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GB/T 40909-2021: Textiles - Determination of methylcyclosiloxane residues 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 40909-2021: Textiles - Determination of methylcyclosiloxane residues---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/GBT40909-2021GB NATIONAL STANDARD OF THE PEOPLE’S REPUBLIC OF CHINA ICS 59.080.01 CCS W 04 Textiles - Determination of methylcyclosiloxane residues ISSUED ON: OCTOBER 11, 2021 IMPLEMENTED ON: MAY 01, 2022 Issued by: State Administration for Market Regulation; Standardization Administration of the People’s Republic of China. Table of ContentsForeword ... 3 1 Scope ... 4 2 Normative references ... 4 3 Terms and definitions ... 4 4 Principle ... 4 5 Reagents or materials ... 4 6 Instruments and equipment ... 5 7 Test procedures ... 6 8 Result calculation and expression ... 8 9 Quantitation-limit and precision ... 8 10 Test report ... 9 Appendix A (Informative) Gas chromatography-mass spectrometry analysis conditions ... 10 Textiles - Determination of methylcyclosiloxane residues 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 ScopeThis document describes the test methods for the determination of octamethylcyclotetrasiloxane (D4), decamethylcyclopentasiloxane (D5) and dodecamethylcyclohexasiloxane (D6) residues in textiles by gas chromatograph-mass spectrometer (GC-MS). This document applies to all types of textiles.2 Normative referencesThere are no normative references in this document.3 Terms and definitionsThere are no terms and definitions that need to be defined in this document.4 PrincipleUse organic solvent to ultrasonically extract the residual methylcyclosiloxane in the textile sample; for the extract after purification, use the gas chromatograph-mass spectrometer for determination and the internal standard method for quantitation.5 Reagents or materialsUnless otherwise specified, all the reagents shall, at least, be analytical reagents. 5.1 n-hexane: CAS No. 110-54-3. 5.2 Tetrahydrofuran: CAS No. 109-99-9. 5.3 Methylcyclosiloxane standard substance: see 5.3.1 ~ 5.3.3. 5.3.1 Octamethylcyclotetrasiloxane (D4): CAS No. 556-67-2, purity ≥98.0%. 5.3.2 Decamethylcyclopentasiloxane (D5): CAS No. 541-02-6, purity ≥98.0%. 5.3.3 Dodecamethylcyclohexasiloxane (D6): CAS No. 540-97-6, purity ≥98.0%. 5.4 Tetramethylsiloxysilane (Trimethylsiloxysilane) (M4Q): CAS No. 3555-47-3, purity ≥98.0%, internal standard (IS). 5.5 Standard stock solution: Use a balance (6.1) to weigh a certain amount of standard substance (5.3); use n-hexane (5.1) to dissolve it and fix volume, to prepare a single- component or mixed standard stock solution of a concentration of 1 000 mg/L. Note: The standard stock solution, which is stored in a refrigerator at 0 °C ~ 4 °C, is valid for 6 months. 5.6 Internal standard stock solution: Use the balance (6.1) to accurately weigh the internal standard substance (5.4); use n-hexane (5.1) to dissolve it and fix volume, to prepare an internal standard stock solution of a concentration of 500 mg/L. Note: The internal standard stock solution, which is stored in a refrigerator at 0 °C ~ 4 °C, is valid for 6 months. 5.7 Mixed standard working solution: Accurately draw an appropriate amount of standard stock solution (5.5) and internal standard stock solution (5.6); use n-hexane (5.1) to prepare a 10.0 mg/L mixed standard working solution. The concentration of internal standard in the mixed standard working solution is 5.0 mg/L. This solution is prepared for immediate use. Other appropriate concentrations can also be used as required. 5.8 Internal standard working solution. 5.8.1 n-hexane internal standard working solution: Use n-hexane (5.1) and internal standard stock solution (5.6) to prepare a n-hexane internal standard working solution of a concentration of 5.0 mg/L. This solution is prepared for immediate use. Other appropriate concentrations can also be used as required. 5.8.2 Tetrahydrofuran internal standard working solution: Use tetrahydrofuran (5.2) and internal standard stock solution (5.6) to prepare a tetrahydrofuran internal standard working solution of a concentration of 5.0 mg/L. This solution is prepared for immediate use. Other appropriate concentrations can also be used as required.6 Instruments and equipment6.1 Balance: the division value is 0.1 mg. 6.2 Extraction bottle: 40 mL ~ 60 mL, made of hard glass, equipped with a screw cap.Appendix A(Informative) Gas chromatography-mass spectrometry analysis conditions A.1 Gas chromatograph-mass spectrometer parameters Since the test results depend on the instrument used, it is impossible to give general parameters for instrumental analysis. The following parameters have been shown to be suitable for testing: a) Chromatographic column: TG-5SilMS, 30.0 m × 0.25 mm × 0.25 μm, or equivalent; b) Column temperature: maintain the initial column temperature at 30 °C for 3 min; rise the temperature to 150 °C at 40 °C/min; rise to 300 °C at 60 °C/min; maintain for 5 min; c) Injection volume: 1 μL; d) Inlet septum: Merlin micro-seal septum; e) Injection port temperature: 200 °C; f) Temperature of chromatography mass spectrometry interface: 280 °C; g) Ion source temperature: 250 °C; h) Carrier gas: helium; purity ≥99.999%; flow rate: 1.0 mL/min; i) Injection method: splitless injection; j) Ionization mode: EI; k) Ionization energy: 70 eV; l) Solvent delay: 5 min; m) Mass spectrometry scanning mode: For qualitative analysis, adopt full scan mode (SCAN), with the scanning mass (m/z) of 50~450; for quantitative analysis, adopt selected monitoring ion mode (SIM), where the selected monitoring ions are shown in Table A.1. ......Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al. |
