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GB/T 36793-2018: Determination of plasticizers in rubber-plastics -- Gas chromatography-mass spectrometry method
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GB/T 36793-2018: Determination of plasticizers in rubber-plastics -- Gas chromatography-mass spectrometry method

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Determination of platicizers in rubber-plastics - Gas chromatography-mass spectrometry method ICS 83.140.01 G40 National Standards of People's Republic of China Determination of plasticizer content in rubber and plastic materials Gas chromatography-mass spectrometry Published on.2018-09-17 Implementation of.2019-04-01 State market supervision and administration China National Standardization Administration issued

Content

Foreword I 1 Scope 1 2 Principle 1 3 reagents and materials 1 4 Instruments and equipment 2 5 Analysis step 2 5.1 Sample Preparation 2 5.2 Extraction 2 5.3 Blank test 2 5.4 Determination 3 6 result calculation 3 7 Detection of low limit, recovery and precision 4 7.1 Detection low limit 4 7.2 Recovery rate 4 7.3 Precision 4 8 test report 4 Appendix A (informative) 18 phthalate plasticizer information 5 Appendix B (informative) phthalate compound quantitative and qualitative selection ion table 6 Appendix C (informative) Typical phthalate compound standard total ion chromatogram and quantitative selective ion chromatogram 7

Foreword

This standard was drafted in accordance with the rules given in GB/T 1.1-2009. This standard was proposed by the China Petroleum and Chemical Industry Federation. This standard is under the jurisdiction of the National Plastics Standardization Technical Committee General Method and Product Subcommittee (SAC/TC15/SC4). This standard was drafted. Fujian Provincial Product Quality Inspection Institute, Zhonglan Chenguang Chengdu Testing Technology Co., Ltd., National Plastics Volume Supervision and Inspection Center (Fuzhou), Qingdao Entry-Exit Inspection and Quarantine Bureau of the People's Republic of China, Qingdao Science and Technology Inspection and Research Institute Co., Ltd. The main drafters of this standard. He Wei, Zhang Xintao, Gao Jianguo, Huang Yonghui, Wang Yonggui, Wei Linlin, Lin Zhaoliang, Sun Zhuojun, Luo Xiaoxia, Liu Lirong, Lu Huizhi, Song Xiaoyun. Determination of plasticizer content in rubber and plastic materials Gas chromatography-mass spectrometry

1 Scope

This standard specifies phthalate plasticizers in rubber (plastic and plastic) materials (a total of 18, see Appendix A) gas chromatography mass spectrometry The method of measurement used in combination. This standard applies to the determination of phthalate plasticizers (a total of 18 kinds) in rubber and plastic materials, other phthalate plasticizers The measurement can be referred to.

2 Principle

Extraction of phthalate plasticizer in rubber and plastic materials by means of cable extraction, and further enriching the extract as needed After collection and purification, determined by gas chromatography-mass spectrometry (GC-MS), using total ion chromatogram (TIC) and mass spectrometry (MS) Sex, select ion detection (SIM) and external standard method for quantification.

3 reagents and materials

Warning - n-hexane, ether, ethyl acetate are toxic reagents, should be used in a fume hood. Unless otherwise indicated, the reagents used in this method are chromatographically pure (or analytically pure and then re-distillated). Water is made with all-glass installation The distilled water is re-distilled and stored in a glass container. 3.1 n-hexane. 3.2 ether. 3.3 Ethyl acetate. 3.4 Carrier gas. helium (He), purity ≥ 99.999%. 3.5 Phthalates standard. dimethyl phthalate (DMP), diethyl phthalate (DEP), dipropyl phthalate (DPRP), diisobutyl phthalate (DIBP), dibutyl phthalate (DBP), di(2-methoxy) phthalate (DMEP), bis(4-methyl-2-pentyl) phthalate (BMPP), di(2-ethoxy)ethyl phthalate (DEEP), phthalate Dipentyl acid ester (DPP), dihexyl phthalate (DHXP), butyl benzyl phthalate (BBP), bis(2-butoxy) phthalate Ethyl ester (DBEP), dicyclohexyl phthalate (DCHP), di(2-ethylhexyl) phthalate (DEHP), diphenyl phthalate (diphenyl ester), di-n-octyl phthalate (DNOP), diisodecyl phthalate (DINP), diisodecyl phthalate (DIDP). Purity > 95.0%. See Appendix A for information on phthalate plasticizers. 3.6 Standard stock solution. accurately weigh the appropriate amount of phthalate standard, and mix it with n-hexane in a 50mL volumetric flask. A single standard stock solution was prepared at a concentration of 1 mg/mL. Note. The standard stock solution should be stored in the refrigerator at 0 °C ~ 4 °C for a period of 6 months. 3.7 Standard working solution. If necessary, use a stepwise dilution method to prepare a standard working solution of the applicable concentration with n-hexane. Note. The standard working solution should be stored in the refrigerator at 0 °C ~ 4 °C for a period of 3 months. 3.8 Solid phase extraction column (SPE). 1 g of silica gel packing, 6 mL of column tube volume, or equivalent. Activate the cartridge with 5 mL of n-hexane before purging. Keep moist. 3.9 Organic microporous membrane. pore size 0.22μm. ...