固体进样-电子电气产品中三(2-氯乙基)磷酸酯的热解析-气质联用法测定  

Determination of Tris(2-chloroethyl) Phosphate in Solid Sampling-Electronic and Electrical Products by TD-GC-MS

作　　者：李彬[1] 黄略略[1] 谢堂堂[2] Li Bin;Huang Luelue;Xie Tangtang(Shenzhen Techno-vocational College,Shenzhen 518055,China;Shenzhen Entry-Exit Inspection and Quarantine Bureau,Shenzhen 518045,China)

机构地区：[1]深圳职业技术学院,广东深圳518055 [2]深圳出入境检验检疫局,广东深圳518045

出　　处：《塑料科技》2018年第12期110-113,共4页Plastics Science and Technology

基　　金：深圳职业技术学院校级重点课题(601722K27006);深圳职业技术学院科研平台项目(GGJS20130331152344401);国家质检总局科技计划项目(2017IK249)

摘　　要：基于裂解仪中低温热解析功能,打开样品大分子基体,释放出高沸点小分子有毒有害物质三(2-氯乙基)磷酸酯(TCEP),并在线联用GC-MS对TCEP进行定性及定量分析。所建方法可对固体样品直接进样,无需任何使用有机溶剂的前处理过程,方法快速、准确和环境友好。文中对裂解器热解析工作条件(热解析温度、热解析时间、升温速率和附件初温)进行了优化,并测试了线性和精密度,线性范围200~1 000 mg/kg,检测下限为30 mg/kg,方法RSD小于15%,能很好地应用于电子电气产品中TCEP的定性及定量测定。Based on the thermal desorption function of the pyrolysis instrument, the large molecular matrix was opened and tris(2-chloroethyl) phosphate (TCEP), a small molecule toxic and harmful substance with high boiling point was released. And then TCEP was qualitatively and quantitatively analyzed by GC-MS on-line. In this method, solid samples can be directly injected without any pre-treatment process with organic solvent. The method is accurate, fast and environmentally friendly. The working conditions of thermal desorption (such as thermal analysis temperature, time, heating rate and appendix temperature) were optimized, and the linearity and precision were tested. The results show that the linear range is between 200~1000 mg/kg, the detection limit was 30 mg/kg, and the relative standard deviation was less than 15%. The method can be well applied to the determination of TCEP in electronic and electrical products.

关 键 词：固体进样 热解析-气质联用法 三(2-氯乙基)磷酸酯 电子电气产品 

分 类 号：TQ320.772[化学工程—合成树脂塑料工业]