Electrotechnical products - Determination of levels of six regulated substances (lead, mercury, cadmium, hexavalent chromium, polybrominated biphenyls, polybrominated diphenyl ethers)

IEC 62321, which is an International Standard, specifies the determination of the levels of lead (Pb), mercury (Hg), cadmium (Cd), hexavalent chromium (Cr(VI)) contained in inorganic and organic compounds, and two types of brominated flame retardants, polybrominated biphenyls (PBB) and polybrominated diphenyl ethers (PBDE) contained in electrotechnical products. This standard refers to the sample as the object to be processed and measured. The nature of the sample and the manner in which it is acquired is defined by the entity carrying out the tests and not by this standard.

Produkte in der Elektrotechnik - Bestimmung von Bestandteilen der sechs Inhaltsstoffe (Blei, Quecksilber, Cadmium, sechswertiges Chrom, polybromiertes Biphenyl, polybromierter Diphenylether), die einer Beschränkung unterworfen sind

Produits électrotechniques - Détermination des niveaux en six substances réglementées (plomb, mercure, cadmium, chrome hexavalent, diphényles polybromes, diphényléthers polybromes)

La CEI 62321:2008, qui est une Norme internationale, spécifie la détermination des niveaux de plomb (Pb), de mercure (Hg), de cadmium (Cd), de chrome hexavalent (Cr(VI)) contenus dans des composés inorganiques et organiques, ainsi que de deux types de retardateurs de flammes bromés, diphényles polybromés (PBB) et diphényles éthers polybromés (PBDE) contenus dans les produits électrotechniques. Cette norme fait référence à l'échantillon comme étant l'objet à traiter et à mesurer. L'entité qui réalise les essais définit la nature de l'échantillon et la manière de l'obtenir, et non pas la présente norme. Elle a le statut de norme horizontale conformément au Guide 108.

Elektrotehniški izdelki - Določanje vsebnosti šestih reguliranih substanc (svinec, živo srebro, kadmij, šestvalentni krom, polibromirani bifenili, polibromirani difenil etri) (IEC 62321:2008)

General Information

Status
Withdrawn
Publication Date
11-May-2009
Withdrawal Date
29-Aug-2018
Current Stage
9900 - Withdrawal (Adopted Project)
Start Date
30-Aug-2018
Due Date
22-Sep-2018
Completion Date
30-Aug-2018

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SLOVENSKI STANDARD
SIST EN 62321:2009
01-junij-2009

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Electrotechnical products - Determination of levels of six regulated substances (lead,

mercury, cadmium, hexavalent chromium, polybrominated biphenyls, polybrominated
diphenyl ethers)

Produkte in der Elektrotechnik - Bestimmung von Bestandteilen der sechs Inhaltsstoffe

(Blei, Quecksilber, Cadmium, sechswertiges Chrom, polybromiertes Biphenyl,
polybromierter Diphenylether), die einer Beschränkung unterworfen sind

Produits électrotechniques - Détermination des niveaux en six substances réglementées

(plomb, mercure, cadmium, chrome hexavalent, diphényles polybromes, diphényléthers

polybromes)
Ta slovenski standard je istoveten z: EN 62321:2009
ICS:
29.020 Elektrotehnika na splošno Electrical engineering in
general
31.020 Elektronske komponente na Electronic components in
splošno general
SIST EN 62321:2009 en,fr,de

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

---------------------- Page: 1 ----------------------
SIST EN 62321:2009
---------------------- Page: 2 ----------------------
SIST EN 62321:2009
EUROPEAN STANDARD
EN 62321
NORME EUROPÉENNE
April 2009
EUROPÄISCHE NORM
ICS 13.020; 43.040.10
English version
Electrotechnical products -
Determination of levels of six regulated substances
(lead, mercury, cadmium, hexavalent chromium,
polybrominated biphenyls, polybrominated diphenyl ethers)
(IEC 62321:2008)
Produits électrotechniques - Produkte in der Elektrotechnik -
Détermination des niveaux Bestimmung von Bestandteilen
de six substances réglementées der sechs Inhaltsstoffe
(plomb, mercure, cadmium, chrome (Blei, Quecksilber, Cadmium,
hexavalent, diphényles polybromés, sechswertiges Chrom, polybromiertes
diphényléthers polybromés) Biphenyl, polybromierter Diphenylether),
(CEI 62321:2008) die einer Beschränkung unterworfen sind
(IEC 62321:2008)

This European Standard was approved by CENELEC on 2009-03-01. 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 Central Secretariat 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 Central Secretariat has the same status as the official versions.

