SIST EN 62321-8:2017
(Main)Determination of certain substances in electrotechnical products - Part 8: Phthalates in polymers by gas chromatography-mass spectrometry (GC-MS), gas chromatography-mass spectrometry using a pyrolyzer/thermal desorption accessory (Py/TD-GC-MS)
Determination of certain substances in electrotechnical products - Part 8: Phthalates in polymers by gas chromatography-mass spectrometry (GC-MS), gas chromatography-mass spectrometry using a pyrolyzer/thermal desorption accessory (Py/TD-GC-MS)
IEC 62321-8:2017 specifies two normative and two informative techniques for the determination of di-isobutyl phthalate (DIBP), di-n-butyl phthalate (DBP), benzylbutyl phthalate (BBP), di-(2-ethylhexyl) phthalate (DEHP), di-n-octyl phthalate (DNOP), di-isononyl phthalate (DINP) and di-iso-decyl phthalate (DIDP) in polymers of electrotechnical products.
Verfahren zur Bestimmung von bestimmten Substanzen in Produkten der Elektrotechnik - Teil 8: Phthalate in Polymeren mittels Gaschromatographie-Massenspektrometrie (GC-MS), Gaschromatographie-Massenspektrometrie mit Nutzung des Zusatzes der Pyrolyse/thermischen Desorption (Py/TD-GC-MS)
Détermination de certaines substances dans les produits électrotechniques - Partie 8: Analyse des phtalates dans les polymères par chromatographie en phase gazeuse-spectrométrie de masse (GC-MS), chromatographie en phase gazeuse-spectrométrie de masse par pyrolyse/thermodésorption (Py/TD-GC-MS)
L'IEC 62321-8:2017 spécifie deux techniques normatives et deux techniques informatives de détermination de la présence de phtalate de diisobutyle (DIBP - di-isobutyl phthalate), de phtalate de dibutyle (DBP - di-n-butyl phthalate), de phtalate de benzyle et de butyle (BBP - benzylbutyl phthalate), de phtalate de bis(2-éthylhexyle) (DEHP - di-(2-ethylhexyl) phthalate), de phtalate de di-n-octyle (DNOP - di-n-octyl phthalate), de phtalate de di-isononyle (DINP - di-isononyl phthalate) et de phtalate de di-isodécyle (DIDP - di-iso-decyl phthalate) dans les polymères qui sont utilisés dans des produits électrotechniques.
Določevanje posameznih substanc v elektrotehniških izdelkih - 8. del: Ftalati v polimerih s plinsko kromatografijo-masno spektrometrijo (GC-MS), plinsko kromatografijo-masno spektrometrijo z uporabo pirolize/toplotne desorpcije (Py/TD-GC-MS)
Ta del standarda IEC 62321 določa dve normativni in dve informativni tehniki za določanje di-izobutil ftalata (DIBP), di-n-butil ftalata (DBP), butil benzil ftalata (BBP), di-2-etilheksil ftalata (DEHP), di-n-oktil ftalata (DNOP), di-izononil ftalata (DINP) in di-izo-decil ftalata (DIDP) v polimerih v elektrotehniških izdelkih.
V normativnem delu tega dokumenta sta opisani plinska kromatografija-masna spektrometrija (GC-MS) in plinska kromatografija-masna spektrometrija z uporabo pirolize/toplotne desorpcije (Py/TD-GC-MS).
Metoda GC-MS je glavna tehnika za kvantitativno določanje DIBP, DBP, BBP, DEHP, DNOP, DINP in DIDP v razponu 50–2000 mg/kg.
Metoda GC-MS z uporabo pirolize/toplotne desorpcije (TD) je primerna za presejalne preskuse in polkvantitativno analizo DIBP, DBP, BBP, DEHP, DNOP, DINP in DIDP v polimerih, ki se uporabljajo kot deli elektrotehniških izdelkov v razponu 100–2000 mg/kg.
Tehnika masne spektrometrije s pripenjanjem iona (IAMS) je primerna za presejalne preskuse in polkvantitativno analizo DIBP, DBP, BBP, DEHP, DNOP, DINP in DIDP. DBP in DIBP ter DEHP in DNOP niso določeni z masno spektrometrijo s pripenjanjem iona (IAMS) zaradi omejitev pri določanju vrhov in omejitev ločljivosti masnega spektra.
