改进的挥硅-ICP-MS法测定高纯四氯化硅中金属杂质  

Determination of 9 Impurities in high Purity SiliconTetrachloride by improved method of blowing SiCl4-ICP-MS

作　　者：郭峰[1] 谭红 何锦林 谢锋 曾广铭[1] 宋光林[1] 

机构地区：[1]贵州大学,贵州贵阳550001 [2]贵州省理化分析测试研究中心,贵州贵阳550001

出　　处：《福建分析测试》2006年第4期7-9,共3页Fujian Analysis & Testing

基　　金：财政部产业技术成果转化项目(No.05063)

摘　　要：本文对钛厂回收副产物高纯四氯化硅中的9种金属杂质进行了测定。采用密封针管取样，转移塑料挥气瓶中，恒温水浴锅控制温度（57℃）通入干燥惰性气体（N2），在塑料挥气瓶挥去基体四氯化硅，富集的金属加入硝酸转变成溶液后定容，用电感耦合等离子质谱法（ICP-MS）直接测定其中Pb、Zn、Mn等9种微量金属杂质。用Rh做内标元素补偿基体效应和灵敏度漂移。样品的加标回收率为98．15-102．0％，相对标准偏差（RSD）为0．9％-3．5％，检出限为0．009-0．051μg／L。A method for determination of 9 metal impurities in high purity silicon tetrachloride was developed. The samples were taken into a plastics bottle maintened at 57℃ by hermetic injection. Dry N2 gas was passed through at the same time in order to make the sicl4 out till no sicl4 liquid was left in the plastics bottle. Then, pure HNO3 was added to dissolve riched metals. Ti,V ,Cr,Co,Ni ,Cu ,Pb,Zn,Mn were analyzed by ICP - MS. Internal Rh standard was selected to compensate the drift of analytical signals. Under the optitum conditions the determination limits for 9 elements were in the range of 0.009 - 0.05μg/L . The RSD were less than5. 0%, linearity correlations were larger than 0. 999 and the recoveries were 98.15 - 102.0%.

关 键 词：高纯四氯化硅 ICP-MS 金属杂质 

分 类 号：O657.3[理学—分析化学]