| 改进的挥硅-ICP-MS法测定高纯四氯化硅中金属杂质 |
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| 引用本文： | 郭峰,谭红,何锦林,谢锋,曾广铭,宋光林.改进的挥硅-ICP-MS法测定高纯四氯化硅中金属杂质[J].福建分析测试,2006,15(4):7-9. |
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| 作者姓名： | 郭峰 谭红 何锦林 谢锋 曾广铭 宋光林 |
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| 作者单位： | 贵州大学,贵州,贵阳,550001;贵州省理化分析测试研究中心,贵州,贵阳,550001;贵州省理化分析测试研究中心,贵州,贵阳,550001 |
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| 基金项目： | 财政部产业技术成果转化项目 |
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| 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0.009~0.05μg/L。
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| 关 键 词： | 高纯四氯化硅 ICP-MS 金属杂质 |
| 文章编号： | 1009-8143（2006）04-0007-03 |
| 收稿时间： | 2006-03-30 |
| 修稿时间： | 2006年3月30日 |
Determination of 9 Impurities in high Purity SiliconTetrachloride by improved method of blowing SiCl4-ICP-MS |
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| Guo Feng,Tan Hong,He Jinlin,Xie Feng,Zeng Guangming,Song Guanglin.Determination of 9 Impurities in high Purity SiliconTetrachloride by improved method of blowing SiCl4-ICP-MS[J].Fujian Anal Ysis & Testing,2006,15(4):7-9. |
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| Authors: | Guo Feng Tan Hong He Jinlin Xie Feng Zeng Guangming Song Guanglin |
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| Abstract: | 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 N_2 gas was passed through at the same time in order to make the sicl_4 out till no sicl_4 liquid was left in the plastics bottle.Then, pure HNO_3 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. |
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| Keywords: | ICP-MS |
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