Tehnika LC-MS je omejena na določanje BBP, DEHP, DNOP, DINP in DIDP. DBP in DIBP nista določena z metodo LC-MS zaradi omejitev pri določanju vrhov in omejitev ločljivosti masnega spektra.
Diagram poteka, ki prikazuje, kako je mogoče uporabiti normativni metodi Py/TD-GC-MS in GC-MS ter informativne metode z masno spektrometrijo s pripenjanjem iona (IAMS) skupaj s sondo za neposredno injiciranje (DIP) in tekočinsko kromatografijo – masno spektrometrijo (LC-MS), je na voljo v dodatkih tega dokumenta.
Te štiri preskusne metode so bile ocenjene s preskusom PE (polietilenskih) in PVC (polivinilkloridnih) materialov, ki vsebujejo posamezne ftalate ~450–30.000 mg/kg, kot je prikazano v normativnem in informativnem delu tega dokumenta. Uporaba teh štirih metod, ki so opisane v tem dokumentu, za druge vrste polimerov, ftalatov ali razpone koncentracij, ki niso določene zgoraj, ni bila posebej ocenjena.
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
01-september-2017
'RORþHYDQMHSRVDPH]QLKVXEVWDQFYHOHNWURWHKQLãNLKL]GHONLKGHO )WDODWLY
SROLPHULKVSOLQVNRNURPDWRJUDILMRPDVQRVSHNWURPHWULMR *&06 SOLQVNR
NURPDWRJUDILMRPDVQRVSHNWURPHWULMR]XSRUDERSLUROL]HWRSORWQHGHVRUSFLMH
3\7'*&06
Determination of certain substances in electrotechnical products - Part 8: Phthalates in
polymers by gas chromatography-mass spectrometry (GC-MS), gas chromatography-
mass spectrometry using a pyrolyzer/thermal desorption accessory (Py/TD-GC-MS)
Ta slovenski standard je istoveten z: EN 62321-8:2017
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
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
EUROPEAN STANDARD EN 62321-8
NORME EUROPÉENNE
EUROPÄISCHE NORM
June 2017
ICS 31.020; 71.040.50
English Version
Determination of certain substances in electrotechnical products
- Part 8: Phthalates in polymers by gas chromatography-mass
spectrometry (GC-MS), gas chromatography-mass spectrometry
using a pyrolyzer/thermal desorption accessory (Py/TD-GC-MS)
(IEC 62321-8:2017)
Détermination de certaines substances dans les produits Verfahren zur Bestimmung von bestimmten Substanzen in
électrotechniques - Partie 8: Analyse des phtalates dans les Produkten der Elektrotechnik - Teil 8: Phthalate in
polymères par chromatographie en phase gazeuse- Polymeren mit Pyrolyse-Gaschromatographie-
spectrométrie de masse (GC-MS), chromatographie en Massenspektrometrie (Py-GC-MS), Ionen-Anlagerungs-
phase gazeuse-spectrométrie de masse par Massenspektrometrie (IAMS), Gaschromatographie-
pyrolyse/thermodésorption (Py/TD-GC-MS) Massenspektrometrie (GC-MS) und
(IEC 62321-8:2017) Flüssigchromatographie-Massenspektrometrie (LC-MS)
(IEC 62321-8:2017)
This European Standard was approved by CENELEC on 2017-05-02. 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, 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: Avenue Marnix 17, B-1000 Brussels
© 2017 CENELEC All rights of exploitation in any form and by any means reserved worldwide for CENELEC Members.
Ref. No. EN 62321-8:2017 E
European foreword
The text of document 111/416/CDV, future edition 1 of IEC 62321-8, 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 62321-8:2017.
The following dates are fixed:
(dop) 2018-02-02
• 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) 2020-05-02
standards conflicting with the
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.
Endorsement notice
The text of the International Standard IEC 62321-8.2017 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:
ISO 3696 NOTE Harmonized as EN ISO 3696.
ISO/IEC 17025 NOTE Harmonized as EN ISO/IEC 17025.
IEC 62321-2:2013 NOTE Harmonized as EN 62321-2:2014.
