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GB/T 39560.303-2024Determination of certain substances in electrical and electronic products—Part 3-3:Screening polybrominated biphenyls, polybrominated diphenyl ethers and phthalates in polymers by gas chromatography-mass spectrometry using a pyrolyser/thermal desorption accessory (Py/TD-GC-MS) (English PDF)

电子电气产品中某些物质的测定 第3-3部分:配有热裂解/热脱附的气相色谱-质谱法 (Py/TD-GC-MS)筛选聚合物中的多溴联苯、多溴二苯醚和邻苯二甲酸酯

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Issued by

State Administration for Market Regulation, China National Standardization Administration

Level / Type

National · Recommended

Issue date

August 23, 2024

Implementation date

August 23, 2024

Scope

GB/T 39560.303-2024 is the English-translated version of 电子电气产品中某些物质的测定 第3-3部分:配有热裂解/热脱附的气相色谱-质谱法 (Py/TD-GC-MS)筛选聚合物中的多溴联苯、多溴二苯醚和邻苯二甲酸酯.

GB/T 39560.303-2024 — This document specifies the use of gas chromatography-mass spectrometry with pyrolysis/thermal desorption (Py/TD-GC-MS) for the analysis of polymers in electrical and electronic products.

Polybrominated biphenyls (PBB), polybrominated diphenyl ethers (PBDE), diisobutyl phthalate (DIBP), dibutyl phthalate (DBP), Benzyl butyl phthalate (BBP), di(2-ethylhexyl) phthalate (DEHP), dioctyl phthalate (DNOP), the present invention provides a screening analysis method for diisononyl formate (DINP) and diisodecyl phthalate (DIDP).

It has been tested for decabromodiphenyl ether (100mg/kg~1000mg/kg) and the above-mentioned single phthalates (100mg/kg~ 4000mg/kg) of polypropylene (PP), polystyrene (PS) and polyvinyl chloride (PVC) materials, and the test method was verified.

The method described in this document is used to determine the presence of PBB (monobrominated to decabrominated), PBDE (monobrominated to decabrominated), phthalates in other types of polymers.

No specific verification has been conducted on esters or concentrations outside the above specified range.

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Document preview — GB/T 39560.303-2024

National Standard of the People's Republic of China

Classification
L 10

Issued by: State Administration for Market Regulation, China National Standardization Administration

Contents

  • Preface
  • Introduction
  • 1 Scope
  • 2 Normative references
  • 3 Terms, definitions and abbreviations
  • 3.1 Terms and Definitions
  • 3.2 Abbreviations
  • 4 Principle
  • 4.1 Overview
  • 4.2 Detection Principle
  • 5 Reagents and Materials
  • 6 Instruments and Equipment
  • 7 Sampling
  • 8 Procedure
  • 8.1 General description of the analysis
  • 8.2 Sample preparation
  • 8.3 Instrument parameters
  • 8.4 Calibration
  • 9 Calculation
  • 9.1 Overview
  • 9.2 Determination of RF of DEHP
  • 9.3 Calculation formula
  • 10 Precision
  • 10.1 Screening and judgment
  • 10.2 Repeatability and reproducibility
  • 11 Quality Assurance and Control 16
  • 11.1 General requirements
  • 11.2 Quality Control
  • 11.3 Method detection limit (MDL) and limit of quantification (LOQ)
  • 12 Test Report
  • Appendix A (Informative) Screening and Verification Test Method Flowchart
  • Appendix B (Informative) Py/T D-GC-MS Instrument Principle
  • Appendix C (Informative) Other test methods
  • Appendix D (Informative) Commercially available standard solutions and substances
  • D.1 Standard solution
  • D.2 Polymer standard substances
  • Appendix E (Informative) Sampling Procedure
  • E.1 Sample preparation using cutting tools

Foreword

This document is in accordance with the provisions of GB/T 1.1-2020 "Guidelines for standardization work Part 1: Structure and drafting rules for standardization documents" Drafting.

This document is part 3-3 of GB/T 39560 "Determination of certain substances in electrical and electronic products". GB/T 39560 has been published the following parts.

--- Part 1: Introduction and overview;

--- Part 2: Disassembly, and mechanical sample preparation;

--- Part 3-1.Screening of lead, mercury, cadmium, total chromium and total bromine by X-ray fluorescence spectrometry;

--- Part 3-2.Screening of fluorine, chlorine and bromine in polymers and electronic components by combustion-ion chromatography (C-IC);

--- Part 3-3.Screening of polybrominated oligomers in polymers by gas chromatography-mass spectrometry with pyrolysis/thermal desorption (Py/TD-GC-MS) benzene, polybrominated diphenyl ethers, and phthalates;

--- Part 4: Determination of mercury in polymers, metals and electronic components by CV-AAS, CV-AFS, ICP-OES and ICP-MS;

--- Part 5: Determination of cadmium, lead, chromium and metals in polymers and electronic components by AAS, AFS, ICP-OES and ICP-MS Cadmium and lead content;

