ROHs的IEC62321 111/54CDV标准
Procedures for the Determination of Levels of Six Regulated Substances
(Lead, Mercury, Hexavalent Chromium, Polybrominated Biphenyls,
Polybrominated Diphenyl Ethers) in Electrotechnical Products
CONTENTS
FOREWORD...........................................................................................................................7
INTRODUCTION.....................................................................................................................9
1 Scope.............................................................................................................................10
2 References.....................................................................................................................10
3 Definitions ......................................................................................................................11
3.12 Abbreviations ........................................................................................................12
4 Test Procedure Overview ...............................................................................................14
4.1 Test Procedure Scope ...........................................................................................14
4.2 Sample..................................................................................................................14
4.3 Test Procedure Flow .............................................................................................15
4.4 Adjustment to Matrix..............................................................................................16
4.5 Laboratory Report .................................................................................................16
4.6 Alternative Procedures ..........................................................................................17
5 Mechanical Sample Preparation .....................................................................................18
5.1 Scope, Application and Summary of Method..........................................................18
5.2 Apparatus / Equipment and Materials ....................................................................18
5.3 Procedure .............................................................................................................19
5.3.1 Sample ......................................................................................................19
5.3.2 Manual Cutting ..........................................................................................19
5.3.3 Coarse grinding /milling .............................................................................19
5.3.4 Homogenizing ...........................................................................................19
5.3.5 Fine grinding / milling ................................................................................20
5.3.6 Very Fine Grinding of Polymers and Organic Materials ..............................20
6 Screening by X-ray Fluorescence Spectrometry (XRF) ...................................................21
6.1 Scope, Application and Summary of Method..........................................................21
6.1.1 Principle ....................................................................................................22
6.1.2 Warnings ...................................................................................................22
6.2 Apparatus / Equipment and Materials ....................................................................22
6.3 Reagents...............................................................................................................22
6.4 Sampling ...............................................................................................................23
6.4.1 Non-Destructive Approach.........................................................................23
6.4.2 Destructive Approach ................................................................................23
6.5 Procedure .............................................................................................................23
6.5.1 General .....................................................................................................23
6.5.2 Preparation of the Spectrometer ................................................................24
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 Precision ...............................................................................................................27
6.8 Quality Assurance and Control ..............................................................................27
6.8.1 Accuracy of calibration ..............................................................................27
6.8.2 Control samples ........................................................................................27
6.9 Special Cases .......................................................................................................27
6.9.1 Presentation of Sample for Measurement ..................................................27
6.9.2 Uniformity of the Sample ...........................................................................28
6.10 Annex (Informative): Practical Application of Method .............................................29
6.10.1 Matrix and Interference Effects ..................................................................29
6.10.2 Interpretation of Results ............................................................................30
7 Determination of PBB and PBDE in Polymers by GC-MS................................................32
7.1 Apparatus / Equipment and Materials ....................................................................32
7.1.1 Apparatus..................................................................................................32
7.1.2 Equipment .................................................................................................32
7.1.3 Reagents ...................................................................................................33
7.2 General instructions on the analysis ......................................................................33
7.3 Sample preparation ...............................................................................................33
7.3.1 Stock solutions ..........................................................................................33
7.3.2 Pre-extraction of the Soxhlet extractors .....................................................33
7.3.3 Sample extraction......................................................................................33
7.3.4 Addition of the internal standard ................................................................34
7.4 Calibration.............................................................................................................34
7.4.1 PBB [1 μg/mL for each congener], PBDE [1 μg/mL for each
congener] and surrogate standard [0.2 μg/mL] stock solution ....................34
7.4.2 Calibration.................................................................................................34
7.4.3 Calculation of PBB and PBDE concentration..............................................35
7.5 GC-MS ..................................................................................................................36
7.6 Quality Control ......................................................................................................38
7.6.1 Method Detection Limit and Reporting Limit...............................................38
7.7 Evaluation of the Method.......................................................................................39
7.8 Annex (Informative) ...............................................................................................39
7.8.1 PBB & PBDE Calibration Standards...........................................................39
7.8.2 Alternative Extraction Procedures for Soluble Polymers.............................40
7.8.3 Examples of Chromatograms at suggested conditions ...............................41
8 Test for the Presence of Hexavalent Chromium (Cr VI) in Colorless and Colored
Chromate Coating on Metals ..........................................................................................44
8.1 Scope, Application and Summary of Method..........................................................44
8.2 Apparatus / Equipment and Materials ....................................................................44
8.3 Reagents...............................................................................................................44
8.4 Sample Preparation...............................................................................................45
8.5 Test Procedures ....................................................................................................45
8.5.1 Spot-test Procedure...................................................................................45
8.5.2 Boiling-water-extraction procedure ............................................................46
8.6 Evaluation of the Method.......................................................................................47
9 Determination of Hexavalent Chromium (Cr VI) by Colorimetric Method in Polymers
and Electronics...............................................................................................................48
9.1 Scope, Application and Summary of Method..........................................................48
9.2 Apparatus / Equipment and Materials ....................................................................48
9.2.1 Apparatus / Equipment ..............................................................................48
9.2.2 Materials ...................................................................................................49
9.2.3 Reagents ...................................................................................................49
9.3 Sample Preparation...............................................................................................50
9.4 Test Procedure......................................................................................................50
9.4.1 Extraction ..................................................................................................50
