GB/T 36929.1-2026 Leather and fur—Determination of per-and polyfluoroalkyl substances—Part 1:Determination of non-volatile compounds by liquid chromatography (English)
GB/T 36929.1-2026 Leather and fur - Determination of per-and polyfluoroalkyl substances - Part 1: Determination of non-volatile compounds by liquid chromatography
WARNING —— The use of this document involves hazardous materials. 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 fulfil the relevant requirements for this purpose.
1 Scope
This document describes the method for the determination of non-volatile per- and polyfluoroalkyl substances (PFAS) in leather and fur by liquid chromatography-tandem mass spectrometry (LC-MS/MS).
This document is applicable to the determination of non-volatile per- and polyfluoroalkyl substances (PFAS) in leather, fur and their products by LC-MS/MS.
Note: See Annex D for the types of PFAS substances.
2 Normative references
The following documents contain requirements 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 6682 Water for analytical laboratory use - Specification and test methods (GB/T 6682-2008, ISO 3696:1987, MOD)
GB/T 39364 Leather - Chemical, physical, mechanical and fastness tests - Sampling location (GB/T 39364-2020, ISO 2418: 2017, MOD)
QB/T 1267 Fur - Chemical, physical and mechanical and fastness tests - Sampling location
QB/T 1272 Fur - Preparation of chemical test samples
QB/T2262 Terminology of leather industry
QB/T 2716 Leather - Preparation of chemical test samples
3 Terms and definitions
For the purposes of this document, the terms and definitions given in GB/T 2262 apply.
4 Rationale
In an ultrasonic bath, leather or fur test specimens are extracted with methanol in the specified conditions, and the PFAS substances in the extract are analyzed and determined by LC-MS/MS.
Note 1: If the test specimen contains perfluoropolymers that release fluorotelomer alcohols (FTOH) due to transesterification with the extraction solvent methanol, the method described in this document cannot accurately quantify the concentration of free FTOH in the test specimen.
Note 2: For degradable perfluoropolymers that can generate PFOA and contain a linear or branched perfluoroheptyl group with a (C7F15)C structural element, e.g., polymers containing 2-perfluorooctylethanol (8:2 FTOH, CAS No. 678-39-7) bonded as esters, to determine whether these perfluoropolymers are intentionally present, it could be necessary to introduce an alkaline hydrolysis method to remove the 8:2 FTOH side-chain from the polymer. In addition, other FTOH, e.g., 6:2 FTOH or 10:2 FTOH, will be released from relevant perfluoropolymers by alkaline hydrolysis.
5 Reagents and materials
5.1 Unless otherwise specified, analytically-pure reagents are adopted. Water, grade 1 (according to GB/T6682).
5.2 Methanol, chromatographically pure;
5.3 Ammonium acetate: CAS number 631-61-8, superior grade pure.
5.4 PFAS stock solutions, prepared using PFAS reference standards/reference materials with a purity greater than 95%. Weigh 10 mg of PFAS standard sample/reference material separately into a 10 mL volumetric flask, dilute to volume with methanol (5.2), and then dilute 1,000-fold with methanol (5.2) to obtain a stock solution with a mass concentration of 1,000 μg/L. It may also be obtained by diluting commercially available solutions.
5.5 PFAS standard solutions: dilute PFAS stock solution (5.4) with methanol (5.2) to prepare PFAS standard solutions with a mass concentration of 25 μg/L. Commercially available solutions with concentrations and solvents conforming to the requirements of this document may also be used directly.
5.6 Internal standard solution I, 2,000 μg/L, prepared by diluting the commercially available internal standard solution with methanol (5.2). At least two internal standards suitable for the analysis of perfluorooctane sulfonic acid (PFOS) and perfluorooctanoic acid (PFOA) shall be used. Prior to the use of a new internal standard for each batch, it is necessary to determine its impurity levels. Suitable internal standards are as follows:
——13Cx-PFOA (e.g., perfluoro[1,2,3,4-13 C4] octanoic-acid, CAS No. 960315-48-4);
——13Cx-PFOS (e.g., sodium perfluoro-1-[1,2,3,4-13C4] octanesulfonate, CAS No. 960315-53-1).
5.7 Internal standard solution II (for the preparation of standard working solutions), 100 μg/L, prepared by diluting the commercially available internal standard solution with methanol (5.2).
5.8 PFAS standard working solution, at least 5 of appropriate concentrations, prepared using methanol (5.2), PFAS standard solution (5.5), and internal standard solution II (5.7). Table 1 give the examples of standard working solutions.
