SIST EN 62321-5:2014
(Main)Determination of certain substances in electrotechnical products - Part 5: Determination of cadmium, lead and chromium in polymers and electronics and cadmium and lead in metals by AAS, AFS, ICP-OES and ICP-MS
Determination of certain substances in electrotechnical products - Part 5: Determination of cadmium, lead and chromium in polymers and electronics and cadmium and lead in metals by AAS, AFS, ICP-OES and ICP-MS
EN-IEC 62321-5 describes the test methods for lead, cadmium and chromium in polymers, metals and electronics by AAS, AFS, ICP-OES and ICP-MS. This standard specifies the determination of the levels of cadmium (Cd), lead (Pb) and chromium (Cr) in electrotechnical products. It covers three types of matrices: polymers/polymeric workpieces, metals and alloys and electronics. This standard refers to the sample as the object to be processed and measured. What the sample is or how to get to the sample is defined by the entity carrying out the tests. Further guidance on obtaining representative samples from finished electronic products to be tested for levels of regulated substances may be found in IEC 62321-2. It is noted that the selection and/or determination of the sample may affect the interpretation of the test results. This standard describes the use of four methods, namely AAS (atomic absorption spectrometry), AFS (atomic fluorescence spectrometry), ICP-OES (inductively coupled plasma optical emission spectrometry), and ICP-MS (inductively coupled plasma mass spectrometry) as well as several procedures for preparing the sample solution from which the most appropriate method of analysis can be selected by experts. As the hexavalent-Cr analysis is sometimes difficult to determine in polymers and electronics, this standard introduces the screening methods for chrome in polymers and electronics except from AFS. Chromium analysis provides information about the existence of hexavalent- Cr in materials. However, elemental analyses cannot selectively detect hexavalent-Cr; it determines the amount of Cr in all oxidation states in the samples. If Cr amounts exceed the hexavalent-Cr limit, testing for hexavalent-Cr should be performed. The test procedures described in this standard are intended to provide the highest level of accuracy and precision for concentrations of Pb, Cd and Cr that range, in the case of ICPOES and AAS, from 10 mg/kg for Pb, Cd and Cr, in the case of ICP-MS, from 0,1 mg/kg for Pb and Cd in the case of AFS, the range is from 10 mg/kg for Pb and 1.5 mg/kg for Cd. The procedures are not limited for higher concentrations. This standard does not apply to materials containing polyfluorinated polymers because of their stability. If sulfuric acid is used in the analytical procedure, there is a risk of losing Pb, thus resulting in erroneously low values for this analyte. In addition, sulfuric acid and hydrofluoric acid are not suitable for determining Cd by AFS, because it disturbs the reduction of Cd. Limitations and risks occur due to the solution step of the sample, e.g. precipitation of the target or other elements may occur, in which case the residues have to be checked separately or dissolved by another method and then combined with the test sample solution.
Verfahren zur Bestimmung von bestimmten Substanzen in Produkten der Elektrotechnik - Teil 5: Bestimmung von Cadmium, Blei und Gesamtchrom in Polymeren und Elektronik und von Cadmium und Blei in Metallen mit AAS, AFS, ICP-OES und ICP-MS
Détermination de certaines substances dans les produits électrotechniques - Partie 5: Détermination du cadmium, du plomb et du chrome dans les polymères et les produits électroniques, et du cadmium et du plomb dans les métaux par AAS, AFS, ICP-OES et ICP-MS
La CEI 62321-5:2013 décrit les quatre méthodes d'essai pour le plomb, le cadmium et le chrome dans les polymères, les métaux et les produits électroniques, à savoir l'AAS (spectrométrie d'absorption atomique), l'AFS (spectrométrie de fluorescence atomique), l'ICP-OES (spectrométrie d'émission optique couplée à un plasma induit) et l'ICP-MS (spectrométrie de masse couplée à un plasma induit), ainsi que plusieurs procédures de préparation de la solution d'échantillon à partir desquelles les experts peuvent choisir la méthode d'analyse la plus appropriée.
