精己二酸中金属杂质元素的分析  

Analysis of Metal Impurities in Purified Adipic Acid by Inductively Coupled Plasma Mass Spectrometry

作　　者：赵风轩 王焕哲 陈涛 谢华林[2] ZHAO Fengxuan;WANG Huanzhe;CHEN Tao;XIE Hualin(Chongqing Huafeng Chemical Co.Ltd.,Fuling 421002,China;College of Chemistry and Chemical Engineering,Yangtze Normal University,Fuling 408100,China)

机构地区：[1]重庆华峰化工有限公司,重庆涪陵408100 [2]长江师范学院化学化工学院,重庆涪陵408100

出　　处：《化工技术与开发》2018年第4期53-56,共4页Technology & Development of Chemical Industry

基　　金：重庆市高校优秀成果转化资助项目(KJZH17131);重庆市涪陵区科委计划项目(FLKJ 2016AAA1005)

摘　　要：建立了精己二酸中金属杂质元素的分析方法。精己二酸用2%(V/V)的硝酸溶解后,采用电感耦合等离子体质谱(ICP-MS)法直接测定其中的Cr、Fe、As、Cd、Sb、Hg、Pb。针对样品溶液中的基质元素所形成的多原子离子干扰,采用八极杆碰撞/反应池(ORS)技术,向ORS中通入He气体。与无气体模式比较,利用氦碰撞模式消除干扰,明显降低了各元素的背景等效浓度和检出限。各元素仪器的检出限为0.86~32.5 ng·L-1。采用加标回收实验验证了方法的准确性,各元素的回收率在93.6%~107.6%之间。样品处理简单,方法完全能满足精己二酸中杂质元素的分析要求,可用于生产现场精己二酸的实时质量监测。A method for the analysis of metal impurities in purified adipic acid was established.The sample was dissolved with 2%(V/V)nitric acid,and the Cr,Fe,As,Cd,Sb,Hg and Pb were directly determined by inductively coupled plasma mass spectrometry(ICP-MS).Aiming at the interference of various polyatomic ions formed by the matrix in the sample solution,the He gas was introduced into the octopole collision/reaction cell(ORS),and the interference was eliminated by the helium collision mode.Compared with the non-gas mode,the background equivalent concentration and the detection limit of each element were significantly reduced.The detection limit of each elemental instrument was 0.86~32.5 ng/L.The accuracy of the method was verified by the spiked recovery experiment.The recoveries of the elements ranged from 93.6%to 107.6%.The sample process was simple and was completely meet the analysis requirements of impurity elements in purified adipic acid,and could be used for the real-time quality monitoring of purified adipic acid in the production site.

关 键 词：精己二酸 电感耦合等离子体质谱法 金属杂质 碰撞模式 

分 类 号：O657.63[理学—分析化学]