IEC 62321-6:2015 NOTE Harmonized as EN62321-6:2016
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 62321-1 2013 Determination of certain substances in EN 62321-1 2013
electrotechnical products -- Part 1:
Introduction and overview
IEC 62321-8 ®
Edition 1.0 2017-03
INTERNATIONAL
STANDARD
NORME
INTERNATIONALE
Determination of certain substances in electrotechnical products –
Part 8: Phthalates in polymers by gas chromatography-mass spectrometry
(GC-MS), gas chromatography-mass spectrometry using a pyrolyzer/thermal
desorption accessory (Py/TD-GC-MS)
Détermination de certaines substances dans les produits électrotechniques –
Partie 8: Analyse des phtalates dans les polymères par chromatographie en
phase gazeuse-spectrométrie de masse (GC-MS), chromatographie en phase
gazeuse-spectrométrie de masse par pyrolyse/thermodésorption (Py/TD-GC-MS)
INTERNATIONAL
ELECTROTECHNICAL
COMMISSION
COMMISSION
ELECTROTECHNIQUE
INTERNATIONALE
ICS 31.020; 71.040.50 ISBN 978-2-8322-4144-8
– 2 – IEC 62321-8:2017 © IEC 2017
CONTENTS
FOREWORD . 6
INTRODUCTION . 8
1 Scope . 9
2 Normative references . 9
3 Terms, definitions and abbreviated terms . 10
3.1 Terms and definitions . 10
3.2 Abbreviated terms . 10
4 Principle . 11
5 Reagents and materials . 11
5.1 GC-MS method . 11
5.2 Py/TD-GC-MS method . 12
6 Apparatus . 12
6.1 GC-MS method . 12
6.2 Py/TD-GC-MS method . 13
7 Sampling . 14
7.1 General . 14
7.2 GC-MS method . 14
7.3 Py/TD-GC-MS method . 14
8 Procedure . 14
8.1 General instructions for the analysis . 14
8.1.1 Overview . 14
8.1.2 GC-MS method . 14
8.1.3 Py/TD-GC-MS method . 14
8.2 Sample preparation . 15
8.2.1 GC-MS method . 15
8.2.2 Py/TD-GC-MS method . 16
8.3 Instrumental parameters . 16
8.3.1 GC-MS method . 16
8.3.2 Py/TD-GC-MS method . 18
8.4 Calibrants . 18
8.5 Calibration . 19
8.5.1 GC-MS method . 19
8.5.2 Py/TD-GC-MS method . 20
9 Calculation of phthalate concentration . 21
9.1 GC-MS method . 21
9.2 Py/TD-GC-MS method . 22
10 Precision . 23
10.1 GC-MS method . 23
10.1.1 Threshold judgement . 23
10.1.2 Repeatability and reproducibility . 24
10.2 Py/TD-GC-MS method . 25
10.2.1 Screening judgement . 25
10.2.2 Repeatability and reproducibility . 26
11 Quality assurance and control . 27
11.1 General . 27
IEC 62321-8:2017 © IEC 2017 – 3 –
11.2 GC-MS method . 27
11.2.1 Performance . 27
11.2.2 Limit of detection (LOD) or method detection limit (MDL) and limit of
quantification (LOQ) . 28
11.3 Py/TD-GC-MS method . 29
11.3.1 Sensitivity . 29
11.3.2 Blank test . 29
11.3.3 Limit of detection (LOD) or method detection limit (MDL) and limit of
quantification (LOQ) . 29
12 Test report . 30
Annex A (informative) Determination of phthalates in polymers by ion attachment
mass spectrometry (IAMS) . 31
A.1 Principle . 31
A.2 Reagents and materials . 31
A.3 Apparatus . 31
A.4 Sampling. 32
A.5 Procedure . 32
A.5.1 General instructions for the analysis . 32
A.5.2 Sample preparation . 32
A.5.3 Instrumental parameters . 33
A.5.4 Calibrants . 34
A.5.5 Calibration . 34
A.6 Calculation of phthalates concentration . 35
A.7 Quality assurance and control . 35
A.7.1 General . 35
A.7.2 Sensitivity . 35
A.7.3 Recovery . 35
A.7.4 Blank test . 36
A.7.5 Limit of detection (LOD) or method detection limit (MDL) and limit of
quantification (LOQ) . 37
A.8 Test report . 37
Annex B (informative) Determination of phthalates in polymers by liquid
chromatography-mass spectrometry(LC-MS) . 38
B.1 Principle . 38
B.2 Reagents and materials . 38
B.3 Apparatus . 38
B.4 Sampling. 39
B.5 Procedure . 39
B.5.1 General instructions for the analysis . 39
B.5.2 Sample preparation . 39
B.5.3 Instrumental parameters . 40
B.5.4 Calibrants . 42
B.5.5 Calibration . 42
B.6 Calculation of phthalates concentration . 43
B.7 Quality assurance and control . 44
B.7.1 General . 44
B.7.2 Performance . 44
B.7.3 Limit of detection (LOD) or method detection limit (MDL) and limit of