Določevanje posameznih snovi v elektrotehničnih izdelkih - 5. del: Določevanje kadmija, svinca in kroma v polimerih in elektronskih elementih ter kadmija in svinca v kovinah z AAS, AFS, ICP-OES in ICP-MS (IEC 62321-5:2013)
Standard EN-IEC 62321-5 opisuje preskusne metode za določevanje svinca, kadmija in kroma v polimerih in elektronskih elementih z atomsko absorpcijsko spektrometrijo (AAS), atomsko fluorescenčno spektrometrijo (AFS), optično emisijsko spektrometrijo z induktivno sklopljeno plazmo (ICP-OES) in masno spektrometrijo z induktivno sklopljeno plazmo (ICP-MS). Ta standard navaja določanje kadmija (Cd), svinca (Pb) in kroma (Cr) v elektronskih elementih. Zajema tri vrste matric: polimere/polimerne obdelovance, kovine in zlitine ter elektroniko. Ta standard se nanaša na vzorec kot predmet, ki se obdela in meri. Kaj ta vzorec je ali kako ga pridobiti, določa subjekt, ki izvaja preskuse. Dodatna navodila o pridobivanju reprezentativnih vzorcev iz končnih elektronskih izdelkov za testiranje ravni reguliranih snovi je mogoče najti v standardu IEC 62321-2. Opozoriti je treba, da lahko izbira in/ali določanje vzorca vpliva na razlago rezultatov preskusa. Ta standard opisuje uporabo štirih metod, in sicer AAS (atomska absorpcijska spektrometrija), AFS (atomska fluorescentna spektrometrija), ICP-OES (optična emisijska spektrometrija z induktivno sklopljeno plazmo) in ICP-MS (masna spektrometrija z induktivno sklopljeno plazmo), kot tudi več postopkov za pripravo vzorčne raztopine, s pomočjo katere lahko strokovnjaki izberejo najbolj primerno metodo analize. Ker je z analizo šestvalentnega kroma tega včasih težko določiti v polimerih in elektroniki, ta standard uvaja presejalne metode za krom v polimerih in elektroniki, z izjemo atomske absorpcijske spektrometrije. Analiza kroma zagotavlja informacije o obstoju šestvalentnega kroma v materialih. Vendar z analizo elementov ni mogoče selektivno zaznati šestvalentnega kroma. Z njo se določi vsebnost kroma v vseh oksidacijskih stanjih v vzorcih. Če vsebnost kroma preseže mejo za šestvalentni krom, je treba testirati vsebnost šestvalentnega kroma. Preskusni postopki, opisani v tem standardu, so namenjeni zagotavljanju najvišje stopnje točnosti in natančnosti za vsebnosti svinca, kadmija in kroma v tem območju; pri optični emisijski spektrometriji z induktivno sklopljeno plazmo in atomski absorpcijski spektrometriji od 10 mg/kg za svinec, kadmij in krom, pri masni spektrometriji z induktivno sklopljeno plazmo od 0,1 mg/kg za svinec in kadmij, pri atomski fluorescentni spektrometriji pa od 10 mg/kg svinec in 1,5 mg/kg za kadmij. Postopki se lahko uporabljajo tudi za višje koncentracije. Zaradi njihove stabilnosti ta standard ne velja za materiale, ki vsebujejo polifluorirane polimere. Če je v analitskem postopku uporabljena žveplova kislina, obstaja tveganje izgube svinca, kar povzroči nepravilne nizke vrednosti tega analita. Ob tem žveplova in fluorovodikova kislina nista primerni za določanje kadmija z atomsko absorpcijsko spektrometrijo, saj ovirata zmanjšanje vsebnosti kadmija. Omejitve in tveganja se pojavijo zaradi koraka z raztopino vzorca, pride lahko npr. do obarjanja ciljnega ali drugih elementov, pri čemer je treba ostanke preveriti posebej ali jih raztopiti na drug način in jih nato združiti z vzorčno raztopino.
