GB/T 32440.1-2023 Footwear - Chemical tests - Determination of phthalate - Part 1: Solvent extraction
WARNING——The use of this document may involve hazardous materials, operations and equipment. It does not purport to address all of the safety or environmental problems associated with its use. It is the responsibility of users of this document to take appropriate measures to ensure the safety and health of personnel and the environment prior to application of this document, and to determine the applicability of regulatory limitations for this purpose.
1 Scope
This document specifies a test method to determine the qualitative and quantitative presence of phthalate (see Annex A) in footwear and footwear components.
This document is applicable to the determination of phthalate in footwear and footwear components.
Note 1: A list of relevant materials may be found in ISO 21061: 2021, Annex C or in CEN/TR 16417.
Note 2: This test method may also be used to determine phthalates other than those listed in Annex A, subject to validation.
When compared with ISO 16181-2, the two analytical methods shall give similar trends but not necessarily the same absolute result. Therefore, in cases of dispute, the method in this document shall be used in preference to ISO 16181-2.
2 Normative references
The following documents contain provisions which, through reference in this text, constitute provisions 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.
GB/T 12810-2021 Laboratory glassware - Capacity methods testing and use of volumetric instruments (ISO 4787: 2010, NEQ)
3 Terms and definitions
No terms and definitions are listed in this document.
4 Principle
The test sample is extracted using toluene at 60℃ in an ultrasonic bath for 1h. An aliquot is then analyzed using a gas chromatograph (GC) with a mass selective detector (MS).
All the abbreviations of phthalates used are given in Annex A.
5 Reagents
5.1 Chemicals
Unless otherwise specified, use only reagents of recognized analytical grade.
5.1.1 Toluene, CAS No.: 108-88-3.
5.1.2 Internal standard, either of the following chemicals may be used as internal standard:
——Bis(2-Ethylhexyl) phthalates-3,4,5,6-D4 (CAS No.: 93951-87-2);
——Diphenylphthalate (CAS No.: 84-62-8).
Note 1: Diphenylphthalate gives appropriate results in case of DEHP<1%. In case of DEHP>1%, the results of all other phthalates may be affected because of poor resolution between DEHP and Diphenylphthalate.
Note 2: Other internal standards have been found applicable as Di-n-propylphthalate-3,4,5,6-D4 (CAS No.: 358731-29-0).
5.1.3 Phthalates, see Annexes A and B.
5.1.4 Acetone, CAS No.: 67-64-1.
5.1.5 Methanol, CAS No.: 67-56-1.
5.1.6 Cyclohexane, CAS No.: 110-82-7.
5.1.7 Tetrahydrofurane (THF), CAS No.: 109-99-9.
5.1.8 N-hexane, CAS No.: 110-54-3.
5.2 Standard solutions
5.2.1 Target phthalates - Stock solution
Based on its tasks, a laboratory shall decide which phthalates from Table A.1 need to be determined.
Based on this decision, standard stock solution for each phthalate shall be available either as commercially available certified mixes, individual components in solution or self-prepared individual standard stock solutions of each phthalate in toluene.
Foreword i
Introduction iv
1 Scope
2 Normative references
3 Terms and definitions
4 Principle
5 Reagents
6 Apparatus
7 Sampling
8 Test procedure
9 Expression of results
10 Test report
Annex A (Informative) Information on identified phthalates
Annex B (Informative) Information on some identified phthalates
Annex C (Informative) Comparison of extraction of phthalates by using toluene and THF
Annex D (Informative) Suitable gas chromatography-mass spectrometry (GC-MS) apparatus and accuracy data for determination of phthalates
Annex E (Informative) Example of a chromatogram for selected phthalates
Annex F (Informative) Results of the interlaboratories tests – Method using toluene extraction (8.1.1)
Bibliography
GB/T 32440.1-2023 Footwear - Chemical tests - Determination of phthalate - Part 1: Solvent extraction
WARNING——The use of this document may involve hazardous materials, operations and equipment. It does not purport to address all of the safety or environmental problems associated with its use. It is the responsibility of users of this document to take appropriate measures to ensure the safety and health of personnel and the environment prior to application of this document, and to determine the applicability of regulatory limitations for this purpose.
1 Scope
This document specifies a test method to determine the qualitative and quantitative presence of phthalate (see Annex A) in footwear and footwear components.
This document is applicable to the determination of phthalate in footwear and footwear components.
Note 1: A list of relevant materials may be found in ISO 21061: 2021, Annex C or in CEN/TR 16417.
Note 2: This test method may also be used to determine phthalates other than those listed in Annex A, subject to validation.
When compared with ISO 16181-2, the two analytical methods shall give similar trends but not necessarily the same absolute result. Therefore, in cases of dispute, the method in this document shall be used in preference to ISO 16181-2.
2 Normative references
The following documents contain provisions which, through reference in this text, constitute provisions 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.
GB/T 12810-2021 Laboratory glassware - Capacity methods testing and use of volumetric instruments (ISO 4787: 2010, NEQ)
3 Terms and definitions
No terms and definitions are listed in this document.
4 Principle
The test sample is extracted using toluene at 60℃ in an ultrasonic bath for 1h. An aliquot is then analyzed using a gas chromatograph (GC) with a mass selective detector (MS).
All the abbreviations of phthalates used are given in Annex A.
5 Reagents
5.1 Chemicals
Unless otherwise specified, use only reagents of recognized analytical grade.
5.1.1 Toluene, CAS No.: 108-88-3.
5.1.2 Internal standard, either of the following chemicals may be used as internal standard:
——Bis(2-Ethylhexyl) phthalates-3,4,5,6-D4 (CAS No.: 93951-87-2);
——Diphenylphthalate (CAS No.: 84-62-8).
Note 1: Diphenylphthalate gives appropriate results in case of DEHP<1%. In case of DEHP>1%, the results of all other phthalates may be affected because of poor resolution between DEHP and Diphenylphthalate.
Note 2: Other internal standards have been found applicable as Di-n-propylphthalate-3,4,5,6-D4 (CAS No.: 358731-29-0).
5.1.3 Phthalates, see Annexes A and B.
5.1.4 Acetone, CAS No.: 67-64-1.
5.1.5 Methanol, CAS No.: 67-56-1.
5.1.6 Cyclohexane, CAS No.: 110-82-7.
5.1.7 Tetrahydrofurane (THF), CAS No.: 109-99-9.
5.1.8 N-hexane, CAS No.: 110-54-3.
5.2 Standard solutions
5.2.1 Target phthalates - Stock solution
Based on its tasks, a laboratory shall decide which phthalates from Table A.1 need to be determined.
Based on this decision, standard stock solution for each phthalate shall be available either as commercially available certified mixes, individual components in solution or self-prepared individual standard stock solutions of each phthalate in toluene.
Contents of GB/T 32440.1-2023
Foreword i
Introduction iv
1 Scope
2 Normative references
3 Terms and definitions
4 Principle
5 Reagents
6 Apparatus
7 Sampling
8 Test procedure
9 Expression of results
10 Test report
Annex A (Informative) Information on identified phthalates
Annex B (Informative) Information on some identified phthalates
Annex C (Informative) Comparison of extraction of phthalates by using toluene and THF
Annex D (Informative) Suitable gas chromatography-mass spectrometry (GC-MS) apparatus and accuracy data for determination of phthalates
Annex E (Informative) Example of a chromatogram for selected phthalates
Annex F (Informative) Results of the interlaboratories tests – Method using toluene extraction (8.1.1)
Bibliography
