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GB/T 45277-2025 PDF English

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GB/T 45277-2025: Determination of nine primary aromatic amines in toys - Gas chromatography-mass spectrometry
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GB/T 45277-2025260 Add to Cart Auto, 9 seconds. Determination of nine primary aromatic amines in toys - Gas chromatography-mass spectrometry Valid

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GB/T 45277-2025: Determination of nine primary aromatic amines in toys - Gas chromatography-mass spectrometry


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GB NATIONAL STANDARD OF THE PEOPLE’S REPUBLIC OF CHINA ICS 97.200.50 CCS Y 57 Determination of nine primary aromatic amines in toys -- Gas chromatography-mass spectrometry Issued on: FEBRUARY 28, 2025 Implemented on: FEBRUARY 28, 2025 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... 4 5 Reagent and materials... 5 6 Instruments... 5 7 Sample preparation... 6 8 Test steps... 6 9 Result calculation... 9 10 Quantification limit and recovery rate of the method... 10 11 Test report... 10 Annex A (normative) 9 primary aromatic amines... 11 Annex B (informative) Qualitative and quantitative information of 9 primary aromatic amines... 12 Annex C (informative) Total ion chromatogram of 9 primary aromatic amines... 13 Bibliography... 14

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". Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. The issuing authority shall not be held responsible for identifying any or all such patent rights. This document was proposed by China Light Industry Federation. This document shall be under the jurisdiction of National Technical Committee on Toys of Standardization Administration of China (SAC/TC 253). The drafting organizations of this document. Hangzhou Vocational and Technical College, Nanjing Customs Light Industry Products and Children's Products Testing Center, Zhejiang Product Quality and Safety Science Research Institute, National Cultural and Educational Supplies Quality Supervision and Inspection Center, Yike Testing and Certification Co., Ltd., Mingmen (China) Preschool Products Co., Ltd., Shantou Quality and Metrology Supervision and Testing Institute in Guangdong Province, Guangzhou Inspection and Testing Certification Group Co., Ltd., Aofei Entertainment Co., Ltd., Zhongjiayuan (Beijing) Testing and Certification Co., Ltd., Beijing Zhongqinglian Certification Center Co., Ltd., Hangzhou Food and Drug Inspection Science Research Institute, Huace Testing and Certification Group Co., Ltd., Shandong Product Quality Inspection and Research Institute, Zhejiang Fangyuan Testing Group Co., Ltd., Yiwu Product (Commodity) Quality Inspection and Research Institute, Shenzhen Metrology and Quality Inspection Research Institute. The sentence is. Guangzhou Customs Technology Center, Shanghai Customs Mechanical and Electrical Product Testing Technology Center, Bijie Vocational and Technical College. Main drafters of this document. Chen Dewen, Wu Min, Li Hongyan, Qian Zhijuan, Hu Dan, Tian Xuling, Li Jiong, Hu Na, Hu Aisheng, Chen Qinxue, Yang Jianying, Yang Fengbo, Lu Xuanben, Lv Shan, He Yi, Yang Yang, Wang Hua, Gong Xudong, Lin Xiaowei, Yang Danhua, Gao Huan, Yang Sen. Determination of nine primary aromatic amines in toys -- Gas chromatography-mass spectrometry WARNING -- The personnel using this document shall have practical experience working in a formal laboratory. This document does not indicate all possible security issues. Users are responsible for taking appropriate safety and health measures and ensuring compliance with relevant national regulations.

1 Scope

This document describes the gas chromatography-mass spectrometry method for the determination of nine primary aromatic amines in toy materials, including aniline, ortho toluidine, 2-methoxyaniline, 4-chloroaniline, 2-naphthylamine, benzidine, 3,3'- dimethylbenzidine, 3,3' - dichlorobenzidine, and 3,3 '- dimethoxybenzidine. This document applies to toy parts and materials such as textiles, leather, wood, paper, liquids, flexible molding materials, etc. that contain coloring agents (including dyes and pigments). This document is not applicable to finger painting pigments.

2 Normative references

The following referenced documents are indispensable for the application of this document. 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

There are no terms or definitions that need to be defined in this document.

4 Principle

Extract the specimen by ultrasonic extraction with an appropriate solvent. Conduct purification and concentration through a diatomaceous earth column. Set it to a set volume. Use gas chromatography-mass spectrometry for determination. Qualify based on its retention time and characteristic ions. Quantify with external standard method.

5 Reagent and materials

5.1 Water. GB/T 6682, Grade three water. 5.2 Methanol. chromatographically pure. 5.3 Tert butyl methyl ether. chromatographically pure. 5.4 9 primary aromatic amine standard substances/standard samples. according to the requirements of Annex A, the purity is greater than 98%. 5.5 Standard stock solution (1000 μg/mL or higher concentration). prepare the above standard substance/sample (5.4) into a standard stock solution using methanol (5.2) or other suitable solvents. Accurately weigh to 0.1 mg. NOTE. Standard stock solution is stored in brown bottles. Store at -18℃. It shall be valid for 3 months. 5.6 Mixed standard working solution. dilute the standard reserve solution (5.5) step by step with methanol (5.2) or other suitable solvents to prepare a series of mixed standard working solutions with mass concentrations of 0.2 μg/mL, 0.5 μg/mL, 1.0 μg/mL, 2.5 μg/mL, and 5.0 μg/mL, respectively. NOTE. As needed, it can be prepared to other suitable concentrations. 5.7 Diatomaceous earth. Porous granular, burned at 600℃ for 4 h. After cooling, store in a dryer for later use.

