EN 62321-6:2015
EN 62321-6:2015
European foreword
The text of document 111/368/FDIS, future edition 1 of IEC 62321-6, 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 62321-6:2015.
The following dates are fixed:
(dop) 2016-04-10
• latest date by which the document has to be
implemented at national level by
publication of an identical national
standard or by endorsement
• latest date by which the national (dow) 2018-07-10
standards conflicting with the
document have to be withdrawn
This document supersedes EN 62321:2009 (partially).
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. CENELEC [and/or CEN] shall not be held responsible for identifying any or all such
patent rights.
Endorsement notice
The text of the International Standard IEC 62321-6.2015 was approved by CENELEC as a European
Standard without any modification.
2
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SIST EN 62321-6:2015
EN 62321-6:2015
Annex ZA
(normative)
Normative references to international publications
with their corresponding European publications
The following documents, in whole or in part, are normatively referenced in this document and are
indispensable for its application. For dated references, only the edition cited applies. For undated
references, the latest edition of the referenced document (including any amendments) applies.
NOTE 1 When 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 2008 Electrotechnical products - Determination EN 62321 2009
of levels of six regulated substances (lead,
mercury, cadmium, hexavalent chromium,
polybrominated biphenyls, polybrominated
diphenyl ethers)
IEC 62321-1 2013 Determination of certain substances in EN 62321-1 2013
electrotechnical products -
Part 1: Introduction and overview
IEC 62321-2 2013 Determination of certain substances in EN 62321-2 2014
electrotechnical products -
Part 2: Disassembly, disjunction and
mechanical sample preparation
3
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SIST EN 62321-6:2015
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SIST EN 62321-6:2015
IEC 62321-6
®
Edition 1.0 2015-06
INTERNATIONAL
STANDARD
NORME
INTERNATIONALE
colour
inside
Determination of certain substances in electrotechnical products –
Part 6: Polybrominated biphenyls and polybrominated diphenyl ethers in
polymers by gas chromatography–mass spectrometry (GC-MS)
Détermination de certaines substances dans les produits électrotechniques –
Partie 6: Diphényles polybromés et diphényléthers polybromés dans des
polymères par chromatographie en phase gazeuse–spectrométrie de masse
(GC-MS)
INTERNATIONAL
ELECTROTECHNICAL
COMMISSION
COMMISSION
ELECTROTECHNIQUE
INTERNATIONALE
ICS 13.020; 43.040.10 ISBN 978-2-8322-2689-6
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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SIST EN 62321-6:2015
– 2 – IEC 62321-6:2015 © IEC 2015
CONTENTS
FOREWORD . 6
INTRODUCTION . 8
1 Scope . 9
2 Normative references. 9
3 Terms, definitions and abbreviations . 10
3.1 Terms and definitions . 10
3.2 Abbreviations . 10
4 Principle . 11
5 Reagents and materials . 11
6 Apparatus . 11
7 Sampling . 12
8 Procedure . 12
8.1 General instructions for the analysis . 12
8.2 Sample preparation . 12
8.2.1 Stock solution . 12
8.2.2 Pre-extraction of the Soxhlet extractors . 13
8.2.3 Extraction . 13
8.2.4 Alternative extraction procedures for soluble polymers . 13
8.2.5 Addition of the internal standard (IS) . 14
8.3 Instrumental parameters . 14
8.4 Calibrants . 16
8.5 Calibration . 17
8.5.1 General . 17
8.5.2 PBB (1 µg/ml for each congener), PBDE (1 µg/ml for each congener)
and surrogate standard (1 µg/ml) stock solution . 18
8.5.3 Standard solutions . 18
9 Calculation of PBB and PBDE concentration . 19
9.1 General . 19
9.2 Calculation . 19
10 Precision . 21
10.1 Threshold judgement . 21
10.2 Repeatability and reproducibility . 22
11 Quality assurance and control . 22
11.1 Resolution. 22
11.2 Performance . 23
11.3 Limit of detection (LOD) or method detection limit (MDL) and limit of
quantification (LOQ) . 24
12 Test report. 25
Annex A (informative) Determination of PBB and PBDE in polymers by ion attachment
mass spectrometry (IAMS) . 26
A.1 Principle . 26
A.2 Reagents and materials . 26
A.3 Apparatus . 26
A.4 Sampling. 27
A.4.1 General . 27
A.4.2 Qualitative stage . 27
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SIST EN 62321-6:2015
IEC 62321-6:2015 © IEC 2015 – 3 –
A.4.3 Semi-quantitative stage . 27
A.5 Procedure . 27
A.5.1 General instructions for the analysis . 27
A.5.2 Sample preparation . 27
A.5.3 Instrumental parameters. 28
A.5.4 Calibrants . 29
A.5.5 Calibration . 29
A.6 Calculation of PBB and PBDE concentration . 30
A.6.1 General . 30
A.6.2 Calculation . 31
A.6.3 Judgement of ambiguous spectrum . 32
A.7 Precision . 34
A.7.1 Threshold judgement . 34
A.7.2 Repeatability and reproducibility . 34
A.8 Quality assurance and control . 35
A.8.1 Sensitivity . 35
A.8.2 Recovery . 35
A.8.3 Blank test . 36
A.8.4 Limits of detection (LOD) and limits of quantification (LOQ) . 36
A.9 Test report . 36
Annex B (informative) Diagram of an IAMS instrument . 37
Annex C (informative) Determination of PBB and PBDE in polymers by high-pressure
liquid chromatography – Ultra violet detection (HPLC-UV) . 38
C.1 Principle . 38
C.2 Reagents and materials . 38
C.3 Apparatus . 38
C.4 Sampling. 39
C.5 Procedure . 39