--- Part 6: Determination of polybrominated biphenyls and polybrominated diphenyl ethers in polymers by gas chromatography-mass spectrometry (GC-MS);

--- Part 7-1.Determination of hexavalent chromium [Cr(VI)] in colorless and colored anti-corrosion coatings on metals by hexavalent chromium colorimetry;

--- Part 7-2.Determination of hexavalent chromium [Cr(VI)] in polymers and electronic components by hexavalent chromium colorimetry;

--- Part 8: Gas chromatography-mass spectrometry (GC-MS) and gas chromatography-mass spectrometry with pyrolysis/thermal desorption (Py/TD-GC-MS) MS) determination of phthalates in polymers;

--- Part 9: Determination of hexabromocyclododecane in polymers by gas chromatography-mass spectrometry (GC-MS);

--- Part 10: Determination of polycyclic aromatic hydrocarbons (PAHs) in polymers and electronic components by gas chromatography-mass spectrometry (GC-MS);

--- Part 12: Simultaneous determination of polybrominated biphenyls, polybrominated diphenyl ethers and phthalates by gas chromatography-mass spectrometry (GC-MS).

This document is equivalent to IEC 62321-3-3:2021 "Determination of certain substances in electrical products Part 3-3.Thermal decomposition/thermal decomposition Screening of polybrominated biphenyls, polybrominated diphenyl ethers and phthalates in polymers by Py/TD-GC-MS.

The following minimal editorial changes were made to this document.

--- To be consistent with the existing standard series in my country, the name of the standard is changed to "Determination of Certain Substances in Electrical and Electronic Products Part 3-3 Screening of polybrominated biphenyls and polybrominated Diphenyl ethers and phthalates.

Introduction

The widespread use of electronic and electrical products has made people more concerned about their impact on the environment. Therefore, many countries in the world have revised their Regulations regarding waste disposal, use of restricted substances and energy consumption related to gas products.

GB/T 39560 "Determination of Certain Substances in Electrical and Electronic Products" provides the electrical and electronic industry with a globally consistent standard for the determination of certain substances in electrical and electronic products.

The detection method for restricted substances is a basic and universal standard for the control of hazardous substances in electronic and electrical products.

It consists of 19 parts.

--- Part 1: Introduction and overview. The purpose is to standardize the general process and method of testing restricted substances in electronic and electrical products.

Technical framework, etc.

--- Part 2: Disassembly, and mechanical sample preparation. The purpose is to standardize the disassembly and disassembly of samples in the detection of restricted substances in electronic and electrical products.

The principles, methods and processes of mechanical sample preparation.

--- Part 3-1.Screening of lead, mercury, cadmium, total chromium and total bromine by X-ray fluorescence spectrometry. The purpose is to standardize the X-ray fluorescence spectrometry Methods and procedures for screening and testing five substances, lead, mercury, cadmium, total chromium and total bromine, in electronic and electrical products.

--- Part 3-2.Combustion-ion chromatography (C-IC) screening of fluorine, chlorine and bromine in polymers and electronic components.

Methods and procedures for screening fluorine, chlorine and bromine in polymers and electronic components using C-IC.

--- Part 3-3.Screening of polybrominated oligomers in polymers by gas chromatography-mass spectrometry with pyrolysis/thermal desorption (Py/TD-GC-MS) the purpose is to standardize the use of Py/T D-GC-MS to screen for polybrominated diphenyl ethers and phthalates in polymers.

Methods and procedures for the determination of brominated biphenyls, polybrominated diphenyl ethers and phthalates.

--- Part 3-4.High performance liquid chromatography with ultraviolet detection (HPLC-UV), thin layer chromatography (TLC) and thermal desorption HPLC the purpose is to standardize the use of HPLC-UV, TLC and TD-MS to screen phthalates in polymers.

MS screening test methods and procedures for phthalates in polymers, etc.

--- Part 4: Determination of mercury in polymers, metals and electronic components by CV-AAS, CV-AFS, ICP-OES and ICP-MS. Purpose Aims to standardize the methods and procedures for determining the mercury content in electrical and electronic products.

--- Part 5: Determination of cadmium, lead, chromium and metals in polymers and electronic components by AAS, AFS, ICP-OES and ICP-MS Cadmium and lead content. The purpose is to standardize the methods and procedures for determining the content of cadmium, lead and chromium in electronic and electrical products.

--- Part 6: Determination of polybrominated biphenyls and polybrominated diphenyl ethers in polymers by gas chromatography-mass spectrometry (GC-MS).

Methods and procedures for the determination of polybrominated biphenyls and polybrominated diphenyl ethers in polymers of electrical and electronic products using GC-MS, etc.

--- Part 7-1.Determination of hexavalent chromium [Cr(VI)] in colorless and colored anti-corrosion coatings on metals by hexavalent chromium colorimetry.

It is used to standardize the methods and procedures for the qualitative determination of hexavalent chromium in colorless and colored anti-corrosion coatings on metal samples.

--- Part 7-2.Determination of hexavalent chromium [Cr(VI)] in polymers and electronic components by hexavalent chromium colorimetry.