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
SIST EN 62321-5:2014
01-junij-2014
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SIST EN 62321:2009
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Determination of certain substances in electrotechnical products - Part 5: Determination
of cadmium, lead and chromium in polymers and electronics and cadmium and lead in
metals by AAS, AFS, ICP-OES and ICP-MS
Verfahren zur Bestimmung von bestimmten Substanzen in Produkten der Elektrotechnik
- Teil 5: Bestimmung von Cadmium, Blei und Gesamtchrom in Polymeren und Elektronik
und von Cadmium und Blei in Metallen mit AAS, AFS, ICP-OES und ICP-MS
Détermination de certaines substances dans les produits électrotechniques - Partie 5:
Détermination du cadmium, du plomb et du chrome dans les polymères et les produits
électroniques, et du cadmium et du plomb dans les métaux par AAS, AFS, ICP-OES et
ICP-MS
Ta slovenski standard je istoveten z: EN 62321-5:2014
ICS:
29.020 Elektrotehnika na splošno Electrical engineering in
general
31.020 Elektronske komponente na Electronic components in
splošno general
SIST EN 62321-5:2014 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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SIST EN 62321-5:2014
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SIST EN 62321-5:2014
EUROPEAN STANDARD
EN 62321-5
NORME EUROPÉENNE
April 2014
EUROPÄISCHE NORM
ICS 13.020; 43.040.10 Supersedes EN 62321:2009 (partially)
English version
Determination of certain substances in electrotechnical products -
Part 5: Cadmium, lead and chromium in polymers and electronics and
cadmium and lead in metals by AAS, AFS, ICP-OES and ICP-MS
(IEC 62321-5:2013)
Détermination de certaines substances Verfahren zur Bestimmung von
dans les produits électrotechniques - bestimmten Substanzen in Produkten der
Partie 5: Du cadmium, du plomb et du Elektrotechnik -
chrome dans les polymères et les produits Teil 5: Cadmium, Blei und Chrom in
électroniques, du cadmium et du plomb Polymeren und Elektronik und Cadmium
dans les métaux par AAS, AFS, ICP-OES und Blei in Metallen mit AAS, AFS, ICP-
et ICP-MS OES und ICP-MS
(CEI 62321-5:2013) (IEC 62321-5:2013)
This European Standard was approved by CENELEC on 2013-11-15. 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.
CENELEC
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
© 2014 CENELEC - All rights of exploitation in any form and by any means reserved worldwide for CENELEC members.
Ref. No. EN 62321-5:2014 E
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SIST EN 62321-5:2014
EN 62321-5:2014 - 2 -
Foreword
The text of document 111/297/FDIS, future edition 1 of IEC 62321-5, 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 62321-5:2014.
The following dates are fixed:
(dop) 2014-10-25
• latest date by which the document has
to be implemented at national level by
publication of an identical national
standard or by endorsement
(dow) 2016-11-15
• latest date by which the national
standards conflicting with the
document have to be withdrawn
EN 62321-5:2014 is a partial replacement of EN 62321:2009, forming a structural revision and generally
replacing Clauses 8 to 10, as well as Annexes F, G and H.
Future parts in the EN 62321 series will gradually replace the corresponding clauses from EN
62321:2009. Until such time as all parts are published, however, EN 62321:2009 remains valid for those
clauses not yet re-published as a separate part.
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 62321-5:2013 was approved by CENELEC as a European
Standard without any modification.
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SIST EN 62321-5:2014
- 3 - EN 62321-5:2014
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 When an international publication has been modified by common modifications, indicated by (mod), the relevant EN/HD
applies.