C.5.1 General instructions for the analysis . 39
C.5.2 Sample preparation . 39
C.5.3 Instrumental parameters. 40
C.5.4 Calibrants . 40
C.6 Calibration . 41
C.6.1 General . 41
C.6.2 Standard solutions . 41
C.7 Calculation of PBB and PBDE concentration . 42
C.7.1 General . 42
C.7.2 Calculation . 42
C.8 Precision . 43
C.8.1 Threshold judgement . 43
C.8.2 Repeatability and reproducibility . 43
C.9 Quality assurance and control . 44
C.9.1 Standards spike recovery . 44
C.9.2 Internal control samples and blanks . 44
C.9.3 Limits of detection (LOD) and limits of quantification (LOQ) . 45
C.10 Test report . 45
Annex D (informative) Examples of chromatograms at suggested conditions . 46
D.1 GC-MS method . 46
D.2 IAMS method . 48
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SIST EN 62321-6:2015
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D.3 HPLC-UV method . 52
Annex E (informative) Example applicability of the IAMS, HPLC and GC-MS test
methods . 53
Annex F (informative) Results of international interlaboratory study 4B (IIS4B) . 54
Bibliography . 57
Figure A.1 – Mass spectra of Deca BB and TBBA obtained in scan mode and profile
mode . 33
Figure A.2 – Identification of Tetra-BDE and Penta-BDE by isotope pattern recognition . 33
Figure B.1 – Diagram of an IAMS instrument . 37
Figure D.1 – Total ion chromatogram of PBDE mixture, BDE-1 to BDE-206 (5 µg/ml),
BDE-209 (50 µg/ml) . 47
Figure D.2 – Total ion chromatogram of PBB mixture (3,5 µg/ml) . 47
Figure D.3 – Total ion chromatogram of PBB and PBDE mixtures (BDE-1 to BDE-206 5
µg/ml, BDE-209 50 µg/ml, PBBs 3,5 µg/ml) . 48
Figure D.4 – Mass spectrum of each PBDE congener by IAMS-1 (TriBDE to HexaBDE) . 49
Figure D.5 – Mass spectrum of each PBDE congener by IAMS-2 (HeptaBDE to
DecaBDE) . 49
Figure D.6 – Mass spectra of technical OctaBDE(a) as mixture . 50
Figure D.7 – Temperature-programmed chromatography of each PBDE congener in the
quantitative analysis of the reference material (ERM EC-590) . 51
Figure D.8 – Chromatogram and UV spectrum of DecaBDE . 52
Figure D.9 – Chromatogram and UV spectrum of decaBB . 52
Figure D.10 – Chromatogram and UV Spectrum of OctaBDE. 52
Figure D.11 – Chromatogram and UV spectrum of octaBB . 52
Figure E.1 – Flow chart, example applicability of the IAMS, HPLC and GC-MS test
methods . 53
Table 1 – Matrix spiking solution . 13
Table 2 – Reference masses for the quantification of PBBs . 15
Table 3 – Reference masses for the quantification of PBDEs . 16
Table 4 – Example list of commercially available calibration congeners considered
suitable for this analysis . 17
Table 5 – Calibration solutions of PBBs and PBDEs . 18
Table 6 – IIS4B threshold judgement . 21
Table 7 – IIS4B repeatability and reproducibility . 22
Table 8 – Example calculation . 23
Table A.1 – Measurement condition of IAMS . 28
Table A.2 – Example list of commercially available calibrant reference materials
considered suitable for this analysis . 29
Table A.3 – Example PBDE response factor standards (i.e. BDE-WD (Wellington),
solution/ mixture of polybrominated diphenyl ether congeners(PBDE)) . 29
Table A.4 – Calibrant amounts . 30
a
Table A.5 – Response factor of each PBDE congener . 32
Table A.6 – IIS4B threshold judgement . 34
Table A.7 – IIS4B repeatability and reproducibility . 35
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SIST EN 62321-6:2015
IEC 62321-6:2015 © IEC 2015 – 5 –
Table C.1 – Example list of commercially available technical calibration mixtures
considered suitable for this analysis . 41
Table C.2 – Standard stock solution concentrations (mg/100 ml) . 41
Table C.3 – IIS4B threshold judgement . 43
Table C.4 – IIS4B Repeatability and reproducibility . 44
Table D.1 – PBB and PBDE congeners in the mixture . 46
Table F.1 – Statistical Data for GC-MS . 54
Table F.2 – Statistical data for IAMS . 55
Table F.3 – Statistical data for HPLC-UV . 56
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SIST EN 62321-6:2015
– 6 – IEC 62321-6:2015 © IEC 2015
INTERNATIONAL ELECTROTECHNICAL COMMISSION
____________
DETERMINATION OF CERTAIN SUBSTANCES
IN ELECTROTECHNICAL PRODUCTS –
Part 6: Polybrominated biphenyls and polybrominated diphenyl ethers
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
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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.
International Standard IEC 62321-6 has been prepared by IEC technical committee 111:
Environmental standardization for electrical and electronic products and systems.
The first edition of IEC 62321:2008 was a 'stand-alone' standard that included an introduction,
an overview of test methods, a mechanical sample preparation as well as various test method
clauses.
This first edition of IEC 62321-6 is a partial replacement of IEC 62321:2008, forming a
structural revision and generally replacing Annex A.
Future parts in the IEC 62321 series will gradually replace the corresponding clauses in
IEC 62321:2008. Until such time as all parts are published, however, IEC 62321:2008 remains
valid for those clauses not yet re-published as a separate part.
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SIST EN 62321-6:2015
IEC 62321-6:2015 © IEC 2015 – 7 –
The text of this standard is based on the following documents:
FDIS Report on voting
111/368/FDIS 111/379/RVD
Fu
...
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