9.4.2 Color development and measurement........................................................51
9.4.3 Preparation of calibration curve .................................................................51
9.4.4 Calculation of Analytical Results................................................................51
9.4.5 Quality Control ..........................................................................................52
9.5 Evaluation of the Method.......................................................................................52
10 Determination of Mercury in Polymers, Metals and Electronics by CV-AAS, AFS,
ICP-OES, and ICP-MS....................................................................................................53
10.1 Scope, Application and Summary of Method..........................................................53
10.2 Apparatus / Equipment and Materials ....................................................................54
10.3 Reagents...............................................................................................................54
10.3.1 Contaminations .........................................................................................55
10.4 Sample Preparation...............................................................................................55
10.4.1 Test portion ...............................................................................................55
10.4.2 Wet Digestion (Digestion of metal materials and electronics) .....................55
10.4.3 Microwave digestion ..................................................................................56
10.5 Test Procedure......................................................................................................56
10.5.1 Standard preparation / Stock solution preparation .....................................56
10.5.2 Calibration.................................................................................................57
10.5.3 Instrument performance.............................................................................57
10.5.4 Sample Analysis ........................................................................................58
10.5.5 Calculation of Analytical Results................................................................58
10.6 Evaluation of the Method.......................................................................................58
10.7 Annex (Informative) ...............................................................................................59
10.7.1 Instrument parameters...............................................................................59
11 Determination of Lead and Cadmium in Polymers by ICP-OES, ICP-MS, and AAS .........61
11.1 Scope, Application and Summary of Method..........................................................61
11.2 Apparatus/Equipment and Materials ......................................................................61
11.2.1 Apparatus/Equipment ................................................................................61
11.3 Reagents...............................................................................................................62
11.4 Sample Preparation...............................................................................................63
11.4.1 Test portion ...............................................................................................63
11.4.2 Preparation of test solution........................................................................63
11.4.3 Preparation of laboratory reagent blank .....................................................65
11.5 Test Procedure......................................................................................................65
11.5.1 Preparation of calibration solution .............................................................66
11.5.2 Development of calibration curve...............................................................66
11.5.3 Measurement of sample ............................................................................66
11.5.4 Calculation ................................................................................................67
11.6 Evaluation of the Method.......................................................................................67
11.7 Annex (Informative) ...............................................................................................67
11.7.1 ICP-OES ...................................................................................................67
11.7.2 ICP-MS......................................................................................................69
11.7.3 AAS...........................................................................................................69
12 Determination of Lead and Cadmium in Metals by ICP-OES, ICP-MS, and AAS .............70
12.1 Scope, Application and Summary of Method..........................................................70
12.2 Apparatus/Equipment and Materials ......................................................................70
12.3 Reagents...............................................................................................................71
12.4 Sample Preparation...............................................................................................72
12.4.1 Test portion ...............................................................................................72
12.4.2 Preparation of test sample solution............................................................72
12.5 Preparation of laboratory reagent blank.................................................................73
12.6 Test Procedure......................................................................................................73
12.6.1 Preparation of calibration standard ............................................................73
12.6.2 Measurement of calibration standard .........................................................73
12.6.3 Measurement of sample ............................................................................74
12.6.4 Calculation ................................................................................................74
12.7 Evaluation of the Method.......................................................................................75
12.8 Annex (Informative) ...............................................................................................75
12.8.1 ICP-OES ...................................................................................................75
12.8.2 ICP-MS......................................................................................................77
12.8.3 AAS...........................................................................................................78
13 Determination of Lead and Cadmium in Electronics by ICP-OES, ICP-MS, and AAS.......79
13.1 Scope, Application and Summary of Method..........................................................79
13.2 Apparatus / Equipment and Materials ....................................................................79
13.3 Reagents...............................................................................................................80
13.4 Sample Preparation...............................................................................................81
13.4.1 Test portion ...............................................................................................81
13.4.2 Digestion with aqua regia ..........................................................................81
13.4.3 Microwave digestion ..................................................................................82
13.5 Test Procedure......................................................................................................83
13.5.1 Preparation of calibration solution .............................................................83
13.5.2 Standard preparation.................................................................................83
13.5.3 Calibration.................................................................................................84
13.5.4 Development of calibration curve...............................................................84
13.5.5 Measurement of sample ............................................................................85
13.5.6 Calculation of Analytical Results................................................................85
13.6 Evaluation of the Method.......................................................................................85
13.7 Annex (Informative) ...............................................................................................86
13.7.1 ICP-OES(-OES) .........................................................................................86
13.7.2 ICP-MS......................................................................................................88
13.7.3 AAS...........................................................................................................89
Annex A (Informative) A Practical Guide for Testing Electronic Products..............................90
A.1 Introduction ....................................................................................................................90
A.2 Scope.............................................................................................................................90
A.3 Testing of Products ........................................................................................................90
A.3.1 Evaluation of a Product without Disassembly.........................................................91
A.3.2 Evaluation of a Product Using Simple Disassembly Techniques ............................92
A.3.3 Evaluation of a Product Using Detailed Disassembly Techniques ..........................94
A.4 Additional Guidance .......................................................................................................94
A.5 Interpretation of Test Results Applied to Materials Isolated from Products ......................95
Annex B (Informative) Bibliography ......................................................................................97
Annex C (Informative) Commercially Available Certified Reference Materials (CRM) ......... 100
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