6 Instruments

6.1 Gas chromatography-mass spectrometer (equipped with EI ionization source). 6.2 Analytical balance. precision is 0.1 mg. 6.3 Vortex oscillator. speed range is from 0 r/min~3000 r/min. 6.4 Ultrasonic extractor. capable of internal or external temperature control. The effective power density range of ultrasound is 0.25 W/cm2~2.0 W/cm2. Example. For an ultrasonic extractor with a total power of 1200 W (including 200 W ultrasonic effective power and 1000 W heating power), the water bath area is 400 cm2, and the ultrasonic effective power density is 0.50 W/cm2 (=200 W/400 cm2). 6.5 Centrifuge. centrifugal force is (5000 ± 500) g. 6.6 Diatomaceous earth column. a glass or polypropylene column with an inner diameter of 25 mm~30 mm and a length of 130 mm~150 mm. Fill approximately 20 g NOTE. Excessive flow rate during elution can lead to incomplete extraction of aromatic amines, resulting in low recovery rates. 8.1.2 Clay and crystal clay specimens Weigh 1 g of the specimen to the nearest 0.1 mg. Place it in a 50 mL centrifuge tube. First, add 2 mL~3 mL of methanol (5.2) and mix thoroughly. Add a certain volume of water to make the total volume 15 mL. Vortex in a vortex oscillator (6.3) for 30 s. After mixing, use an ultrasonic extractor (6.4) to extract for 15 min at room temperature. When necessary, centrifuge for 5 min using a centrifuge (6.5) with a centrifugal force of (5000 ± 500) g. Transfer all the supernatant into a diatomaceous earth column (6.6). Adsorb for 20 min. Wash twice with tert butyl methyl ether, 40 mL each time. The flow rate shall be controlled to form droplets during elution. Collect tert butyl methyl ether eluent in a round bottom flask with a standard grinding mouth or a glass container suitable for vacuum rotary evaporator (6.7). 8.2 Concentration Place the round bottom flask containing the elution solution of tert butyl methyl ether collected above on a vacuum rotary evaporator (6.7). Concentrate to about 5 mL under low vacuum conditions at (35 ± 2)℃. Then transfer to a nitrogen blower (6.8). Blow nitrogen to near dryness at room temperature (do not blow dry). Immediately and accurately transfer 1.0 mL of methanol (5.2) or other suitable solvent into a nearly dry round bottom flask. After vortex mixing, filter with a 0.45 μm filter membrane (6.9). The obtained specimen solution shall be analyzed on the machine in a timely manner. 8.3 Blank test Each batch of samples shall undergo a method blank test. Using the same testing procedure as the sample test, except without adding samples. The results of the blank test can be used to evaluate the contamination experienced during the testing process. The blank test result shall be less than the quantification limit of the method (10.1). 8.4 Analysis and determination 8.4.1 Analysis reference conditions Due to the fact that the test results depend on the instrument used, it is not possible to provide universal parameters for chromatographic analysis. The following operating conditions have been proven to be suitable for the test results. a) Chromatography column. 5% benzyl polysiloxane chromatography column, 30 m × 0.25 mm × 0.25 μm, or equivalent; b) Injection port temperature. 280℃; c) Heating program. initial temperature is 60℃, maintain for 1 min; heat up to 300℃ at a rate of 15℃/min and maintain for 5 min; d) Carrier gas. helium, purity ≥ 99.999%; e) Flow rate. 1.0 mL/min; f) Split ratio. 10.1; g) Injection volume. 1 μL; h) Transmission line temperature. 250℃; i) Ion source. EI source; j) Ion source temperature. 280℃; k) Fourth level rod temperature. 150℃; l) Ionization energy. 70 eV; m) Measurement method. (50~350) m/z full scan mode (SCAN); select ion monitoring (SIM) for quantification; n) Solvent delay time. 3.5 min. The qualitative and quantitative information of 9 primary aromatic amines can be found in Annex B. The total ion chromatogram can be found in Annex C. 8.4.2 Qualitative analysis According to the measurement conditions in 8.4.1, take 1 μL of the specimen solution and test it on the machine. Qualitative analysis is conducted by comparing the retention time of primary aromatic amines and the relative abundance of characteristic ions (see Table B.1) in the specimen and mixed standard working solution (5.6). The following conditions can be used to determine whether the specimen contains the corresponding primary aromatic amine. a) The deviation between the retention time of primary aromatic amines in the specimen and the retention time of primary aromatic amines in the mixed standard working solution is within ± 0.5%; b) Characteristic ions appear at the retention time of primary aromatic amines in mixed standard working solutions; c) The relative abundance of characteristic ions is consistent with the relative abundance of primary aromatic amines in the mixed standard working solution (when the relative abundance is >50%, a deviation of ±10% is allowed; when the relative abundance is between 20%~50%, a deviation of ± 15% is allowed; when the relative abundance is between>10%~< 20%, a deviation of ± 20% is allowed; when the relative abundance is ≤ 10%, a deviation of ± 50% is allowed). ......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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