CENELEC members are the national electrotechnical committees of Austria, Belgium, Bulgaria, Cyprus, the

Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia,

Lithuania, Luxembourg, Malta, the Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain,

Sweden, Switzerland and the United Kingdom.
CENELEC
European Committee for Electrotechnical Standardization
Comité Européen de Normalisation Electrotechnique
Europäisches Komitee für Elektrotechnische Normung
Central Secretariat: avenue Marnix 17, B - 1000 Brussels

© 2009 CENELEC - All rights of exploitation in any form and by any means reserved worldwide for CENELEC members.

Ref. No. EN 62321:2009 E
---------------------- Page: 3 ----------------------
SIST EN 62321:2009
EN 62321:2009 – 2 –
Foreword

The text of document 111/116/FDIS, future edition 1 of IEC 62321, prepared by IEC TC 111,

Environmental standardization for electrical and electronic products and systems, was submitted to the

IEC-CENELEC parallel vote and was approved by CENELEC as EN 62321 on 2009-03-01.
The following dates were fixed:
– latest date by which the EN has to be implemented
at national level by publication of an identical
national standard or by endorsement (dop) 2009-12-01
– latest date by which the national standards conflicting
with the EN have to be withdrawn (dow) 2012-03-01
Annex ZA has been added by CENELEC.
__________
Endorsement notice

The text of the International Standard IEC 62321:2008 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 60730-1 NOTE Harmonized as EN 60730-1:2000 (modified).
ISO 3613 NOTE Harmonized as EN ISO 3613:2001 (not modified).
ISO 17294-1 NOTE Harmonized as EN ISO 17294-1:2006 (not modified).
__________
---------------------- Page: 4 ----------------------
SIST EN 62321:2009
– 3 – EN 62321:2009
Annex ZA
(normative)
Normative references to international publications
with their corresponding European publications

The following referenced documents are indispensable for the application 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 When an international publication has been modified by common modifications, indicated by (mod), the relevant EN/HD

applies.
Publication Year Title EN/HD Year
ISO/IEC Guide 98 1995 Guide to the expression of uncertainty in - -
measurement (GUM)
1) 2)
ISO/IEC 17025 - General requirements for the competence EN ISO/IEC 17025 2005
of testing and calibration laboratories
1) 2)
ISO 3696 - Water for analytical laboratory use - EN ISO 3696 1995
Specification and test methods
1) 2)
ISO 5961 - Water quality - Determination of cadmium EN ISO 5961 1995
by atomic absorption spectrometry
Undated reference.
Valid edition at date of issue.
---------------------- Page: 5 ----------------------
SIST EN 62321:2009
---------------------- Page: 6 ----------------------
SIST EN 62321:2009
IEC 62321
Edition 1.0 2008-12
INTERNATIONAL
STANDARD
NORME
INTERNATIONALE
Electrotechnical products – Determination of levels of six regulated substances
(lead, mercury, cadmium, hexavalent chromium, polybrominated biphenyls,
polybrominated diphenyl ethers)
Produits électrotechniques – Détermination des niveaux de six substances
réglementées (plomb, mercure, cadmium, chrome hexavalent, diphényles
polybromés, diphényléthers polybromés)
INTERNATIONAL
ELECTROTECHNICAL
COMMISSION
COMMISSION
ELECTROTECHNIQUE
PRICE CODE
INTERNATIONALE
CODE PRIX
ICS 13.020; 43.040.10 ISBN 2-8318-1020-7
® Registered trademark of the International Electrotechnical Commission
Marque déposée de la Commission Electrotechnique Internationale
---------------------- Page: 7 ----------------------
SIST EN 62321:2009
– 2 – 62321 © IEC:2008
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 ........................................................................................................11

