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GB/T 36922-2018 Related PDF English

GB/T 36922-2018 (GB/T36922-2018, GBT 36922-2018, GBT36922-2018) & related versions
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GB/T 36922-2018 NATIONAL STANDARD OF THE PEOPLE’S REPUBLIC OF CHINA ICS 97.200.50 Y 57 Determination of organophosphorus flame retardants in toys - Gas chromatometry-mass spectrometry method ISSUED ON: DECEMBER 28, 2018 IMPLEMENTED ON: DECEMBER 28, 2018 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 Principle ... 4  3 Reagents and materials ... 4  4 Instruments and devices ... 5  5 Analysis steps ... 5  6 Result calculation ... 8  7 Lower limit of quantitation, recovery rate and precision ... 8  8 Test report ... 9  Annex A (informative) Chromatogram of organic phosphorus flame retardant ... 10  Annex B (informative) Precision ... 11  Bibliography ... 12  Determination of organophosphorus flame retardants in toys - Gas chromatometry-mass spectrometry method WARNING - Personnel using this Standard shall have practical experience in formal laboratory work. This Standard does not indicate all possible safety issues. It is the user's responsibility to take appropriate safety and health measures and to ensure compliance with the conditions prescribed by the relevant national regulations. 1 Scope This Standard specifies gas chromatometry-mass spectrometry method for three organic phosphorus flame retardants: tris(2-chloroethyl) phosphate (TCEP), tris(1,3-dichloroisopropyl) phosphate (TDCP) and tris(2-chloro-1- methylethyl) phosphate (TCPP) in toys. This Standard is applicable to determination of organic phosphorus flame retardant in polymer materials in toys. 2 Principle Use toluene to extract TCEP, TDCP and TCPP in the sample in Soxhlet extractor. After setting the volume of the extract, use gas chromatography-mass spectrometry (GC-MS) to determine. Use external standard method to quantify. 3 Reagents and materials 3.1 Toluene. 3.2 TCEP standard product: purity is not less than 97%. 3.3 TDCP standard product: purity is not less than 97%. 3.4 TCPP standard: purity not less than 95%. 3.5 Standard stock solution: Accurately weigh TCEP standard products (see 3.2), TDCP standard products (see 3.3) and TCPP standard products (see 3.4). Use toluene (see 3.1) to prepare 1000mg/L stock solution. Take test solution. Filter through the membrane filter (see 4.3). Conduct gas chromatography-mass spectrometry analysis. Soxhlet extraction process: The temperature shall be controlled at the reflux temperature of toluene, about 110°C. Rotary evaporator water bath temperature is 40°C ~ 50°C. At the same time, keep the pressure between 5 kPa~8 kPa. 5.4 Gas chromatometry-mass spectrometry method 5.4.1 GC-MS determination conditions Different GC-MS has different analysis parameters. The set parameters shall ensure that the measured component can be effectively separated from other components during the measurement. The following parameters are one of the GC-MS measurement conditions: a) Chromatography column: HP-5MS column, 30m×0.25mm×0.25μm, or equivalent; b) Inlet temperature: 300°C; c) Chromatography-mass spectrometer interface temperature: 280°C; d) Sampling method: pressure-splitless injection. Apply a pressure of 344.75kPa. Open the valve after 1.0min; e) Carrier gas: helium, purity ≥99.999%; control mode: constant flow; flow rate: 1.8mL/min; f) Temperature programming: After maintaining at 80°C for 2min, raise to 160°C at 20°C/min. Maintain 1min. Then raise to 320°C at 40°C/min. Maintain 2min; g) Injection volume: 1μL; h) Ion source: EI source; i) Ionization energy: 70eV; j) Scanning method: Select ion monitoring (SIM); k) Quadrupole temperature: 150°C; l) Ion source temperature: 230°C; m) Solvent delay time: 3min. The chromatogram of each standard under the above measurement conditions 6 Result calculation If it is determined that TCEP, TDPP, and TCPP are present, perform external standard quantitative analysis based on the extracted ion chromatographic peak area. The content of TCEP, TDPP and TCPP in the sample is calculated according to formula (1): Where, Xi - The content of organic phosphorus flame retardant in the sample, in milligrams per kilogram (mg/kg); CS - The concentration of organic phosphorus flame retardant in the test solution, in milligrams per liter (mg/L); V - The set volume of toluene, in milliliters (mL); D - The dilution factor; m - The mass of test material, in grams (g). Calculate the concentration of organic phosphorus flame retardant in the sample according to the above formula. If the test response value of the test solution exceeds the linear range, it shall be appropriately diluted and measured. The result is kept to one decimal place. 7 Lower limit of quantitation, recovery rate and precision 7.1 Lower limit of quantitation The three organic phosphorus flame retardant methods have a lower limit of 1mg/kg. 7.2 Recovery rate Quantitatively add an appropriate standard solution of known concentration to the sample. Perform recovery rate analysis according to the above test steps 5.2~5.4. The recovery rate of TCEP, TDPP and TCPP in the polymer shall be 85%~110%. ......

BASIC DATA
Standard ID GB/T 36922-2018 (GB/T36922-2018)
Description (Translated English) Determination of organophosphorous flame retardants in toys -- Gas chromatography-mass spectrography method
Sector / Industry National Standard (Recommended)
Classification of Chinese Standard Y57
Classification of International Standard 97.200.50
Word Count Estimation 10,171
Date of Issue 2018-12-28
Date of Implementation 2018-12-28
Drafting Organization Mechanical and Electrical Products Testing Technology Center of Shanghai Entry-Exit Inspection and Quarantine Bureau of the People's Republic of China, Toys and Children's Products Laboratory of Inspection and Quarantine Technology Center of Guangdong Entry-Exit Inspection and Quarantine Bureau of the People's Republic of China, Shanghai Quality Supervision and Inspection Technology Research Institute, Shenzhen Metrology Quality Inspection Research Institute, Shenzhen Tianxiang Quality Technology Service Co., Ltd., National Daily Commodity Quality Supervision and Inspection Center, Zhejiang Fangyuan Testing Group Co., Ltd., Jiangsu Yike Testing Technology Service Co., Ltd., Beijing Zhongqinglian Certification Center
Administrative Organization National Toy Standardization Technical Committee
Proposing organization China Light Industry Federation