IEC 62321:2008

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

IEC 62321:2008, 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. It has the status of a horizontal standard in accordance with IEC Guide 108.

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

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 IEC 108.

General Information

• Status: Withdrawn
• Publication Date: 10-Dec-2008
• Withdrawal Date: 22-Mar-2018
• ICS: 13.020.01 - Environment and environmental protection in general
• ICS: 43.040.10 - Electrical and electronic equipment
• Technical Committee: TC 111 - Environmental standardization for electrical and electronic products and systems
• Drafting Committee: WG 3 - TC 111/WG 3
• Current Stage: WPUB - Publication withdrawn
• Start Date: 26-Mar-2018
• Completion Date: 23-Mar-2018

Standards Content (Sample)

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)

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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
XE
CODE PRIX
ICS 13.020; 43.040.10 ISBN 978-2-88910-672-1
– 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

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

– 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

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
a
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

– 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
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patent rights. The IEC shall not be held responsible for identifying any or all such patent rights.
International Standard IEC 62321 has been prepared by IEC technical committee 111:
Environmental standardization for electrical and electronic products and systems.
It has the status of a horizontal standard in accordance with IEC Guide 108.
The text of this standard is based on the following documents:
FDIS Report on voting
111/116/FDIS 111/125/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 ISO/IEC Directives, Part 2.

62321 © IEC:2008 – 7 –
The committee has decided that the contents of this publication will remain unchanged until
the maintenance result 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.
– 8 – 62321 © IEC:2008
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 such as 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) in electrotechnical products, is regulated in current and proposed regional

legislation.
The purpose of IEC 62321 is therefore to provide test methods that will allow the
electrotechnical industry to determine the levels of regulated substances Pb, Hg, Cd, Cr(VI)
and their compounds, as well as PBB and PBDE in electrotechnical products on a consistent
global basis.
62321 © IEC:2008 – 9 –
ELECTROTECHNICAL PRODUCTS –
DETERMINATION OF LEVELS OF SIX REGULATED SUBSTANCES (LEAD,

MERCURY, CADMIUM, HEXAVALENT CHROMIUM, POLYBROMINATED

BIPHENYLS, POLYBROMINATED DIPHENYL ETHERS)

1 Scope
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.
NOTE 1 Further guidance on obtaining representative samples from finished electronic products to be tested for
levels of regulated substances may be found in the future IEC Publicly Available Specification (PAS) for sampling
disjointment .
It is noted that the selection of the sample may affect the interpretation of the test results.
This standard does not determine:
• the definition of a “unit” or “homogenous material” as the sample;
• the disassembly procedure employed for obtaining a sample;
• assessment procedures.
NOTE 2 Further guidance on assessment procedures may be found in the future IEC Technical Specification
[1]
IEC/TS 62476 .
2 Normative references
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.

ISO/IEC Guide 98:1995, ISO Guide to the expression of uncertainty in measurement (GUM)
ISO 3696, Water for analytical laboratory use – Specification and test methods
ISO 5961, Water quality – Determination of cadmium by atomic absorption spectrometry
ISO 17025, General requirements for the competence of testing and calibration laboratories
—————————
Under consideration, no number yet assigned.
Figures in square brackets refer to the bibliography.

– 10 – 62321 © IEC:2008
3 Terms, definitions and abbreviations

3.1 Terms and definitions
For the purposes of this document, the following terms and definitions apply.

3.1.1
analyte
substance to be measured
3.1.2
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)
3.1.3
calibration blank
substance identical in form and matrix composition to the calibrant(s) but containing no
analyte(s)
3.1.4
certified reference material
CRM
reference material, accompanied by a certificate, one or more of whose properties are
certified by a procedure which establishes traceability to an accurate realization of the unit in
which the property values are expressed, and for which each certified value is accompanied
by an uncertainty at a stated level of confidence
[2]
[ISO Guide 30]
3.1.5
digestate
solution obtained after completion of sample digestion process
3.1.6
electronic assembly
group of components, at least one of which is an electronic device, but in which individual
parts may be replaced without damage to the assembly
EXAMPLE Group of components mounted on a printed wiring board.

