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GB/T 45043-2024 PDF English

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GB/T 45043-2024: Textiles - Determination of adipate esters - Gas chromatography-mass spectrometry method

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GB NATIONAL STANDARD OF THE PEOPLE'S REPUBLIC OF CHINA ICS 59.080.01 CCS W 04 Textiles - Determination of adipate esters - Gas chromatography-mass spectrometry method Issued on. DECEMBER 31, 2024 Implemented on. JULY 1, 2025 Issued by. State Administration for Market Regulation; Standardization Administration of PRC.

Foreword... 3 1 Scope... 4 2 Normative references... 4 3 Terms and definitions... 4 4 Principle... 4 5 Reagents... 5 6 Instruments and equipment... 5 7 Test steps... 6 8 Result calculation and presentation... 7 9 Limit of quantitation and precision... 7 10 Test report... 8 Appendix A (Informative) Basic information on 5 adipate esters... 9 Appendix B (Informative) Gas chromatography-mass spectrometry analysis conditions ... 10 Appendix C (Informative) Total ion current chromatogram of 5 adipate ester standard substances... 12

Foreword

This document was drafted in accordance with the provisions of GB/T 1.1-2020 Directives for standardization - Part 1.Rules for the structure and drafting of standardizing documents. Please note that some of the contents of this document may involve patents. The issuing organization of this document does not assume the responsibility for identifying patents. This document was proposed by the China National Textile and Apparel Council. This document is under the jurisdiction of the National Technical Committee on Textiles of Standardization Administration of China (SAC/TC209). Drafting organizations of this document. Chengdu Customs District Technology Center, Urumqi Customs District, Zhejiang Shengshan Technology Textile Co., Ltd., Chinatesta Textile (Shenzhen) Testing & Certification Services, Xiamen Huaxi Knitting Co., Ltd., Shaoxing Feisuo Textile Technology Co., Ltd., Chinatesta Textile Testing & Certification Services, Tan Kah Kee Innovation Laboratory, Ningbo Customs District Technology Center, Guangzhou Customs District Technology Center, Tianjin Physical and Chemical Analysis Center Co., Ltd., Hangzhou Qianyang Technology Co., Ltd., Zhejiang Changshan Textile Co., Ltd., United Testing Services (Dongguan) Co., Ltd., and Shaoxing Customs Comprehensive Technical Service Center. Main drafters of this document. Liu Jun, Li Yongli, Zhang Yi, Su Youzhi, Si Ying, Dong Wei, Xie Tangtang, Xu Weizhong, Huang Liming, Chen Qinyong, Bei Zhongjie, Xu Chaojie, Lan Lili, Chen Qinwei, Li Haitao, Zhu Guoquan, Ran Yao. Textiles - Determination of adipate esters - Gas chromatography-mass spectrometry method WARNING -- People who use this document shall have practical experience in regular laboratory work. This document does not point out all possible safety issues. Users are responsible for taking appropriate safety and health measures and ensuring that the conditions stipulated by relevant national laws and regulations are met.

1 Scope

This document describes a method for the determination of five adipate esters in textiles by gas chromatography-mass spectrometry. This document is applicable to the determination of the content of 5 types of adipate esters in various textile products.

2 Normative references

The provisions of the following documents constitute the essential clauses of this document through normative references in this text. Among them, for referenced documents with dates, only the versions corresponding to the dates are applicable to this document; for referenced documents without dates, the latest versions (including all amendments) are applicable to this document. GB/T 8170 Rules of rounding off for numerical values & expression and judgment of limiting values GB/T 10629 Textiles - Preparation of laboratory test samples and test specimens for chemical testing

3 Terms and definitions

There are no terms or definitions that require definition in this document.

4 Principle

The test specimen is extracted with tetrahydrofuran by the ultrasonic method and then precipitated with a suitable solvent (acetonitrile, n-hexane). After centrifugation, the extract is detected by gas chromatography-mass spectrometer for 5 types of adipate esters, including diethyl adipate (DEA), diisobutyl adipate (DIBA), dibutyl adipate (DBA), bis(2-butoxyethyl) adipate (BBOEA) and bis(2-ethylhexyl) adipate (DEHA), which are quantified by using the external standard method.

