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GB/T 46183-2025: Footwear - Chemical tests - Determination of chlorinated phenols - GC-MS/MS
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GB/T 46183-2025: Footwear - Chemical tests - Determination of chlorinated phenols - GC-MS/MS

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ICS 61.060 CCSY78 National Standards of the People's Republic of China Chemical testing methods for footwear. Determination of chlorophenol content Gas chromatography-tandem mass spectrometry Published on 2025-08-29 Implemented on 2026-03-01 State Administration for Market Regulation The State Administration for Standardization issued a statement.

Foreword

This document complies with the provisions of GB/T 1.1-2020 "Standardization Work Guidelines Part 1.Structure and Drafting Rules of Standardization Documents". Drafting. Please note that some content in this document may involve patents. The issuing organization of this document assumes no responsibility for identifying patents. This document was proposed by the China National Light Industry Council. This document is under the jurisdiction of the National Technical Committee on Standardization of Footwear (SAC/TC305). This document was drafted by. Yierkang Co., Ltd., Wenzhou Municipal Institute of Quality and Technical Inspection, and China Leather and Footwear Industry Research Institute. Research Institute (Jinjiang) Co., Ltd., Jinhou Group Weihai Shoes Co., Ltd., China Leather and Footwear Research Institute Co., Ltd., China Light Industry Inspection and Certification Co., Ltd. company. The main drafters of this document are. Wei Xiaochun, Shan Erkang, Chang Wenkai, Cai Zhenhua, Wang Ning, Zhang Xiaomei, Meng Ziyan, Wang Zhi, and Yang Yang. Chemical testing methods for footwear. Determination of chlorophenol content Gas chromatography-tandem mass spectrometry Warning---Personnel using this document should have practical experience working in a formal laboratory. This document does not address all possible safety issues. Users are responsible for taking appropriate safety and health measures and ensuring compliance with relevant national regulations. 1.Scope This document describes a method for the determination of chlorophenols in footwear and footwear components by gas chromatography-tandem mass spectrometry (GC-MS/MS). This document applies to the determination of chlorophenol content in textiles, leather, fur, synthetic leather, and artificial leather materials used in footwear and footwear components. The determination of chlorophenol content in other materials has been verified and is carried out in accordance with this document.

