IEC 62321:2008

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)


IEC 62321:2008

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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
® Registered trademark of the International Electrotechnical Commission
Marque déposée de la Commission Electrotechnique Internationale

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– 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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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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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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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

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INTERNATIONAL ELECTROTECHNICAL COMMISSION

___________



ELECTROTECHNICAL PRODUCTS –

DETERMINATION OF LEVELS OF SIX REGULATED SUBSTANCES

(LEAD, MERCURY, CADMIUM, HEXAVALENT CHROMIUM,

POLYBROMINATED BIPHENYLS, POLYBROMINATED DIPHENYL ETHERS)





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