[3]
[IEC 60730-1:1999, definition H.2.5.9]
3.1.7
electronic components
electrical or electronic devices that are not subject to disassembly without destruction or
impairment of design use. They are sometimes called electronic parts, or piece parts
EXAMPLES Resistors, capacitors, diodes, integrated circuits, hybrids, application-specific
integrated circuits, wound components and relays.
[4]
[IEC/TS 62239:2003]
3.1.8
electronics
electronic assembly and/or electronic component and/or field-replaceable unit

62321 © IEC:2008 – 11 –
3.1.9
field replaceable unit
FRU
part, component or subassembly that is easily removed (mechanically disjointed) using

ordinary tools
NOTE “Easily removed” means using ordinary tools to perform such functions as screwing or disconnecting, and
only without irreversibly destroying the unit.

[5]
[IEC Guide 114:2005, definition 3.7]

3.1.10
matrix
material or substance and its form or state in which analyte is embedded or to which analyte
is attached
3.1.11
performance-based measurement system
PBMS
set of processes wherein the data needs, mandates or limitations of a program or project are
specified, serving as criteria for selecting appropriate methods to meet those needs in a cost-
effective manner
NOTE The criteria may be published in regulations, technical guidance documents, permits, work plans or
enforcement orders.
3.1.12
reference material
material or substance, one or more of whose property values are sufficiently homogeneous
and well established to be used for the calibration of an apparatus, the assessment of a
measurement method or for assigning values to materials
[ISO Guide 30, modified]
3.2 Abbreviations
AAS Atomic absorption spectrometry
ABS Acrylonitrile butadiene styrene
AFS Atomic fluorescence spectrometry
ASTM American Society for Testing and Materials
BCR Community Bureau of Reference (BCR : Bureau Communautaire de Référence)
BL Below limit
BSA N,O-bis(trimethylsilyl) acetamide
BSTFA N,O-bis(trimethylsilyl)-trifluoroacetamide
CCC Continuing calibration check standard
CCFL Cold cathode fluorescent lamp
CFR Code of Federal Regulations
CRM Certified reference material
CV-AAS Cold vapour atomic absorption spectrometry
CV-AFS Cold vapour atomic fluorescence spectrometry
DBOFB 4,4’-dibromooctafluorobiphenyl
DIN Deutsches Institut für Normung
DMDCS Dimethyldichlorosilane in dichloromethane
EC European Community
– 12 – 62321 © IEC:2008
EDXRF Energy dispersive X-ray fluorescence

EI Electron ionization
EN European norm
EPA Environmental Protection Agency

EVAC Ethylene vinyl acetate
FEP Perfluoro(ethylene-propylene)

FP Fundamental parameters
FRU Field replaceable unit
GC Gas chromatography
GC-MS Gas chromatography – mass spectrometry
GLP Good laboratory practice
HPLC-UV High-performance liquid chromatography – ultraviolet
ICP-MS Inductively coupled plasma mass spectrometry
ICP-OES Inductively coupled plasma optical emission spectrometry
IS Internal standard
IIS International interlaboratory study
IUPAC International Union of Pure and Applied Chemistry
JIS Japanese Industrial Standard
LN Liquid nitrogen
LOD Limit of detection
LOQ Limit of quantification
MDL Method detection limit
NIST National Institute of Standards and Technology
NMIJ National Metrology Institute of Japan
OctaBB Octabromobiphenyl
OctaBDE Octabromodiphenyl ether
OL Over limit
PAS Publicly Available Specification
PBB Polybrominated biphenyl
PBDE Polybrominated diphenyl ether
PBMS Performance-based measurement system

