GB/T 24153-2009 PDF English
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GB/T 24153-2009: Rubber and Elastomer Materials - Determination of N-nitrosaminess
---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/GBT24153-2009GB NATIONAL STANDARD OF THE PEOPLE’S REPUBLIC OF CHINA ICS 83.060 G 40 Rubber and Elastomer Materials – Determination of N-nitrosamines Issued on. JUNE 15, 2009 Implemented on. FEBRUARY 1, 2010 Issued by. General Administration of Quality Supervision, Inspection and Quarantine; Standardization Administration of PRC.
Table of Contents
Foreword... 3 1 Scope... 4 2 Principle... 4 3 Reagents and Materials... 4 4 Apparatus... 5 5 Analytical Procedures... 5 6 Result calculation... 7 7 Determination Lower Limit... 7 8 Test Report... 7 Appendix A (Normative) 12 Types of N-Nitrosamines Names and their GC/MS Selective Quantitative Ions... 9 Appendix B (Informative) N-Nitrosamines Standard Products’ GC/MS Total Ion Flow Diagram... 10Foreword
This Standard’s Appendix A is normative; while Appendix B is informative. This Standard was proposed by China Petroleum and Chemical Industry Association. This Standard shall be under the jurisdiction of National Technical Committee for Standardization of Rubber and Rubber Products (SAC/TC 35). Drafting organizations of this Standard. Fujian Putian Entry-Exit Inspection and Quarantine Bureau, Shenyang Rubber Research and Design Institute, and Fujian Quanzhou Entry-Exit Inspection and Quarantine Bureau. Chief drafting staffs of this Standard. Tong Yugui, Cheng Qun, Lin Bifen, Li Yijun, Liu Huichun, and Lin Zhong. Rubber and Elastomer Materials – Determination of N-nitrosamines Warning. personnel using this Standard shall have practical working experience in the formal laboratory. This Standard doesn’t indicate all possible laboratory work. The users shall take responsibility to take appropriate safety and health measures; and ensure compliance with the conditions set forth in the relevant national regulations.1 Scope
This Standard specifies adopting gas chromatography – mass selective detector (GC- MSD) to determine 12 types of N-nitrosamines (see Appendix A) contents in the rubber and elastomer. This Standard is applicable to the rubber, elastomer materials and their products.2 Principle
The sample was extracted by methanol; after concentrating, the extracting solution passes through C18 solid-phase extraction column to purify; the sample solution enters into the gas chromatography – mass selective detector (GC-MSD) to be measured; qualified by full-scanning detection; select ions to quantify by external standard method.3 Reagents and Materials
Unless otherwise is specified, all the reagents used are chromatographic pure. 3.1 Methanol, the blank test check there are no interfering substances. 3.2 C18 solid-phase extraction column. 500mg/3mL. 3.3 Standard stock solution. separately and accurately weigh the appropriate amount of each N-nitrosamines standard products; use methanol to prepare the standard stock solution with concentration of 200mg/L; inject into the brown reagent bottle; store in the refrigerator at 5°C below; and valid for 3 months.4 Apparatus
4.1 Gas chromatograph. equipped with mass selective detector (MSD). 4.2 Ultrasonic generator. operating frequency of 40kHz. 4.5 Vortex mixer. 4.6 Conical flask. brown, with ground stopper, 100mL. 4.7 Concentrated bottle. brown, 150mL. 4.8 Centrifuge tube. brown, 10mL.5 Analytical Procedures
5.1 Specimen preparation and extraction Take the representative sample, use appropriate tool to cut it into particles with edges of 3mm below, mix evenly. 5.2 Purification Place C18 solid-phase extraction column (3.2) onto the solid-phase extraction apparatus (4.4), use 5mL of methanol to pre-leach C18 column; discard the effluent. 5.3 Determination 5.3.1 Determination condition of gas chromatography-mass spectrometry Since the test results depend on the apparatus used, the general parameters for chromatographic analysis can’t be given. The operating parameters given below have been shown to be feasible, which only serve as reference for measurement. 5.3.2 Qualitative and quantitative analysis of gas chromatography-mass spectrometry Separately take 1µL standard working solution (3.4) and sample solution (5.2), inject into the chromatograph for determination. If there is a chromatogram peak at the same retention time in the total ion flow diagram of sample solution and standard working solution, qualify through comparing the characteristic ions of sample and standard products; use the selective ion monitoring method to perform the external standard method.6 Result calculation
Each N-nitrosamines content in the sample shall be calculate as per Formula (1).7 Determination Lower Limit
The determination lower limit of this method is 0.5mg/kg.8 Test Report
The test report shall give the following contents at least. ......Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