quantification (LOQ) . 44
B.8 Test report . 45
– 4 – IEC 62321-8:2017 © IEC 2017
Annex C (informative) Examples of chromatograms at suggested conditions . 46
C.1 GC-MS method . 46
C.2 Py/TD-GC-MS method . 47
C.3 LC-MS method . 47
C.4 IAMS method . 48
Annex D (informative) Verification of the EGA thermal desorption zone . 51
Annex E (informative) Example of IAMS and Py/TD-GC-MS instruments . 52
Annex F (informative) Example of false positive detection of phthalates . 54
Annex G (informative) Examples of sample preparation for quantitative analysis of
phthalates by GC-MS . 55
G.1 General . 55
G.2 Soxhlet extraction of phthalates using proper organic solvents . 55
Annex H (informative) Extraction of phthalates by dissolution in THF using sonication
and precipitation of polymer matrix . 58
Annex I (informative) Commercially available reference materials considered suitable
for GC-MS and Py/TD-GC-MS. 60
I.1 GC-MS . 60
I.2 Py/TD-GC-MS . 60
Annex J (informative) Commercially available capillary columns considered suitable
for GC-MS and Py-GC-MS . 62
Annex K (informative) Labware cleaning procedure for phthalate testing . 63
K.1 With the use of a furnace (non-volumetric glassware only) . 63
K.2 Without the use of a furnace (glassware and plastic-ware) . 63
K.3 Estimation of cleanness of the inner areas of volumetric glassware . 64
Annex L (informative) Results of international inter-laboratory study 5 . 65
Annex M (informative) Sample analysis sequence . 70
M.1 GC-MS . 70
Annex N (informative) Flow chart . 71
Bibliography . 72
Figure C.1 – Total ion current chromatogram of each phthalate (10 µg/ml, 1 µl,
splitless) . 46
Figure C.2 – Extracted ion chromatogram of DINP (10 µg/ml, 1 µl, splitless) . 46
Figure C.3 – Extracted ion chromatogram of DIDP (10 µg/ml, 1 µl, splitless) . 47
Figure C.4 – Total ion current chromatogram of 100 µg/ml of phthalate mixture by
Py/TD-GC-MS . 47
Figure C.5 – Total ion current chromatogram of 5 µg/ml of phthalate mixture by LC-MS . 48
Figure C.6 – Mass spectrum of each phthalate by IAMS . 49
Figure C.7 – Total ion current chromatogram of each absolute amount (0,08 µg) of
phthalate mixture by IAMS . 50
Figure C.8 – Total ion current chromatogram of approximately 0,3 mg of PVC which
contains 300 mg/kg of each phthalate mixture by IAMS (Absolute amount: 0,09 µg) . 50
Figure D.1 – Example of EGA thermogram of a PVC sample containing phthalates . 51
Figure E.1 – Example of IAMS instrument . 52
Figure E.2 – Example of Py/TD-GC-MS instrument . 53
Figure F.1 – Typical laboratory wares made of plastic materials that may cause
phthalate contamination . 54
IEC 62321-8:2017 © IEC 2017 – 5 –
Figure F.2 – Example of a chromatogram of a blank solvent (THF) in a plastic bottle
showing DEHP contamination. . 54
Figure G.1 – Recovery ratios of Di-(2-ethylhexyl) phthalate using Soxhlet extraction
with different organic solvents . 57
Figure G.2 – Comparison of recovery ratios of phthalates using different extracting
conditions . 57
Figure I.1 – Sample preparation of reference materials . 61
Figure N.1 – Flow chart for screening step and quantitative step . 71
Table 1 – Measurement condition of GC-MS . 17
Table 2 – Reference masses for the quantification of each phthalate . 17
Table 3 – Measurement condition of Py/TD-GC-MS . 18
Table 4 – Calibration standard solution of phthalates . 19
Table 5 – IIS5 Threshold judgement. 23
Table 6 – IIS5 Repeatability and reproducibility . 24
Table 7 – IIS5 screening and threshold judgement . 25
Table 8 – IIS5 Repeatability and reproducibility . 26
Table A.1 – Measurement condition of IAMS . 34
Table A.2 – Certified value of constituent phthalates in KRISS CRM 113-03-006 . 36
Table B.1 – Measurement condition of LC-MS . 42
Table B.2 – Standard stock solution concentrations . 43