Publication Year Title EN/HD Year
IEC 62321-1 - Determination of certain substances in EN 62321-1 -
electrotechnical products -
Part 1: Introduction and overview
IEC 62321-2 - Determination of certain substances in EN 62321-2 -
electrotechnical products -
Part 2: Disassembly, disjunction and
mechanical sample preparation
IEC 62321-3-1 - Determination of certain substances in EN 62321-3-1 -
electrotechnical products -
Part 3-1: Screening electrotechnical products
for lead, mercury, cadmium, total chromium
and total bromine using X-ray Fluorescence
Spectrometry
ISO 3696 - Water for analytical laboratory use - EN ISO 3696 -
Specification and test methods
ISO 5961 - Water quality - Determination of cadmium by EN ISO 5961 -
atomic absorption spectrometry
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SIST EN 62321-5:2014
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SIST EN 62321-5:2014
IEC 62321-5
®
Edition 1.0 2013-06
INTERNATIONAL
STANDARD
NORME
INTERNATIONALE
colour
inside
Determination of certain substances in electrotechnical products –
Part 5: Cadmium, lead and chromium in polymers and electronics and cadmium
and lead in metals by AAS, AFS, ICP-OES and ICP-MS
Détermination de certaines substances dans les produits électrotechniques –
Partie 5: Du cadmium, du plomb et du chrome dans les polymères et les
produits électroniques, du cadmium et du plomb dans les métaux par AAS,
AFS, ICP-OES et ICP-MS
INTERNATIONAL
ELECTROTECHNICAL
COMMISSION
COMMISSION
ELECTROTECHNIQUE
PRICE CODE
INTERNATIONALE
CODE PRIX W
ICS 13.020; 43.040.10 ISBN 978-2-83220-842-7
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 62321-5:2014
– 2 – 62321-5 © IEC:2013
CONTENTS
FOREWORD . 4
INTRODUCTION . 6
1 Scope . 7
2 Normative references . 8
3 Terms, definitions and abbreviations . 8
3.1 Terms and definitions . 8
3.2 Abbreviations . 9
4 Reagents . 9
4.1 General . 9
4.2 Reagents . 9
5 Apparatus . 11
5.1 General . 11
5.2 Apparatus . 12
6 Sampling . 13
6.1 General . 13
6.2 Test portion . 13
6.2.1 Polymers . 13
6.2.2 Metals . 13
6.2.3 Electronics . 13
7 Procedure. 13
7.1 Polymers . 13
7.1.1 General . 13
7.1.2 Dry ashing method . 14
7.1.3 Acid digestion method . 15
7.1.4 Microwave digestion . 15
7.2 Metals . 16
7.2.1 General . 16
7.2.2 Common methods of sample digestion. 17
7.2.3 Samples containing Zr, Hf, Ti, Ta, Nb or W . 17
7.2.4 Samples containing Sn . 17
7.3 Electronics . 18
7.3.1 General . 18
7.3.2 Digestion with aqua regia . 18
7.3.3 Microwave digestion . 19
7.4 Preparation of reagent blank solution . 20
8 Calibration . 20
8.1 General . 20
8.2 Preparation of the calibration solution . 20
8.3 Development of the calibration curve . 20
8.4 Measurement of the sample . 21
9 Calculation . 22
10 Precision . 22
11 Quality control . 24
11.1 General . 24
11.2 Limits of detection (LOD) and limits of quantification (LOQ) . 25
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SIST EN 62321-5:2014
62321-5 © IEC:2013 – 3 –
Annex A (informative) Practical application of determination of Cd , Pb and Cr in polymers
and electronics and Cd and Pb in metals by AAS, AFS, ICP-OES and ICP-MS . 27
Annex B (informative) Results of international interlaboratory study nos. 2 (IIS2) and
4A (IIS 4A) . 33
Bibliography . 36
Figure A.1 – Background correction . 31
Table 1 – Repeatability and reproducibility . 22
Table 2 – Acceptance criteria of items for the quality control . 24
Table 3 – Method detection limit = t × s . 26
n–1
Table A.1 – Spectral interferences for the wavelengths of Cd and Pb . 28
Table A.2 – Spectral interferences for the wavelengths of Cr . 29
Table A.3 – Examples of mass/charge (m/z) ratios . 30
Table A.4 – Examples of wavelengths for AAS . 30
Table A.5 – Examples of wavelengths for AFS . 31
Table A.6 – Program for microwave digestion of samples . 32
Table B.1 – Statistical data for AAS . 33
Table B.2 – Statistical data for AFS . 33
