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SN/T 5267-2020 English PDFUS$179.00 · In stock
Delivery: <= 3 days. True-PDF full-copy in English will be manually translated and delivered via email. SN/T 5267-2020: (Determination of carragaldehyde in detergents gas chromatography-mass spectrometry) Status: Valid
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SN/T 5267-2020: (Determination of carragaldehyde in detergents gas chromatography-mass spectrometry)---This is a DRAFT version for illustration, not a final translation. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.) will be manually/carefully translated upon your order. Determination of karanal in detergents-Gas chromatography-mass spectrometry The People's Republic of China Entry-Exit Inspection and Quarantine Industry Standards 2020-08-27 release Issued by the General Administration of Customs of the People's Republic of China 2021-03-01 implementation ForewordThis standard was drafted in accordance with the rules given in GB/T 1.1-2009. This standard was proposed and managed by the General Administration of Customs of the People's Republic of China. Drafting organization of this standard. Guangzhou Customs of the People's Republic of China. The main drafters of this standard. Liu Yingfeng, Wang Jing, Wang Chunli, Zhang Zihao, Li Quanzhong, Zhou Minghui, Xiao Qian, Zhai Cuiping, Zheng Jian Guo, Peng Ying, Li Chunyan, Yu Jianlong, Xiao Dahui. Determination of carragaldehyde in detergents Gas chromatography-mass spectrometry1 ScopeThis standard specifies the gas chromatography-mass spectrometry method for the determination of carragaldehyde in detergents. This standard applies to the determination of carragaldehyde in detergents. The lower limit of determination of carragaldehyde in this standard is 100 mg/kg.2 Method summaryThe sample is ultrasonically extracted with methanol, the extract is concentrated and then purified by a solid phase extraction column, filtered by a filter membrane, and combined with gas chromatography-mass spectrometry The instrument is used for determination and the external standard method is used for quantification.3 Reagents and materials3.1 Methanol. chromatographically pure. 3.2 Carragaldehyde (CAS number. 117933-89-8). The purity is greater than 95%. 3.3 Standard stock solution. accurately weigh an appropriate amount of carrageenaldehyde (3.2), dilute to volume with methanol (3.1), and prepare a concentration of 1 000 μg/mL The standard stock solution of carragaldehyde should be stored at 0 ℃~4 ℃. 3.4 Standard working solution. accurately pipette 50 μL, 100 μL,.200 μL, 500 μL, 1 000 μL of the above standard stock solution (3.3) Into five 10 mL volumetric flasks (4.8), make the volume constant with methanol (3.1), and prepare the concentration to be 5 μg/mL, 10 μg/mL, 20 μg/mL, The standard working solutions of 50 μg/mL and 100 μg/mL are ready for use. 3.5 Silica gel cartridge (6 mL, 1 g). activate it with 6 mL methanol (3.1) before use, and keep it wet. 3.6 Organic phase microporous filter membrane. pore size 0.2 μm. 3.7 Quantitative filter paper.4 Apparatus and equipment4.1 Gas chromatograph-mass spectrometer, equipped with EI source. 4.2 Analytical balance. Sensitivity 0.1 mg. 4.3 Ultrasound instrument. 4.4 Rotary evaporator. 4.5 Pipette. 100 μL, 1,000 μL. 4.6 Conical flask with stopper. 25 mL. 4.7 Test tube with stopper. 10 mL. 4.8 Volumetric flask. 10 mL, 25 mL. 4.9 Round bottom flask. 50 mL.5 Analysis steps5.1 Extraction 5.1.1 Soap and powder solid samples Crush the sample to a particle size of less than 2 mm, weigh 0.5 g (accurate to 0.1 mg), and put it into a 25 mL conical flask (4.6) with a stopper. Ultrasonic extraction with 10 mL methanol (3.1) for 30 min. After the extraction is completed, it is filtered through quantitative filter paper (3.7) to a 50 mL round bottom flask (4.9), Use 2 mL methanol (3.1) to rinse the stoppered Erlenmeyer flask (4.6) and the sample, and add the extract. The extract is concentrated with a rotary evaporator (4.4) To close to 1 mL, to be purified. 5.1.2 Liquid samples Accurately weigh 0.5 g (accurate to 0.1 mg) of the sample, put it into a 10 mL test tube (4.7) with a stopper, and use 1 mL of methanol (3.1) to supersede it. Acoustic extraction for 30 minutes, to be purified. 5.2 Purification Transfer the purified solution to the activated silica gel cartridge (3.5), eluting with 6 mL methanol (3.1), collect the eluate, and use methanol (3.1) Dilute the volume to 10 mL, and then filter through the organic phase microporous membrane (3.6) for testing.6 Determination6.1 Reference conditions for gas chromatography-mass spectrometry Since the test results depend on the instrument used, it is impossible to give general parameters for gas chromatography-mass spectrometry. Set parameters It should be ensured that the measured component and other components can be effectively separated during chromatographic determination. The following parameters have been proved to be feasible. a) Chromatographic column. DB-5MS, 30 m×0.25 mm (inner diameter)×0.25 μm (film thickness), or equivalent; b) Column temperature. 120 ℃, keep for 1 min; 10 ℃/min increase to 260 ℃, keep 10 min; 20 ℃/min increase to 290 ℃, Keep for 2 min; c) Temperature of the injection port. 280 ℃; d) Carrier gas. helium, purity ≥ 99.999%, 1.0 mL/min; e) Chromatography-mass spectrometry interface temperature. 300 ℃; f) Ion source temperature. 230 ℃; g) Quadrupole temperature. 150 ℃; h) Ionization method. EI; i) Ionization energy. 70 eV; j) Scanning range. m/z 50~450; k) Measurement method. SCAN mode; l) Injection volume. 1.0 μL, without splitting; m) Solvent delay. 4 min. 6.2 Drawing a standard working curve According to the reference conditions listed in 6.1, the standard working solution (3.4) was determined by gas chromatography-mass spectrometry. Take the measured substance concentration as horizontal Coordinates, with the peak area corresponding to the quantitative ion as the ordinate, draw a standard working curve to obtain a linear equation. Typical carragaldehyde standard Refer to Figure A.1 in Appendix A for the total ion current diagram of solution gas chromatography-mass spectrometry. 6.3 Qualitative and quantitative analysis by gas chromatography-mass spectrometry Analyze the test solution according to the above reference conditions (6.1). According to the retention time of the chromatographic peak, refer to the card in Table B.1 in Appendix B Qualitative analysis was performed on the qualitative ions of lamanthaldehyde. Perform quantitative analysis according to the standard working curve (6.2). 6.4 Blank test Carry out a blank test along with the sample, and perform pre-processing and testing in accordance with the sample processing steps.7 Result calculationThe carragaldehyde content in the sample is calculated according to formula (1).8 PrecisionThe repeatability and reproducibility of the method are shown in Table 1.Appendix A(Informative appendix) Typical total ion chromatogram of carragaldehyde standard solution gas chromatography-mass spectrometry The gas chromatography-mass spectrometry total ion current diagram of a typical carragaldehyde standard solution is shown in Figure A.1. ...... |