Table G.1 – Recovery ratios of phthalates according to different Soxhlet extraction
times (extracting solvent: n-hexane) . 56
Table H.1 – Comparison of the efficiency of the sample preparation method of
dissolution in THF using sonication and precipitation of polymeric matrix with that of
Soxhlet extraction for soluble sample . 58
Table H.2 – Comparison of the efficiency of the sample preparation method of
dissolution in THF using sonication and precipitation of polymeric matrix with that of
Soxhlet extraction for insoluble samples . 59
Table I.1 – Example list of commercially available reference solutions considered
suitable for GC-MS . 60
Table I.2 – Example list of commercially available reference materials considered
suitable for Py/TD-GC-MS. 61
Table J.1 – Example list of commercially available capillary columns considered
suitable for GC-MS and Py-GC-MS analysis . 62
Table L.1 – Statistical data for Py/TD-GC-MS . 65
Table L.2 – Statistical data for GC-MS . 67
Table L.3 – Statistical data for IAMS . 68
Table L.4 – Statistical Data For LC-MS . 69
Table M.1 – Sample analysis sequence for GC-MS analysis . 70
Table M.2 – Sample analysis sequence for Py/TD-GC-MS analysis . 70
– 6 – IEC 62321-8:2017 © IEC 2017
INTERNATIONAL ELECTROTECHNICAL COMMISSION
____________
DETERMINATION OF CERTAIN SUBSTANCES
IN ELECTROTECHNICAL PRODUCTS –
Part 8: Phthalates in polymers by gas chromatography-mass spectrometry
(GC-MS), gas chromatography-mass spectrometry using
a pyrolyzer/thermal desorption accessory (Py/TD-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.
International Standard IEC 62321-8 has been prepared by IEC technical committee 111:
Environmental standardization for electrical and electronic products and systems.
The text of this International Standard is based on the following documents:
CDV Report on voting
111/416/CDV 111/430/RVC
Full information on the voting for the approval of this International Standard can be found in
the report on voting indicated in the above table.
This document has been drafted in accordance with the ISO/IEC Directives, Part 2.
IEC 62321-8:2017 © IEC 2017 – 7 –
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 publication will remain unchanged until
the stability date indicated on the IEC website under "http://webstore.iec.ch" in the data
related to the specific publication. At this date, the publication will be
• reconfirmed,
• withdrawn,
• replaced by a revised edition, or
• amended.
– 8 – IEC 62321-8:2017 © IEC 2017
INTRODUCTION
The widespread use of electrotechnical products has drawn increased attention to their impact
on the environment. In many countries all over the world this has resulted in the adaptation of
regulations affecting wastes, substances and energy use of electrotechnical products.
The use of certain substances (e.g. lead (Pb), cadmium (Cd), polybrominated diphenyl ethers
(PBDEs) and specific phthalates) in electrotechnical products is a source of concern in
current and proposed regional legislation.
The purpose of the IEC 62321 series 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.
This first edition of IEC 62321-8 introduces a new part in the IEC 62321 series.
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.
IEC 62321-8:2017 © IEC 2017 – 9 –
DETERMINATION OF CERTAIN SUBSTANCES
IN ELECTROTECHNICAL PRODUCTS –
Part 8: Phthalates in polymers by gas chromatography-mass spectrometry
(GC-MS), gas chromatography-mass spectrometry using
a pyrolyzer/thermal desorption accessory (Py/TD-GC-MS)
1 Scope
This part of IEC 62321 specifies two normative and two informative techniques for the
determination of di-isobutyl phthalate (DIBP), di-n-butyl phthalate (DBP), benzylbutyl
phthalate (BBP), di-(2-ethylhexyl) phthalate (DEHP), di-n-octyl phthalate (DNOP), di-isononyl
phthalate (DINP) and di-iso-decyl phthalate (DIDP) in polymers of electrotechnical products.