Table 1 Examples of standard working solutions
Mass concentration /(μg/mL) 0.25 0.5 1 2.5 5 10
Volume of methanol /μL 940 930 910 850 750 550
Volume of standard solution at 25μg/L /μL 10 20 40 100 200 400
Volume of internal standard solution II at 100μg/L /μL 50 50 50 50 50 50
5.9 LC-MS/MS mobile phase: 10 mmol/L ammonium acetate solution is prepared by dissolving 0.771 g of ammonium acetate (5.3) in 1,000 ml deionized water (5.1).
5.10 Internal standard extraction solution: prepare Internal standard extraction solution with an internal standard mass concentration of 10 μg/L by diluting internal standard solution I (5.6) in methanol (5.2), for test specimen extraction.
6 Instruments and apparatus
6.1 General provisions: Equipment or any accessible part of it that could come into contact with the sample or the extract shall be free from interfering compounds listed in Annex E. The equipment used shall not contain any fluoropolymers, including polytetrafluoroethylene (PTFE). Instruments and equipment made of polypropylene (PP) or polyethylene (PE) may be used. Rinse all test instruments and accessible parts of the extraction apparatus with methanol (5.2). Sample containers shall be rinsed thoroughly with water (5.1) and methanol (5.2) before use.
6.2 Cutter, with a sharp blade to cut leather specimen.
6.3 Volumetric flask, made of polypropylene (PP) or polyethylene (PE), with an inert stopper.
6.4 Extraction vials, suitable PP or PE vials, volume at least 20 ml and able to be used in a centrifuge.
Contents
Foreword i
Introduction iii
1 Scope
2 Normative references
3 Terms and definitions
4 Rationale
5 Reagents and materials
6 Instruments and apparatus
7 Sampling and preparation of specimens
8 Test procedure
9 Calculation and expression of results
10 Method feasibility
11 Test report
Annex A (Informative) Comparison of clause/subclause numbers between this document and ISO 23702-1: 2023
Annex B (Informative) Technical differences between this document and ISO 23702-1: 2023 and their justifications
Annex C (Informative) PFAS substance categories and applications
Annex D (Informative) PFAS substances
Annex E (Informative) Interferences
Annex F (Informative) LC-MS/MS conditions
Annex G (Informative) Usable ions and possible quantification limits for PFAS analysis by LC-MS/MS
Annex H (Informative) Accuracy
GB/T 36929.1-2026 Leather and fur—Determination of per-and polyfluoroalkyl substances—Part 1:Determination of non-volatile compounds by liquid chromatography (English)
Standard No.
GB/T 36929.1-2026
Status
to be valid
Language
English
File Format
PDF
Word Count
17000 words
Translation Price(USD)
510.0
Implemented on
2027-2-1
Delivery
via email in 1 business day
Detail of GB/T 36929.1-2026
Standard No.
GB/T 36929.1-2026
English Name
Leather and fur—Determination of per-and polyfluoroalkyl substances—Part 1:Determination of non-volatile compounds by liquid chromatography
GB/T 36929.1-2026 Leather and fur - Determination of per-and polyfluoroalkyl substances - Part 1: Determination of non-volatile compounds by liquid chromatography
WARNING —— The use of this document involves hazardous materials. 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 fulfil the relevant requirements for this purpose.
1 Scope
This document describes the method for the determination of non-volatile per- and polyfluoroalkyl substances (PFAS) in leather and fur by liquid chromatography-tandem mass spectrometry (LC-MS/MS).
This document is applicable to the determination of non-volatile per- and polyfluoroalkyl substances (PFAS) in leather, fur and their products by LC-MS/MS.
Note: See Annex D for the types of PFAS substances.
2 Normative references
The following documents contain requirements 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 6682 Water for analytical laboratory use - Specification and test methods (GB/T 6682-2008, ISO 3696:1987, MOD)
GB/T 39364 Leather - Chemical, physical, mechanical and fastness tests - Sampling location (GB/T 39364-2020, ISO 2418: 2017, MOD)
QB/T 1267 Fur - Chemical, physical and mechanical and fastness tests - Sampling location
QB/T 1272 Fur - Preparation of chemical test samples
QB/T2262 Terminology of leather industry
QB/T 2716 Leather - Preparation of chemical test samples
3 Terms and definitions
For the purposes of this document, the terms and definitions given in GB/T 2262 apply.
4 Rationale
In an ultrasonic bath, leather or fur test specimens are extracted with methanol in the specified conditions, and the PFAS substances in the extract are analyzed and determined by LC-MS/MS.
Note 1: If the test specimen contains perfluoropolymers that release fluorotelomer alcohols (FTOH) due to transesterification with the extraction solvent methanol, the method described in this document cannot accurately quantify the concentration of free FTOH in the test specimen.