Table B.3 – Statistical data for ICP-OES . 34
Table B.4 – Statistical data for ICP-MS . 35
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SIST EN 62321-5:2014
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INTERNATIONAL ELECTROTECHNICAL COMMISSION
____________
DETERMINATION OF CERTAIN SUBSTANCES
IN ELECTROTECHNICAL PRODUCTS –
Part 5: Cadmium, lead and chromium in polymers and electronics
and cadmium and lead in metals by AAS, AFS, ICP-OES and ICP-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 62321-5 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 62321-5 is a partial replacement of IEC 62321:2008, forming a
structural revision and generally replacing Clauses 8 to 10, as well as Annexes F, G and H.
Future parts in the IEC 62321 series will gradually replace the corresponding clauses from
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 62321-5:2014
62321-5 © IEC:2013 – 5 –
The text of this standard is based on the following documents:
FDIS Report on voting
111/297/FDIS 111/307/RVD
Full information on the voting for the approval of this standard can be found in the report on
voting indicated in the above table.
This publication has been drafted in accordance with the ISO/IEC Directives, Part 2.
A list of all parts in the IEC 62321 series can be found on the IEC website under the general
title: Determination of certain substances in electrotechnical products.
The committee has decided that the contents of this publication will remain unchanged until
the stability date indicated on the IEC web site 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.
IMPORTANT – The 'colour inside' logo on the cover page of this publication indicates
that it contains colours which are considered to be useful for the correct
understanding of its contents. Users should therefore print this document using a
colour printer.
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SIST EN 62321-5:2014
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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 adaptation 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 (PBDE’s)) 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.
WARNING – Persons using this International Standard should be familiar with normal
laboratory practice. This standard 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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SIST EN 62321-5:2014
62321-5 © IEC:2013 – 7 –
DETERMINATION OF CERTAIN SUBSTANCES
IN ELECTROTECHNICAL PRODUCTS –
Part 5: Cadmium, lead and chromium in polymers and electronics
and cadmium and lead in metals by AAS, AFS, ICP-OES and ICP-MS
1 Scope
This Part of IEC 62321 describes the test methods for lead, cadmium and chromium in
polymers, metals and electronics by AAS, AFS, ICP-OES and ICP-MS.
This standard specifies the determination of the levels of cadmium (Cd), lead (Pb) and
chromium (Cr) in electrotechnical products. It covers three types of matrices:
polymers/polymeric workpieces, metals and alloys and electronics.
This standard refers to the sample as the object to be processed and measured. What the
sample is or how to get to the sample is defined by the entity carrying out the tests. Further
guidance on obtaining representative samples from finished electronic products to be tested
for levels of regulated substances may be found in IEC 62321-2. It is noted that the selection
and/or determination of the sample may affect the interpretation of the test results.
This standard describes the use of four methods, namely AAS (atomic absorption
spectrometry), AFS (atomic fluorescence spectrometry), ICP-OES (inductively coupled plasma
optical emission spectrometry), and ICP-MS (inductively coupled plasma mass spectrometry)
as well as several procedures for preparing the sample solution from which the most
appropriate method of analysis can be selected by experts.