Gas chromatography-mass spectrometry (GC-MS) and gas chromatography-mass
spectrometry (Py/TD-GC-MS) techniques are described in the normative part of this document.
The GC-MS method is considered the referee technique for the quantitative determination of
DIBP, DBP, BBP, DEHP, DNOP, DINP and DIDP in the range of 50 mg/kg to 2 000 mg/kg.
The GC-MS coupled with a pyrolyzer/thermal desorption (TD) accessory is suitable for
screening and semi-quantitative analysis of DIBP, DBP, BBP, DEHP, DNOP, DINP, and DIDP
in polymers that are used as parts of the electrotechnical products in the range of 100 mg/kg
to 2 000 mg/kg.
The IAMS technique is suitable for screening and semi-quantitative analysis of DIBP, DBP,
BBP, DEHP, DNOP, DINP, and DIDP. Determination of DBP and DIBP, DEHP and DNOP by
IAMS has not been established due to peak and mass spectral resolution limitations.
The LC-MS technique is limited to the determination of of BBP, DEHP, DNOP, DINP, and
DIDP. Determination of DBP and DIBP by LC-MS has not been established due to peak and
mass spectral resolution limitations.
A flow chart depicting how the normative Py/TD-GC-MS and GC-MS methods and informative
methods using ion attachment mass spectrometry (IAMS) coupled with direct injection probe
(DIP) and liquid chromatography-mass spectrometry (LC-MS) can be used are provided in
annexes of this document.
These four test methods have been evaluated by the test of PE (polyethylene) and PVC
(polyvinyl chloride) materials containing individual phthalates between ~450 mg/kg to
30 000 mg/kg as depicted in the normative and informative parts of this document. The use of
the four methods described in this document for other polymer types, phthalate compounds or
concentration ranges other than those specified above has not been specifically evaluated.
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
– 10 – IEC 62321-8:2017 © IEC 2017
3 Terms, definitions and abbreviated terms
3.1 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
ISO and IEC maintain terminological databases for use in standardization at the following
addresses:
• IEC Electropedia: available at http://www.electropedia.org/
• ISO Online browsing platform: available at http://www.iso.org/obp
3.1.1
screening
analytical procedure to determine the presence or absence of substances in the
representative part or section of a product, relative to the value or values chosen as the
criterion for presence, absence or further testing
Note 1 to entry: If the screening method produces values that are not conclusive, then additional analysis or other
follow-up actions may be necessary to make a final presence/absence decision.
[SOURCE: IEC 62321-1:2013, 3.1.10]
3.1.2
semi-quantitative
level of accuracy in a measurement amount where the relative uncertainty of the result is
typically 30 % or better at a defined level of confidence of 68 %
[SOURCE: IEC 62321-6:2015, 3.1.1]
3.1.3
calibrant
calibration standard
substance in solid or liquid form with known and stable concentration(s) of the analyte(s) of
interest used to establish instrument response (calibration curve) with respect to analyte(s)
concentration(s)
3.2 Abbreviated terms
ACN Acetonitrile
BBP Benzyl butyl phthalate
BSA N,O-bis(trimethylsilyl)acetamide
BSTFA N,O-bis(trimethylsilyl)trifluoroacetamide
CRM Certified reference material
DBP Di-n-butyl phthalate
DEHP Di-(2-ethylhexyl) phthalate
DIBP Di-isobutyl phthalate
DIDP Di-iso-decyl phthalate
DINP Di-isononyl phthalate
DIP Direct injection probe
DNOP Di-n-octyl phthalate
EGA Evolved gas analysis
EI Electron ionization
GC-MS Gas chromatography – mass spectrometry
IEC 62321-8:2017 © IEC 2017 – 11 –
IAMS Ion attachment mass spectrometry
IS Internal standard
LC-MS Liquid chromatography – mass spectrometry
LOD Limit of detection
LOQ Limit of quantification
MDL Method detection limit
PVC Polyvinyl chloride
Py Pyrolyzer
QC Quality control
SIM Selected ion monitoring
TD Thermal desorption
THF Tetrahydrofuran
4 Principle
In the GC-MS method, DIBP, DBP, BBP, DEHP, DNOP, DINP and DIDP are quantitatively
determined using ultrasonic dissolution and precipitation of the sample matrix or Soxhlet
extraction from polymers with separation by gas chromatography separation and mass
spectrometry detection.