4 Test methods – Overview ...............................................................................................13

4.1 Field of application ................................................................................................13

4.2 Sample..................................................................................................................13

4.3 Test methods – Flow chart ....................................................................................14

4.4 Adjustment to the matrix........................................................................................15

4.5 Limits of detection (LOD) and limits of quantification (LOQ)...................................15

4.6 Test report ............................................................................................................16

4.7 Alternative test methods ........................................................................................16

5 Mechanical sample preparation ......................................................................................17

5.1 Overview ...............................................................................................................17

5.1.1 Field of application ....................................................................................17

5.1.2 Quality assurance......................................................................................17

5.2 Apparatus, equipment and materials .....................................................................17

5.3 Procedure .............................................................................................................18

5.3.1 Manual cutting...........................................................................................18

5.3.2 Coarse grinding/milling ..............................................................................18

5.3.3 Homogenizing ...........................................................................................18

5.3.4 Fine grinding/milling ..................................................................................18

5.3.5 Very fine grinding of polymers and organic materials .................................19

6 Screening by X-ray fluorescence spectrometry (XRF) .....................................................19

6.1 Overview ...............................................................................................................19

6.1.1 Principle ....................................................................................................21

6.1.2 Warnings ...................................................................................................22

6.2 Apparatus, equipment and materials .....................................................................22

6.2.1 XRF spectrometer .....................................................................................22

6.2.2 Materials and tools ....................................................................................22

6.3 Reagents...............................................................................................................22

6.4 Sampling ...............................................................................................................22

6.4.1 Non-destructive approach..........................................................................22

6.4.2 Destructive approach.................................................................................23

6.5 Procedure .............................................................................................................23

6.5.1 General .....................................................................................................23

6.5.2 Preparation of the spectrometer ................................................................23

6.5.3 Test portion ...............................................................................................24

6.5.4 Verification of spectrometer performance...................................................24

6.5.5 Tests .........................................................................................................25

6.5.6 Calibration.................................................................................................25

6.6 Calculations ..........................................................................................................26

6.7 Evaluation of the method.......................................................................................27

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SIST EN 62321:2009
62321 © IEC:2008 – 3 –

6.7.1 Lead..........................................................................................................27

6.7.2 Mercury .....................................................................................................27

6.7.3 Cadmium ...................................................................................................27

6.7.4 Chromium..................................................................................................27

6.7.5 Bromine.....................................................................................................28

6.8 Quality control .......................................................................................................28

6.8.1 Accuracy of calibration ..............................................................................28

6.8.2 Control samples ........................................................................................28

6.9 Special cases ........................................................................................................28

6.9.1 Presentation of a sample for measurement................................................28

6.9.2 Uniformity of the sample............................................................................29

7 Determination of mercury in polymers, metals and electronics by CV-AAS, CV-

AFS, ICP-OES and ICP-MS ............................................................................................30

7.1 Overview ...............................................................................................................30

7.2 Apparatus, equipment and materials .....................................................................31

7.3 Reagents...............................................................................................................32

7.4 Sample preparation ...............................................................................................33

7.4.1 Test portion ...............................................................................................33

7.4.2 Wet digestion (digestion of electronics) .....................................................33

7.4.3 Microwave digestion ..................................................................................34

7.4.4 Preparation of laboratory reagent blank .....................................................34

7.5 Test procedure ......................................................................................................34

7.5.1 Preparation of calibrant solutions ..............................................................34

7.5.2 Development of the calibration curve .........................................................35

7.5.3 Measurement of the sample.......................................................................36

7.5.4 Calculation ................................................................................................36

7.6 Evaluation of the method.......................................................................................36

8 Determination of lead and cadmium in polymers by ICP-OES, ICP-MS and AAS ............37

8.1 Overview ...............................................................................................................37

8.2 Apparatus, equipment and materials .....................................................................38

8.3 Reagents...............................................................................................................39

