GB/T 36922-2018 PDF EnglishUS$150.00 · In stock · Download in 9 seconds
GB/T 36922-2018: Determination of organophosphorus flame retardants in toys - Gas chromatometry-mass spectrometry method Delivery: 9 seconds. True-PDF full-copy in English & invoice will be downloaded + auto-delivered via email. See step-by-step procedure Status: Valid
Similar standardsGB/T 36922-2018: Determination of organophosphorus flame retardants in toys - Gas chromatometry-mass spectrometry method---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/GBT36922-2018 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 ContentsForeword ... 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 ScopeThis 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 PrincipleUse 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 materials3.1 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 conditions6 Result calculationIf 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 andprecision 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%. ......Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al. 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