5 Reagents

5.1 Tetrahydrofuran. chromatographic grade. 5.2 Precipitant. acetonitrile or n-hexane, chromatographic grade. 5.3 Adipate ester standards. The basic information of the five adipate ester compounds is shown in Appendix A. The purity of all of them is ≥98%. 5.4 Standard stock solution. Weigh appropriate amounts of adipate ester standards (5.3) (accurate to 0.1 mg) and prepare 1000 μg/mL stock solutions with a precipitant (5.2). The standard stock solutions should be stored in a refrigerator at 0 ℃~4 ℃ away from light and have a shelf life of 6 months. 5.5 Standard working solution. Take appropriate amounts of standard stock solutions (5.4) of various adipate esters, and dilute into at least 5 mixed standard working solutions of appropriate concentrations using a mixture of tetrahydrofuran (5.1) and precipitant (5.2) (volume ratio of 1.2) as solvent as needed. The standard working solutions should be stored in a refrigerator at 0 ℃～4 ℃ away from light, and the validity period is 1 month.

6 Instruments and equipment

6.1 Gas Chromatography-Mass Spectrometer (GC-MS). It is equipped with an electron impact ionization source (EI). 6.2 Balance. Graduation values are 0.1 mg and 0.01 g. 6.3 Extraction bottle. with an airtight stopper, 50 mL, made of hard glass. 6.4 Ultrasonic generator. The operating frequency is 40 kHz±5 kHz. 6.5 Vortex mixer.

7 Test steps

7.1 Test specimen preparation and extraction Take a sufficient amount of representative sample according to the method described in GB/T 10629, cut it into pieces with a maximum size of no more than 5 mm, mix it, weigh 1.0 g (accurate to 0.01 g) from it using a balance (6.2) as the test specimen; place it in a 50 mL extraction bottle (6.3), add 10 mL of tetrahydrofuran (5.1), extract it in an ultrasonic generator (6.4) at 60 ℃ for 30 min, let it stand, and cool it to room temperature. Use a pipette (6.8) to add 20 mL of precipitant (5.2) dropwise to the extraction bottle (6.3). Vortex it on a vortex oscillator (6.5) for at least 30 s, let it stand for 30 min, centrifuge it at 3000 r/min for 5 min, filter the supernatant through a 0.45 μm organic phase filter membrane (6.6), and then test it on the machine. 7.2 Qualitative analysis Under the same experimental conditions, take equal volumes of the sample solution (7.1) and the standard working solution (5.5) for injection and measurement, and refer to the gas chromatography-mass spectrometry analysis conditions in Appendix B for test and analysis. 7.3 Quantitative analysis Under the same determination conditions, the standard working curve is drawn with the concentration of the standard solution as the abscissa and the peak area of the quantitative ion as the ordinate. The content of the analyte in the test specimen is calculated by the external standard method. The target response value in the sample solution shall be within the linear range of the instrument detection. If the target Relative ion abundance/%

8 Result calculation and presentation

Calculate the content of each adipate ester in the test specimen according to formula (1). The calculation result shall be rounded to one decimal place in accordance with GB/T 8170.

9 Limit of quantitation and precision

9.1 Limit of quantitation 9.2 Precision In the same laboratory, the same operator uses the same equipment, according to the same test method, and conducts independent tests on the same object within a short period of time; the absolute difference between two independent test results shall not be greater than 15% of the arithmetic mean of the two measured values, and the premise is that the probability of exceeding the 15% of the arithmetic mean of the two measured values does not exceed 5%.

10 Test report

The test report shall at least include the following. a) The number of this document; b) Source and description of the sample; c) Analytical instruments used; d) Test results; e) Any details that deviate from this document; f) Date of the test.

Appendix A

(Informative) Basic information on 5 adipate esters Table A.1 gives the basic information on the Chinese and English names, CAS numbers, molecular formulas and relative molecular masses of five adipate esters.

Appendix B

(Informative) Gas chromatography-mass spectrometry analysis conditions B.1 Chromatographic conditions Since the test results depend on the instrument used, it is not possible to give universal parameters for chromatographic analysis. The parameters set shall ensure that the component being measured can be effectively separated from other components during chromatographic determination. The parameters given below have proven to be feasible. a) Chromatographic column. HP-5MS capillary column, 30 m (column length) × 0.25 mm (inner diameter) × 0.25 μm (film thickness), or equivalent. b) Injection port temperature. 280 °C. c) Injection mode. splitless injection. d) Column temperature program. hold at 100 °C for 2 min, increase to 200 °C at 10 °C/min, then increase to 280 °C at 20 °C/min and hold for 10 min. e) Carrier gas. helium, with a purity of ≥99.999% and a flow rate of 1.0 mL/min. f) Injection volume. 1.0 μL. B.2 Mass spectrometry conditions Since the test results depend on the instrument used, it is not possible to give universal parameters for chromatographic analysis. The parameters set shall ensure that the component being measured can be effectively separated from other components during chromatographic determination. The parameters given below have proven to be feasible.

Appendix C

(Informative) Total ion current chromatogram of 5 adipate ester standard substances Figure C.1 shows the total ion current chromatogram of five adipate ester standard substances. ......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.