PC Polycarbonate
PE Polyethylene
PE-HD High-density polyethylene
PFA Perfluoro alkoxyl alkane resin
PS-HI High-impact polystyrene
PTFE Polytetrafluoroethylene
PTV Programmable temperature vaporization
PVC Polyvinyl chloride
PWB Printed wiring board
QA Quality assurance
QC Quality control
RH Relative humidity
62321 © IEC:2008 – 13 –
RSD Relative standard deviation

SIM Single (or “selected”) ion monitoring

SOP Standard Operating Procedure

SRM Standard reference material

TFM Tetrafluoroethylene modified

US United States
WC Tungsten carbide
WDXRF Wavelength dispersive X-ray fluorescence

XRF X-ray fluorescence
4 Test methods – Overview
4.1 Field of application
The contents of the test methods to determine the levels of regulated substances are grouped
in two important steps:
• Analytical test methods
• Laboratory implementation
Analytical test methods were developed and validated to ensure their suitability to the task.
They are divided into five main parts:
• Overview
• Apparatus/equipment and materials
• Reagents
• Sample preparation
• Test method, which includes:
– calibration;
– instrument performance;
– sample analysis;
– calculation of analytical results;
– test report;
– quality control.
Descriptions of individual test methods follow this outline.
Laboratory implementation is not covered in this standard, as laboratories are able to
implement test methods described using test methods and standards addressed in other
sources. The implementation step includes suitable quality assurance measures and a
validation protocol that documents the performance of the analytical method using the
instruments in the laboratory. Quality assurance systems such as good laboratory practice
(GLP) and/or accreditation to similar international or national systems (e.g. ISO 17025) are
strongly encouraged.
4.2 Sample
This standard refers to the sample as the object to be processed and measured according to
the test methods to determine the levels of the regulated substances. A sample can either be
a polymer, a metal or electronics.

– 14 – 62321 © IEC:2008
What the sample is or how to get to the sample shall be defined with respect to applicable

normative documents by the entity carrying out the test methods.

NOTE The entity can be either the organization commissioning the work or the organization carrying out the work.

In practice the requestor and the analyst will probably agree on the sample to be taken.

The entity may decide to prepare a sample that is a homogenous material. For this kind of

sample, the test methods applicable to metals or polymers are especially suitable.

The entity may also decide to prepare a sample which is an electronic component, an

electronic assembly or a field replaceable unit (FRU). For this kind of sample, the test

methods applicable to electronics are especially suitable.

The methods to obtain the sample are outside the scope of this standard. Further guidance
may be found in the future IEC Publicly Available Specification (PAS) for sample disjointment.
4.3 Test methods – Flow chart
Figure 1 gives a flow chart of the test methods to determine the levels of regulated
substances in electrotechnical products.

Non-destructive
Yes
sample
preparation
Entity based
Meets Pass
Screening
Sample
conforming
limits?
procedure
uniform?
sample
Mechanical
sample
Fail
No
preparation
Samples
Yes
Entity based
No
Yes
Further
Metallic
non conforming
materials, testing?
sample
polymer
Screening?
materials
Entity based
Electronics
Pass
No conforming
(PWB/
component)
sample
Mechanical Verification test
Meets
sample procedure –
limits?
preparation Various methods
Entity based
Fail
non conforming
sample
Decision criteria will
Decision
be entity base
IEC  2244/08
Figure 1 – Flow chart of the test methods
After obtaining the sample, which is either a polymer, a metal or electronics (e.g. in the form
of electronic components, electronic assemblies or FRUs), a decision is taken as to whether
the screening procedure or the verification procedure using a variety of test methods will be
used.
The screening procedure may be carried out either by directly measuring the sample (non-
destructive sample preparation) or by destroying the sample to make it uniform (mechanical
sample preparation). This decision shall be made by judging the uniformity of the sample. A
screening of representative samples of many uniform materials (such as polymers, alloys,
glass) may be done non-destructively, while for other more complex samples (such as a
FRU), mechanical sample preparation may be an appropriate solution. Mechanical sample
preparation is the same for both the screening and the verification test procedure. The
procedure for mecha
...