8.4 Sample preparation ...............................................................................................40

8.4.1 Test portion ...............................................................................................40

8.4.2 Preparation of test solution........................................................................40

8.4.3 Preparation of laboratory reagent blank .....................................................42

8.5 Test procedure ......................................................................................................42

8.5.1 Preparation of calibration solution .............................................................42

8.5.2 Development of the calibration curve .........................................................43

8.5.3 Measurement of the sample.......................................................................43

8.5.4 Calculation ................................................................................................44

8.6 Evaluation of the method.......................................................................................44

9 Determination of lead and cadmium in metals by ICP-OES, ICP-MS and AAS ................44

9.1 Overview ...............................................................................................................44

9.2 Apparatus, equipment and materials .....................................................................45

9.3 Reagents...............................................................................................................45

9.4 Sample preparation ...............................................................................................46

9.4.1 Test portion ...............................................................................................46

9.4.2 Preparation of the test sample solution......................................................47

9.5 Preparation of laboratory reagent blank.................................................................48

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SIST EN 62321:2009
– 4 – 62321 © IEC:2008

9.6 Test procedure ......................................................................................................48

9.6.1 Preparation of the calibrant .......................................................................48

9.6.2 Measurement of the calibrant ....................................................................49

9.6.3 Measurement of the sample.......................................................................49

9.6.4 Calculation ................................................................................................50

9.7 Evaluation of the method.......................................................................................50

10 Determination of lead and cadmium in electronics by ICP-OES, ICP-MS and AAS..........50

10.1 Overview ...............................................................................................................50

10.2 Apparatus, equipment and materials .....................................................................51

10.3 Reagents...............................................................................................................52

10.4 Sample preparation ...............................................................................................53

10.4.1 Test portion ...............................................................................................53

10.4.2 Digestion with aqua regia ..........................................................................53

10.4.3 Microwave digestion ..................................................................................54

10.5 Test procedure ......................................................................................................55

10.5.1 Preparation of a calibrant solution .............................................................55

10.5.2 Standard preparation.................................................................................55

10.5.3 Calibration.................................................................................................56

10.5.4 Development of the calibration curve .........................................................56

10.5.5 Measurement of the sample.......................................................................57

10.5.6 Calculation ................................................................................................57

10.6 Evaluation of the method.......................................................................................58

Annex A (informative) Determination of PBB and PBDE in polymers by GC-MS ...................59

Annex B (informative) Test for the presence of hexavalent chromium (Cr(VI)) in

colourless and coloured corrosion-protected coatings on metals ...........................................75

Annex C (Informative) Determination of hexavalent chromium (Cr(VI)) in polymers and

electronics by the colorimetric method ..................................................................................80

Annex D (informative) Practical application of screening by X-ray fluorescence

spectrometry (XRF)...............................................................................................................88

Annex E (informative) Practical application of determination of mercury in polymers,

metals and electronics by CV-AAS, CV-AFS, ICP-OES and ICP-MS .....................................95

Annex F (informative) Practical application of determination of lead and cadmium in

polymers by ICP-OES, ICP-MS and AAS ..............................................................................97

Annex G (informative) Practical application of determination of lead and cadmium in

metals by ICP-OES, ICP-MS and AAS ..................................................................................99

Annex H (informative) Practical application of determination of lead and cadmium in

electronics by ICP-OES, ICP-MS and AAS..........................................................................102

Bibliography........................................................................................................................106

Figure 1 – Flow chart of the test methods .............................................................................14

Figure A.1 – Total ion chromatogram of PBDE mixture, BDE-1 to BDE-206 (5 μg/ml),

BDE-209 (50 μg/ml) ..............................................................................................................73

Figure A.2 – Total ion chromatogram of PBB mixture (3,5 μg/ml) ..........................................74

Figure A.3 – Total ion chromatogram of PBB and PBDE mixtures (BDE-1 to BDE-206 5

μg/ml, BDE-209 5,0 μg/ml, PBBs 3,5 μg/ml)..........................................................................74

