GB/T 43832-2024Textiles - Determination of aniline (English PDF)

Foreword

This document was drafted in accordance with the rules given in 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 is not responsible for identifying patents. This document is proposed by China National Textile and Apparel Council. This document shall be under the jurisdiction of National Technical Committee 209 on Textiles of Standardization Administration of China (SAC/TC 209). Drafting organizations of this document. Fujian Fiber Inspection Center, Anhui Optimizing Customized Garment Technology CO. LTD, Xiamen Huaxi Knitting Co., Ltd., Zhejiang Rongda Fashion Technique Co., Ltd., Shaoxing Haicheng Chemical Co., Ltd., Zhejiang Shougu Technology Development Co., Ltd., Chinatesta Textile Testing & Certification Services Co., Ltd., Guangdong Xinhuwei Industrial Investment Co., Ltd. Main drafters of this document. Zhu Feng, Lin Jinmei, Lv Jing, Pan Xingxing, Shen Jianliang, Lin Ningting, Meng Xiaodong, Yan Yaqun, Tian Shusong, Liang Jiajun, Zhang Taoyong. Textiles - Determination of aniline WARNING - The personnel who uses this document shall have hands-on experience in formal laboratory work. This document does not address all possible security issues. It is the responsibility of the user to take appropriate safety and health measures and to ensure compliance with the conditions which are set by the relevant national regulations.

1 Scope

GB/T 43832-2024 gives the determination of aniline in textiles. Aniline is a carcinogen and a residue of azo dyeing: it can be present as free aniline left from manufacture, or bound in the dye and released when the azo bond is reduced, which is the same chemistry that occurs on skin. The standard therefore measures both. Method A extracts free aniline with dichloromethane under ultrasound; method B decomposes the dye with sodium dithionite and extracts the total aniline; either is then measured by gas chromatography-mass spectrometry or by liquid chromatography with diode array detection. The standard sets the principle, the reagents, the instruments and equipment, the test procedure, the calculation and presentation of the result, the quantitation limit and precision, and the test report, with informative annexes on the extraction method and on example GC-MS and HPLC-DAD conditions. It took effect on 1 October 2024.

This document describes the determination of free aniline (Method A) and total aniline (Method B) in textiles. This document applies to all types of textile products.

2 Normative references

The following documents, in whole or in part, are normatively referenced in this document and are indispensable for its application. 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

3 Terms and definitions

For the purposes of this document, the following terms and definitions apply.

3.1 free aniline Aniline in the form of chemical residues.

3.2 cleavable aniline Aniline produced after reductive cleavage.

3.3 total aniline The sum of cleavable aniline and free aniline.

4 Principle

The sample is subjected to ultrasonic extraction of free aniline with dichloromethane (method A), or decomposed by sodium dithionite followed by liquid-liquid extraction to extract the total aniline (method B), and then measured by gas chromatography-mass spectrometry (GC-MS) or high performance liquid chromatography-diode array detector (HPLC-DAD), and quantified by gas chromatography-mass spectrometry internal standard method or high performance liquid chromatography external standard method.

5 Reagents

Unless otherwise specified, all reagents used shall be of analytical grade or above.

5.1 Water. Grade III water in GB/T 6682.Water for chromatography shall comply with Grade I water in GB/T 6682.

5.2 Dichloromethane.

5.3 Tert-butyl methyl ether.

5.4 Acetonitrile, chromatographic reagent.

5.5 Sodium chloride.

5.6 Aniline standard substance/standard sample. CAS No. 62-53-3 (purity not less than 99%).

5.7 Naphthalene-d8 standard substance/standard sample. CAS No. 1146-65-2 (purity not less than 99%).

5.9 Naphthalene-d8 internal standard stock solution. mass concentration not less than 200 mg/L. Accurately weigh naphthalene-d8 standard substance (5.7) and prepare it with dichloromethane (5.2) or tert-butyl methyl ether (5.3).

Note. Store this solution in a (-18±2) °C refrigerator away from light, which has a shelf life of 6 months.

6 Instruments and equipment

6.1 Gas chromatography-mass spectrometer (GC-MS). equipped with electron impact ionization source (EI).

6.2 High performance liquid chromatography (HPLC). equipped with diode array detector (DAD).

7 Test procedure

7.1 Sample preparation Take 5 g ~ 10 g of representative test sample; cut into pieces of about 5 mm × 5 mm. For samples such as yarn, cut into pieces of about 5 mm in length and mix well. Use an analytical balance (6.3) to weigh

1.0 g of sample (accurate to

0.01

g) and place it in a glass reaction vessel (6.5).

8 Result calculation and presentation

Calculate the aniline content according to Formula (1). Round the calculation result to the nearest digit.

9 Quantitation-limit and precision

9.1 Quantitation-limit The quantitation-limit of this method is 5 mg/kg.

9.2 Precision The absolute difference between two test results obtained by the same operator using the same equipment, following the same test method and independently conducting on the same object within a short period of time shall not exceed 10% of the arithmetic mean of the two measured values.

10 Test report

The test report shall at least give the following contents.

a) a reference to this document;

b) sample source and description;

d) method used [free aniline (method A), total aniline (method B)], the pre- treatment method, if using the method (extraction method) in Appendix A, must be indicated;

f) details of any deviation from this document.

Appendix A

(Informative) Extraction method A.1 Reagents and materials A.1.1 Xylene. analytical reagent. A.1.2 Methanol. analytical reagent. A.1.3 Undyed yarn. A.2 Instruments and apparatuses A.2.1 Extraction device. using the extraction device specified in GB/T 17592. A.2.2 Vacuum rotary evaporator. A.2.3 Ultrasonic generator. operating frequency (40±5) kHz. A.2.4 Analytical balance. graduation value

0.01 g. A.2.5 Pipette. capacity 25 mL. A.3 Test procedure A.3.1 Sample pretreatment Take a representative sample; cut it into pieces of about 40 mm × 5 mm or other strips of suitable size; mix well. Weigh

1.0 g of sample (accurate to