As the hexavalent-Cr analysis is sometimes difficult to determine in polymers and electronics,
this standard introduces the screening methods for chrome in polymers and electronics
except from AFS. Chromium analysis provides information about the existence of hexavalent-
Cr in materials. However, elemental analyses cannot selectively detect hexavalent-Cr; it
determines the amount of Cr in all oxidation states in the samples. If Cr amounts exceed the
hexavalent-Cr limit, testing for hexavalent-Cr should be performed.
The test procedures described in this standard are intended to provide the highest level of
accuracy and precision for concentrations of Pb, Cd and Cr that range, in the case of ICP-
OES and AAS, from 10 mg/kg for Pb, Cd and Cr, in the case of ICP-MS, from 0,1 mg/kg for
Pb and Cd in the case of AFS, the range is from 10 mg/kg for Pb and 1.5 mg/kg for Cd. The
procedures are not limited for higher concentrations.
This standard does not apply to materials containing polyfluorinated polymers because of
their stability. If sulfuric acid is used in the analytical procedure, there is a risk of losing Pb,
thus resulting in erroneously low values for this analyte. In addition, sulfuric acid and
hydrofluoric acid are not suitable for determining Cd by AFS, because it disturbs the reduction
of Cd.
Limitations and risks occur due to the solution step of the sample, e.g. precipitation of the
target or other elements may occur, in which case the residues have to be checked separately
or dissolved by another method and then combined with the test sample solution.
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SIST EN 62321-5:2014
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2 Normative references
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.
IEC 62321-1, Determination of certain substances in electrotechnical products – Part 1:
1
Introduction and overview
IEC 62321-2, Determination of certain substances in electrotechnical products – Part 2:
1
Disassembly, disjointment and mechanical sample preparation
IEC 62321-3-1, Determination of certain substances in electrotechnical products – Part 3-1:
Screening – Lead, mercury, cadmium, total chromium and total bromine using X-ray
1
fluorescence spectrometry
ISO 3696, Water for analytical laboratory use – Specification and test methods
ISO 5961, Water quality – Determination of cadmium by atomic absorption spectrometry
3 Terms, definitions and abbreviations
3.1 Terms and definitions
For the purposes of this document, the terms and definitions given in IEC 62321-1, as well as
the following, apply.
3.1.1
accuracy
closeness of agreement between a test result and an accepted reference value
3.1.2
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)
3.1.3
calibration solution
solution used to calibrate the instrument prepared either from (a) stock solution(s) or from a
(certified) reference material
3.1.4
certified reference material
reference material, accompanied by documentation issued by an authoritative body and
providing one or more specified property values with associated uncertainties and
traceabilities using valid procedures
3.1.5
laboratory control sample
known matrix spiked with compound(s) representative of the target analytes, used to
document laboratory performance
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To be published.
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SIST EN 62321-5:2014
62321-5 © IEC:2013 – 9 –
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[Based on US EPA SW-846] [1]
3.1.6
reagent blank solution
prepared by adding to the solvent the same amounts of reagents as those added to the test
sample solution (same final volume)
3.1.7
test sample solution
solution prepared with the test portion of the test sample according to the appropriate
specifications such that it can be used for the envisaged measurement
3.2 Abbreviations
CCV continuing calibration verification
LCS laboratory control sample
4 Reagents
4.1 General
For the determination of elements at trace level, the reagents shall be of adequate purity. The
concentration of the analyte or interfering substances in the reagents and water shall be
negligible compared to the lowest concentration to be determined.
All reagents for ICP-MS analysis, including acids or chemicals used shall be of high-purity:
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trace metals shall be less than 1 × 10 % in total.
For measurements by ICP-OES and ICP-MS, the memory effect occurs in cases where high
concentrations of elements are introduced. Dilution of the sample solution is required for high
levels of each element. If the memory effect is not decreased by dilution, thorough washing of
the equipment is required.
4.2 Reagents
The following reagents are used:
a) Water: Grade 1 specified in ISO 3696 used for preparation and dilution of all sample
solutions.
b)
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