Figure E.1 – Heating digester equipped with reaction vessel, reflux cooler and

absorption vessel..................................................................................................................95

Figure G.1 – Background correction....................................................................................100

Figure H.1 – Background correction....................................................................................104

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SIST EN 62321:2009
62321 © IEC:2008 – 5 –

Table 1 – Overview of the content of the verification procedure ............................................15

Table 2 – Tested concentration ranges for lead in materials ..................................................20

Table 3 – Tested concentration ranges for mercury in materials............................................20

Table 4 – Tested concentration ranges for cadmium in materials ..........................................20

Table 5 – Tested concentration ranges for total chromium in materials .................................20

Table 6 – Tested concentration ranges for bromine in materials............................................20

Table 7 – Recommended X-ray lines for individual analytes..................................................24

Table 8 – Mean results and recovery rates of mercury obtained in the IIS2 study..................37

Table A.1 – Matrix spiking solution .......................................................................................61

Table A.2 – Calibration solutions of PBBs and PBDEs ..........................................................62

Table A.3 – Reference masses for the quantification of PBBs ...............................................67

Table A.4 – Reference masses for the quantification of PBDEs.............................................67

Table A.5 – Example calculation ...........................................................................................68

Table A.6 – Example list of commercially available calibration congeners considered

suitable for this analysis .......................................................................................................71

Table A.7 – PBB and PBDE congeners in the mixture ...........................................................72

Table C.1 – Method detection limit = t × s ........................................................................86

n–1

Table D.1 – Effect of matrix composition on limits of detection of some controlled

elements...............................................................................................................................89

Table D.2 – Screening limits in mg/kg for regulated elements in various matrices .................90

Table D.3 – Mean results and recovery rates for lead obtained in the IIS2 study...................91

Table D.4 – Mean results and recovery rates for mercury obtained in the IIS2 study.............92

Table D.5 – Mean results and recovery rates for cadmium obtained in the IIS2 study ...........92

Table D.6 – Mean results and recovery rates for total chromium obtained in the IIS2

study ....................................................................................................................................93

Table D.7 – Mean results and recovery rates for total bromine obtained in the IIS2

study ....................................................................................................................................94

Table E.1 – Program for microwave digestion of samples (power output for five

vessels) ................................................................................................................................96

Table F.1 – Spectral interferences for the wavelengths of cadmium and lead........................97

Table F.2 – Examples of mass/charge (m/z) ratios................................................................98

Table F.3 – Examples of wavelengths for AAS ......................................................................98

Table G.1 – Spectral interferences for the wavelengths of cadmium and lead .......................99

Table G.2 – Examples of mass/charge (m/z) ratios ............................................................. 101

Table G.3 – Examples for wavelengths for AAS ..................................................................101

Table H.1 – Program for microwave digestion of samples .................................................102

Table H.2 – Spectral interferences for the wavelengths of cadmium and lead ..................... 103

Table H.3 – Examples of mass/charge (m/z) ratios ............................................................. 105

Table H.4 – Examples of wavelengths for AAS....................................................................105

---------------------- Page: 11 ----------------------
SIST EN 62321:2009
– 6 – 62321 © IEC:2008
INTERNATIONAL ELECTROTECHNICAL COMMISSION
___________
ELECTROTECHNICAL PRODUCTS –
DETERMINATION OF LEVELS OF SIX REGULATED SUBSTANCES
(LEAD, MERCURY, CADMIUM, HEXAVALENT CHROMIUM,
POLYBROMINATED BIPHENYLS, POLYBROMINATED DIPHENYL ETHERS)
FOREWORD

1) The International Electrotechnical Commission (IEC) is a worldwide organisation for standardisation comprising

all national electrotechnical committees (IEC National Committees). The object of the IEC is to promote

international co-operation on all questions concerning standardisation in the electrical and electronic fields. To

this end and in addition to other activities, the 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 organisations liaising with the IEC also participate in this preparation. The IEC collaborates

closely with the International Organisation for Standardisation (ISO) in accordance with conditions determined

by agreement between the two organisations.

2) The formal decisions or agreements of the 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

...

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