CEI 62321 Ed.1: Produits électrotechniques – Détermination des niveaux de six
substances réglementées (plomb, mercure, cadmium, chrome hexavalent, diphényles,
polybromes, diphénylethers polybromes)
1 Scop9
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/FDIS IEC – 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, CVAFS,
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......................................................46
9.5 Preparation of laboratory reagent blank.................................................................48
– 4 – 62321/FDIS IEC
9.6 Test procedure ......................................................................................................48
9.6.1 Preparation of the calibrant .......................................................................48
9.6.2 Measurement of the calibrant ....................................................................48
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
Bibl 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 g/ml),
BDE-209 (50 g/ml) ..............................................................................................................73
Figure A.2 – Total ion chromatogram of PBB mixture (3,5 g/ml) ..........................................74
Figure A.3 – Total ion chromatogram of PBB and PBDE mixtures (BDE-1 to BDE-206 5
g/ml, BDE-209 5,0 g/ml, PBBs 3,5 g/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/FDIS IEC – 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 sn–1........................................................................86
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 samplesa ................................................. 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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