Note 2: For degradable perfluoropolymers that can generate PFOA and contain a linear or branched perfluoroheptyl group with a (C7F15)C structural element, e.g., polymers containing 2-perfluorooctylethanol (8:2 FTOH, CAS No. 678-39-7) bonded as esters, to determine whether these perfluoropolymers are intentionally present, it could be necessary to introduce an alkaline hydrolysis method to remove the 8:2 FTOH side-chain from the polymer. In addition, other FTOH, e.g., 6:2 FTOH or 10:2 FTOH, will be released from relevant perfluoropolymers by alkaline hydrolysis.
5 Reagents and materials
5.1 Unless otherwise specified, analytically-pure reagents are adopted. Water, grade 1 (according to GB/T6682).
5.2 Methanol, chromatographically pure;
5.3 Ammonium acetate: CAS number 631-61-8, superior grade pure.
5.4 PFAS stock solutions, prepared using PFAS reference standards/reference materials with a purity greater than 95%. Weigh 10 mg of PFAS standard sample/reference material separately into a 10 mL volumetric flask, dilute to volume with methanol (5.2), and then dilute 1,000-fold with methanol (5.2) to obtain a stock solution with a mass concentration of 1,000 μg/L. It may also be obtained by diluting commercially available solutions.
5.5 PFAS standard solutions: dilute PFAS stock solution (5.4) with methanol (5.2) to prepare PFAS standard solutions with a mass concentration of 25 μg/L. Commercially available solutions with concentrations and solvents conforming to the requirements of this document may also be used directly.
5.6 Internal standard solution I, 2,000 μg/L, prepared by diluting the commercially available internal standard solution with methanol (5.2). At least two internal standards suitable for the analysis of perfluorooctane sulfonic acid (PFOS) and perfluorooctanoic acid (PFOA) shall be used. Prior to the use of a new internal standard for each batch, it is necessary to determine its impurity levels. Suitable internal standards are as follows:
——13Cx-PFOA (e.g., perfluoro[1,2,3,4-13 C4] octanoic-acid, CAS No. 960315-48-4);
——13Cx-PFOS (e.g., sodium perfluoro-1-[1,2,3,4-13C4] octanesulfonate, CAS No. 960315-53-1).
5.7 Internal standard solution II (for the preparation of standard working solutions), 100 μg/L, prepared by diluting the commercially available internal standard solution with methanol (5.2).
5.8 PFAS standard working solution, at least 5 of appropriate concentrations, prepared using methanol (5.2), PFAS standard solution (5.5), and internal standard solution II (5.7). Table 1 give the examples of standard working solutions.
Table 1 Examples of standard working solutions
Mass concentration /(μg/mL) 0.25 0.5 1 2.5 5 10
Volume of methanol /μL 940 930 910 850 750 550
Volume of standard solution at 25μg/L /μL 10 20 40 100 200 400
Volume of internal standard solution II at 100μg/L /μL 50 50 50 50 50 50
5.9 LC-MS/MS mobile phase: 10 mmol/L ammonium acetate solution is prepared by dissolving 0.771 g of ammonium acetate (5.3) in 1,000 ml deionized water (5.1).
5.10 Internal standard extraction solution: prepare Internal standard extraction solution with an internal standard mass concentration of 10 μg/L by diluting internal standard solution I (5.6) in methanol (5.2), for test specimen extraction.
6 Instruments and apparatus
6.1 General provisions: Equipment or any accessible part of it that could come into contact with the sample or the extract shall be free from interfering compounds listed in Annex E. The equipment used shall not contain any fluoropolymers, including polytetrafluoroethylene (PTFE). Instruments and equipment made of polypropylene (PP) or polyethylene (PE) may be used. Rinse all test instruments and accessible parts of the extraction apparatus with methanol (5.2). Sample containers shall be rinsed thoroughly with water (5.1) and methanol (5.2) before use.
6.2 Cutter, with a sharp blade to cut leather specimen.
6.3 Volumetric flask, made of polypropylene (PP) or polyethylene (PE), with an inert stopper.
6.4 Extraction vials, suitable PP or PE vials, volume at least 20 ml and able to be used in a centrifuge.
Contents of GB/T 36929.1-2026
Contents
Foreword i
Introduction iii
1 Scope
2 Normative references
3 Terms and definitions
4 Rationale
5 Reagents and materials
6 Instruments and apparatus
7 Sampling and preparation of specimens
8 Test procedure
9 Calculation and expression of results
10 Method feasibility
11 Test report
Annex A (Informative) Comparison of clause/subclause numbers between this document and ISO 23702-1: 2023
Annex B (Informative) Technical differences between this document and ISO 23702-1: 2023 and their justifications
Annex C (Informative) PFAS substance categories and applications
Annex D (Informative) PFAS substances
Annex E (Informative) Interferences
Annex F (Informative) LC-MS/MS conditions
Annex G (Informative) Usable ions and possible quantification limits for PFAS analysis by LC-MS/MS
Annex H (Informative) Accuracy