Methods and procedures for quantitative detection of hexavalent chromium in samples of physical and electronic components.

--- Part 8: Gas chromatography-mass spectrometry (GC-MS) and gas chromatography-mass spectrometry with pyrolysis/thermal desorption (Py/TD-GC-MS) the purpose is to standardize the use of GC-MS and Py/TD-GC-MS to determine phthalates in polymers.

Methods and procedures for measuring the content of phthalates in foods.

--- Part 9: Determination of hexabromocyclododecane in polymers by gas chromatography-mass spectrometry (GC-MS). The purpose is to standardize the use of GC-Method and procedure for determining the hexabromocyclododecane content in polymers by MS, etc.

--- Part 10: Determination of polycyclic aromatic hydrocarbons (PAHs) in polymers and electronic components by gas chromatography-mass spectrometry (GC-MS).

To standardize the methods and procedures for determining the content of PAHs in polymers and electronic components using GC-MS.

--- Part 11: Determination of tri(2-chloro-2-nitropropene) in polymers by gas chromatography-mass spectrometry (GC-MS) and liquid chromatography-mass spectrometry (LC-MS) the purpose is to standardize the method of determining TCEP content in polymers using GC-MS and LC-MS.

Laws and procedures, etc.

--- Part 12: Simultaneous determination of polybrominated biphenyls, polybrominated diphenyl ethers and phthalates by gas chromatography-mass spectrometry (GC-MS). Purpose the purpose is to standardize the methods and procedures for the simultaneous determination of polybrominated biphenyls, polybrominated diphenyl ethers and phthalates using GC-MS.

--- Part 13: Liquid chromatography with diode array detection (LC-DAD), liquid chromatography-mass spectrometry (LC-MS) and liquid chromatography-mass spectrometry (LC-MS) the purpose of this study is to standardize the use of LC-DAD, LC-MS/MS to determine bisphenol A (BPA) in polymers.

Methods and procedures for determining BPA content in polymers using MS and LC-MS/MS, etc.

--- Part 14: Determination of short-chain chlorinated paraffins (SCCP) and medium-chain chlorinated paraffins (MCCP) by gas chromatography-negative chemical ionization mass spectrometry (GC-NCI-MS) Chlorinated paraffins (MCCP). The purpose is to standardize the method and procedure for the determination of SCCP and MCCP content using GC-NCI-MS.

Sequence, etc.

--- Part 15: Determination of tetrabromobisphenol in polymers by gas chromatography-mass spectrometry (GC-MS) and liquid chromatography-mass spectrometry (LC-MS) A(TBBPA). The purpose is to standardize the method and method for determining TBBPA content in polymers using GC-MS and LC-MS Programs, etc.

Determination of Certain Substances in Electrical and Electronic Products Part. Gas chromatography-mass spectrometry with thermal desorption Screening of polymers by Py/TD-GC-MS Polybrominated biphenyls, polybrominated diphenyl ethers and phthalates Warning---People who use this document should have practical experience in formal laboratory work. This document does not address all possible safety issues.

The user is responsible for taking appropriate safety and health measures and ensuring compliance with the conditions stipulated in relevant national laws and regulations.

1 Scope

This document specifies the use of gas chromatography-mass spectrometry with pyrolysis/thermal desorption (Py/TD-GC-MS) for the analysis of polymers in electrical and electronic products.

Polybrominated biphenyls (PBB), polybrominated diphenyl ethers (PBDE), diisobutyl phthalate (DIBP), dibutyl phthalate (DBP), Benzyl butyl phthalate (BBP), di(2-ethylhexyl) phthalate (DEHP), dioctyl phthalate (DNOP), the present invention provides a screening analysis method for diisononyl formate (DINP) and diisodecyl phthalate (DIDP).

It has been tested for decabromodiphenyl ether (100mg/kg~1000mg/kg) and the above-mentioned single phthalates (100mg/kg~ 4000mg/kg) of polypropylene (PP), polystyrene (PS) and polyvinyl chloride (PVC) materials, and the test method was verified.

The method described in this document is used to determine the presence of PBB (monobrominated to decabrominated), PBDE (monobrominated to decabrominated), phthalates in other types of polymers.

No specific verification has been conducted on esters or concentrations outside the above specified range.

2 Normative references

This document has no normative references.

3 Terms, definitions and abbreviations

3.1 Terms and Definitions

The following terms and definitions apply to this document.

The terminology databases used for standardization maintained by ISO and IEC are located at.

3.1.1

Standard material reference material A material that is sufficiently homogeneous and stable in properties and is prepared to be suitable for the measurement or inspection of nominal properties.

[Source. GB/T 39560.1-2020, 3.1.7] 3.1.2 screening an analytical method for determining the presence or absence of certain substances in a representative part or component of a product by comparing the presence, absence and Further testing is performed against the set limit to determine whether the substance is present, absent or requires further testing.

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This preview omits tables, figures, formulas and parts of the technical clauses. The complete document — 39 pages — is available in the English PDF.

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