The Py/TD-GC-MS uses gas chromatography-mass spectrometry coupled with a
pyrolyzer/thermal desorption accessory to screen for the presence of DIBP, DBP, BBP, DEHP,
DNOP, DINP and DIDP in polymeric materials. The polymer sample is directly introduced into
the pyrolyzer/thermal desorption accessory to thermally extract phthalates from the polymer
using a specified heating programme. Thermally desorbed phthalates are then transferred to
the gas chromatograph, separated by a capillary column and detected by a mass
spectrometer. The respective phthalates are identified based on the retention times，m/z
(quantitative and confirmation ions) and ion ratios. A SIM mode is used to improve the limits
of detection. A one-point calibration is applied for screening and semi-quanititative analysis of
phthalates in the sample.
NOTE A full scan run using a total ion current (“full scan”) MS method for each sample can be used in order to
check for the existence of negative matrix interference from other additives in the polymer. Negative matrix
interference causes ion suppression which provides lower concentration results. Scan/SIM measurement
(simultaneous measurements) is also applicable.
5 Reagents and materials
5.1 GC-MS method
All chemicals shall be tested for contamination and blank values prior to application, as
follows:
a) ACN (HPLC grade);
b) THF (GC grade or higher);
c) n-Hexane (GC grade or higher);
d) helium (purity of greater than a volume fraction of 99,999 %);
e) calibrants: refer to 8.4;
f) surrogate and internal standards:
– surrogate standard used to monitor analytes recovery according to 8.2.1.1, 8.2.1.3,
and 8.5.1.1, for example dibutyl phthalate-3,4,5,6-d or di-(2-ethylhexyl)phthalate-
3,4,5,6-d standard;
– 12 – IEC 62321-8:2017 © IEC 2017
– internal standard used to correct for injection errors, according to 8.2.1.1 and 8.5.1.2,
for example anthracene-d or benzyl benzoate.
The standards are acceptable when using a quadruple-type mass spectrometer. A high-
resolution mass spectrometer will require the use of other suitable standard substances
having a mass and elution time similar to that of the analyte. Deuterium substituted DBP and
DEHP are recommended for specified phthalates.
NOTE Commercially available surrogates and internal standards are listed in Annex I.
5.2 Py/TD-GC-MS method
All reagent chemicals shall be tested for contamination and blank values prior to application
as follows:
a) helium (purity of greater than a volume fraction of 99,999 %);
b) reference polymer materials:
one contains approximately 100 mg/kg and the other 1 000 mg/kg of phthalates;
c) blank polymer material (no phthalates shall be included).
The following reagent chemicals, when used for preparing the polymer sample, shall be
similarly tested as the above.
d) n-hexane for preparing the phthalate standard solution (GC grade or higher);
e) THF, or a solvent suitable for preparing the polymer sample (GC grade or higher).
NOTE Commercially available reference materials are listed in Annex I.
6 Apparatus
6.1 GC-MS method
The following items shall be used for the analysis:
a) analytical balance capable of measuring accurately to 0,000 1 g;
b) cryogenic grinding/milling with liquid N cooling;
c) 1 ml, 5 ml, 10 ml, 100 ml volumetric flasks;
d) Soxhlet extractors:
– 30 ml Soxhlet extractors;
– 250 ml round-bottomed flask;
– ground-in stopper NS 29/32;
– Dimroth condenser NS 29/32;
– boiling stones (e.g. glass pearls or Raschig rings);
e) extraction thimble (cellulose 30 ml, ID 22 mm, height 80 mm);
f) glass wool (for extraction thimble);
g) ultrasonic bath;
h) deactivated injector liner (for GC-MS);
i) heating jackets;
j) funnels;
k) aluminium foil;
l) cork rings;
m) 0,45 µm PTFE filter;
n) microlitre syringe or automatic pipettes;
IEC 62321-8:2017 © IEC 2017 – 13 –
o) rotary evaporator with vacuum capability;
p) Pasteur pipettes;
q) 1,5 ml sample vials and a screw cap with polytetrafluoroethylene (PTFE) gasket or,
depending on the analytical system,
...
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