GB/T 45043-2024Textiles—Determination of adipate esters—Gas chromatography-mass spectrometry method (English PDF)

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

GB/T 8170

GB/T 10629

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.

6 Instruments and equipment

7 Test steps

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

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 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 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) x 0.25 mm (inner diameter) x 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 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. ......