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GB/T 43832-2024: Textiles - Determination of aniline
---This is an excerpt. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.), auto-downloaded/delivered in 9 seconds, can be purchased online: https://www.ChineseStandard.net/PDF.aspx/GBT43832-2024GB NATIONAL STANDARD OF THE PEOPLE’S REPUBLIC OF CHINA ICS 59.080.01 CCS W 04 Textiles - Determination of aniline Issued on. MARCH 15, 2024 Implemented on. OCTOBER 01, 2024 Issued by. State Administration for Market Regulation; Standardization Administration of the People’s Republic of China.
Table of Contents
Foreword... 3 1 Scope... 4 2 Normative references... 4 3 Terms and definitions... 4 4 Principle... 5 5 Reagents... 5 6 Instruments and equipment... 6 7 Test procedure... 7 8 Result calculation and presentation... 9 9 Quantitation-limit and precision... 10 10 Test report... 10 Appendix A (Informative) Extraction method... 11 Appendix B (Informative) Example of GC-MS analysis conditions... 12 Appendix C (Informative) Example of HPLC-DAD analysis conditions... 14 Bibliography... 16Foreword
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
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 methods3 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) ℃ refrigerator away from light, which has a shelf life of 6 months. 5.10 Standard working solution. aniline concentration 0.5 mg/L ~ 20 mg/L. Accurately pipette an appropriate amount of aniline standard stock solution (5.8). When using GC- MS for determination, add an appropriate amount of naphthalene-d8 internal standard stock solution (5.9) to make the naphthalene-d8 mass concentration 2 mg/L; use dichloromethane (5.2) or tert-butyl methyl ether (5.3) to dilute. When using HPLC- DAD for determination, use acetonitrile (5.4) to dilute. a shelf life of 15 days. 5.11 Naphthalene-d8 dichloromethane internal standard working solution. mass concentration 2 mg/L. Accurately pipette an appropriate amount of naphthalene-d8 internal standard stock solution (5.9); use dichloromethane (5.2) to prepare. Note. Store this solution in a refrigerator at 0 ℃ ~ 4 ℃ away from light, which has a shelf life of 15 days. 5.12 Naphthalene-d8 tert-butyl methyl ether internal standard working solution. mass concentration 2 mg/L. Accurately pipette an appropriate amount of naphthalene-d8 internal standard stock solution (5.9); use tert-butyl methyl ether (5.3) to prepare. Note. Store this solution in a refrigerator at 0 ℃ ~ 4 ℃ away from light, which has a shelf life of 15 days.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). 6.3 Analytical balance. graduation values being 0.01 g and 0.1 mg, respectively. 6.4 Pipette. capacity being 0.2 mL, 0.5 mL, 1 mL, 2 mL, 5 mL and 10 mL, respectively. 6.5 Glass reaction vessel. made of heat-resistant glass, capacity being approximately 30 mL and 60 mL respectively, and provided with a sealing stopper. During the ultrasonic extraction process, the reaction vessel shall be sealed to prevent the evaporation of dichloromethane and shall be able to withstand a pressure of at least 0.2 MPa. 6.6 Ultrasonic generator. operating frequency at (40±5) kHz, capable of controlling temperature at (60±2) ℃. When the test results are consistent, ultrasonic generators of other frequencies can be used. 6.7 Constant temperature water bath heater. capable of controlling the temperature at (40±2) ℃.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). 7.2 Extraction 7.2.1 Free aniline (Method A) Accurately add 10.0 mL of extraction solvent into a sealable glass reaction vessel (6.5). When used for GC-MS analysis, the extraction solvent shall be naphthalene-d8 dichloromethane internal standard working solution (5.11). When used for HPLC-DAD analysis, the extraction liquid shall be dichloromethane (5.2). Seal the reaction container and shake it vigorously to ensure that all samples are immersed in the liquid. Place the reaction container in an ultrasonic generator (6.6) and ultrasonicate at (60±2) °C for (40±5) min. Cool to room temperature; use a disposable syringe (6.9) to take the supernatant; filter through an organic phase needle filter (6.10); analyze using GCMS (6.1). Alternatively, take 1 mL of the filtrate; replace the solvent with acetonitrile; analyze using HPLC-DAD (6.2). Note. If 10 mL of extraction solvent cannot completely immerse the sample, increase the amount of extraction solvent to 20 mL. 7.2.2 Total aniline (Method B) Add 9.0 mL of sodium hydroxide solution (5.13) to a sealable glass reaction vessel (6.5); seal the reaction container; shake vigorously to immerse all the sample in the liquid. Open the bottle cap; add 1.0 mL of sodium dithionite solution (5.14); seal the reaction vessel; shake vigorously to mix the solution thoroughly. Place in a (40±2) ℃ constant temperature water bath heater (6.7) and maintain for (30±1) min. Cool to room temperature within 2 minutes after taking out. Add 2 g of sodium chloride (5.5) to the reaction container; then add 10.0 mL of extraction solvent. When used for GC-MS analysis, the extraction solvent is naphthalene-d8 tert-butyl methyl ether internal standard working solution (5.12). When used for HPLC-DAD analysis, the extraction liquid is tert-butyl methyl ether (5.3). Seal the reaction vessel and shake vigorously to mix. Place in a mechanical oscillator (6.8) and shake for (20±1) min. Allow to stand for two phases to separate; use a disposable syringe (6.9) to take the supernatant; filter it through an organic phase needle filter (6.10); analyze it using GC-MS (6.1); alternatively, take 1 mL of the filtrate; replace the solvent with acetonitrile; analyze it using HPLC-DAD (6.2). Fiber samples dyed with disperse dyes can also be extracted first and then analyzed according to method B. The extraction steps are shown in Appendix A. 7.3 GC-MS analysis method 7.4 HPLC-DAD analysis method 7.4.1 HPLC-DAD analysis conditions Since the test results depend on the instrument used, it is not possible to give universal parameters for chromatographic analysis. The set parameters shall ensure that the component to be measured can be effectively separated from other components during chromatographic determination. Appendix C gives an example of HPLC-DAD analysis conditions. 7.4.2 Qualitative and quantitative analysis Under the same test conditions, take equal volumes of the sample solution (7.2.1 or8 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; c) test date; 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; e) test result; 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 0.01 g); use undyed yarn (A.1.3) to tie it tightly; place it in the extraction device (A.2.1) so that the condensed solvent can flow over the sample. A.3.2 Extraction Add 25 mL of xylene (A.1.1) into the extraction device (A.2.1); extract for 40 minutes; stop the extraction when the reflux reagent on the sample bag turns colorless. After cooling the extract to room temperature, concentrate it to near dryness on a vacuum rotary evaporator (A.2.2) at 45 °C ~ 75 °C. In an ultrasonic generator (A.2.3), use methanol to transfer the residue to the reactor in several times (if the final volume is greater than 2 mL, concentrate to about 2 mL). Dry the extracted sample; cut into pieces of about 5 mm × 5 mm; place them in the above reactor. ......Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