2 Normative references

The contents of the following documents, through normative references within the text, constitute essential provisions of this document. Dated citations are not included. For references to documents, only the version corresponding to that date applies to this document; for undated references, the latest version (including all amendments) applies. This document. GB/T 6682 Specifications and test methods for water used in analytical laboratories 3.Terms and Definitions This document does not contain any terms or definitions that need to be defined. 4.Principles Chlorinated phenol in the sample was extracted by ultrasonic extraction with methanol-potassium hydroxide solution, followed by acetylation with acetic anhydride, extraction with n-hexane, and then gas chromatography. The determination was performed using chromatographic-tandem mass spectrometry (GC-MS/MS), and quantification was performed using the internal standard method. 5.Reagents or materials 5.1 General. Unless otherwise specified, all reagents used shall be of analytical grade and the water used in the tests shall meet at least the requirements of Grade III water as specified in GB/T 6682. 5.2 Potassium hydroxide, purity ≥ 85.0%. 5.3 Potassium hydroxide aqueous solution, 2.0 mol/L. 5.4 Anhydrous sodium sulfate, purity ≥99.0%, dried at 400℃ or above for no less than 4 hours, cooled and placed in a desiccator for later use. 5.5 Acetic anhydride, purity ≥98.5%. 5.6 Methanol. Analytical grade reagents should be used for sample extraction, and chromatographic grade reagents should be used for the preparation of standard substances/standard samples. 5.7 n-Hexane, chromatographic grade. 5.8 Chlorophenol (CP) standard substances/standard samples, purity ≥95%. Detailed information on the 19 CPs is provided in Appendix A. 5.9 2-Chlorophenol-d4, CAS No.. 93951-73-6, purity ≥94%, internal standard. 5.10 2,4-Dichlorophenol-d3, CAS No.. 93951-74-7, purity ≥94%, internal standard. 5.11 2,3,4,6-Tetrachlorophenol-13C6, CAS No.. 1246820-81-4, purity ≥94%, internal standard. 5.12 Pentachlorophenol-13C6, CAS No.. 85380-74-1, purity ≥94%, internal standard. 5.13 CP Stock Solution. Prepare CP standard substances/standard samples listed in Table A.1 with methanol (5.6) to a concentration of [missing value]. A stock solution of 1000 mg/L. 5.14 CP Mixed Working Solution (10 mg/L). Transfer an appropriate amount of CP stock solution (5.13) and prepare a solution with methanol (5.6) to a concentration of [missing value]. A mixed working solution of 10 mg/L. 5.15 CP Mixed Working Solution (1 mg/L). Transfer an appropriate amount of CP mixed working solution (10 mg/L) (5.14) and prepare it with methanol (5.6). Prepare a mixed working solution with a mass concentration of 1 mg/L. 5.16 Internal standard stock solution (100 mg/L). Prepare internal standard substances (5.9~5.12) with methanol (5.6) to a mass concentration of 100 mg/L. Internal standard stock solution. 5.17 Internal Standard Stock Solution (10 mg/L). Transfer an appropriate amount of the internal standard stock solution (5.16) and dissolve it in methanol (5.6) to prepare a solution with a mass concentration of [missing value]. 10 mg/L internal standard mixed stock solution. 5.18 Methanol solution containing internal standard. Transfer an appropriate amount of the internal standard mixed stock solution (10 mg/L) (5.17), and prepare a solution of a certain mass with methanol (5.6). A methanol solution containing an internal standard at a concentration of (e.g., 0.05 mg/L). 6.Instruments and Equipment 6.1 Gas chromatography-tandem mass spectrometry (GC-MS/MS) equipped with an electron impact ionization source (EI source). 6.2 Analytical balance, scale division 0.0001g. 6.3 Ultrasonic extractor, temperature adjustable to (70±3)℃, working frequency up to (40±5)kHz. 6.4 Centrifuge. 6.5 Mechanical oscillator, with an oscillation frequency ≥.200 times/min, or other suitable oscillation device. 6.6 A closed container capable of separating the organic phase and the aqueous phase, such as a 40 mL glass bottle with a sealable screw cap. 6.7 Vortex mixer. 6.8 Sample vials. 6.9 Volumetric flasks. 6.10 Organic microporous filter membrane, pore size 0.22μm. 7.Experimental Procedure 7.1 Sample Preparation The specimens were made from a single material from the shoe and were prepared with a diameter (side length) not exceeding 4 mm. 7.2 Sample Extraction Weigh 1.0 g (accurate to 1 mg) of the sample into a sealed container (6.6), add 10 mL of potassium hydroxide aqueous solution (5.3) and 10 mL of solution containing... The internal standard methanol solution (5.18) was sealed tightly and placed in an ultrasonic extractor (6.3) at (70±3)℃ for ultrasonic extraction (120±5) min. The extraction result was obtained. Cool to room temperature after beam treatment. 7.3 Acetylation Add 2.5 mL of acetic anhydride (5.5) to the extract after treatment according to 7.2, and vortex on a vortex mixer (6.7) for about 1 min. Add 5.0 mL of n-hexane (5.7), place on a mechanical shaker (6.5) and shake for (30±3) min. After standing and separating into layers, take the upper layer solution and use the added... An appropriate amount of anhydrous sodium sulfate (5.4) was filtered through an organic microporous membrane (6.10) into a sample vial (6.8) for GC-MS/MS (6.1) analysis. If necessary... To separate the upper layer of solution, centrifuge the solution in a centrifuge (6.4), and then take the n-hexane layer to perform the above steps. 7.4 Preparation of Standard Working Solutions Accurately transfer an appropriate amount of CP mixed working solution into a sealed container (6.6), add 10 mL of potassium hydroxide aqueous solution (5.3) and 10 mL of... Acetylation was performed using a methanol solution containing internal standard (5.18) following step 7.3.For example, accurately transfer 50 μL and.200 μL of the CP mixed working solution. Acetylation was performed on a mixture of 1 mg/L (5.15) and 50 μL, 100 μL, and.200 μL of a CP working solution (10 mg/L) (5.14) to obtain a mass... CP standard working solutions with concentrations of 10 μg/L, 40 μg/L, 100 μg/L,.200 μg/L, and 400 μg/L (with an internal standard concentration of 100 μg/L for all solutions). Note. Select an appropriate concentration point to establish a standard curve, and adjust the concentration range of the standard working solution according to the chlorophenol content level in the actual sample. 7.5 Gas Chromatography-Tandem Mass Spectrometry (GC-MS/MS) Determination The determination was performed using a gas chromatography-tandem mass spectrometer (GC-MS/MS) (6.1), and the instrument conditions given in Appendix B have been proven to be feasible. Examples of chromatographic analysis are shown in Appendix C. 7.6 Blank Test A blank test must be performed for each batch of tests. Follow steps 7.2 to 7.3, except without adding a sample. 8.Experimental Data Processing 8.1 Calibration Curve Establish a linear regression function based on equation (1). As Ais= a× Cs Cis b (1) In the formula. As --- the peak area of CP in the standard working solution; Ais --- Peak area of the internal standard in the standard working solution; a --- The slope of the calibration curve; Cs --- The mass concentration of CP in the standard working solution, expressed in micrograms per liter (μg/L); Cis --- The mass concentration of the internal standard in the standard working solution, expressed in micrograms per liter (μg/L); b --- The ordinate intercept of the calibration curve. Calculate the mass concentration Css of each CP in the sample solution according to formula (2). CSS= Cis a × As Ais- ÷ (2) In the formula. Css --- The mass concentration of CP in the sample solution, expressed in micrograms per liter (μg/L); Cis --- The mass concentration of the internal standard in the sample solution, expressed in micrograms per liter (μg/L); a --- The slope of the calibration curve; As --- Peak area of CP in the sample solution; Ais --- Peak area of the internal standard in the sample solution; b --- The ordinate intercept of the calibration curve. 8.2 Calculation of CP content results The mass concentration Css of CP was obtained from the calibration curve. The content Xi of each CP in the sample was calculated according to Equation (3). The calculation results were retained to the nearest whole number. Two digits after the point. ...