张坤鹏,刘 宏,徐进勇.电感耦合等离子体质谱(ICP-MS)法测定高铁基体样品中微量元素[J].中国无机分析化学,2018,8(1):37-40.
电感耦合等离子体质谱(ICP-MS)法测定高铁基体样品中微量元素
Determination of Trace Elements in High Iron Matrix Samples by Inductively Coupled Plasma-mass Spectrometry (ICP-MS)
投稿时间:2017-09-18  最后修改时间:2017-12-10
DOI:doi:10.3969/j.issn.2095-1035.2018.01.009
中文关键词:  ICP-MS  高纯铁  Fe  微量元素  基体效应  MIBK
英文关键词:ICP-MS  high purity iron  Fe  trace elements  matrix effect  MIBK
基金项目:钛白废酸与蛇纹石镍矿尾矿渣综合利用的扩大实验项目(14ZC0788)资助
        
作者单位
张坤鹏 成都理工大学,成都 610000
刘 宏 成都理工大学,成都 610000
徐进勇 成都理工大学,成都 610000
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中文摘要:
      由于高纯铁样品中含有大量的铁基体,直接用电感耦合等离子体质谱(ICP-MS)法测定高含量铁基体样品中的微量元素会遇到很多困难,其中主要问题为基体效应,故研究了铁对ICP-MS的基体效应,并采甲基异丁基甲酮(MIBK)萃取的方法去除铁基体,从而实现了高纯铁中Mn、Ni、Cr、Cu、Ti、Co 6种杂质元素的准确测定。研究表明,当萃取时,水相盐酸浓度为7 mol/L,油水相比为1.5,萃取时间为2 min时,萃取率达到最大。各种待测元素方法的检出限为0.4~2.7 ng/g,样品测定结果的相对标准偏差(RSD,n=6)为2.3%~4.5%。为验证方法的可靠性,选用高纯铁国家一级标准物质(GBW01401a)作为样品,采用ICP-MS法进行测定,测得的高纯铁样品中Mn、Ni、Cr、Cu、Ti、Co 6种杂质元素的结果与推荐值吻合得很好,验证了方法的可靠性。
英文摘要:
      Since high-purity iron samples contain a large amount of iron matrix, there are many difficulties in the direct determination of trace elements in high-iron matrix samples by inductively coupled plasma mass spectrometry (ICP-MS). The main problem is the matrix effect. This paper mainly discusses the iron matrix effect for ICP-MS analysis. The MIBK extraction method was proposed to remove the iron matrix. An accurate determination of 6 impurity elements (Mn, Ni, Cr, Cu, Ti and Co) in pure iron was achieved. Results showed that when the hydrochloric acid concentration was 7 mol/L compared to the oil water 1.5, the extraction time was 2 min. The detected extraction rate reached maximum. The detection limit was 0.4—2.7 ng/g for various analytes. The relative standard deviations of the sample determination (RSDs, n= 6) were 2.3%—4.5%. In order to verify the reliability of the method, the highly-pure iron national standard (GBW01401a) was selected as a sample. The content of 6 impurity elements (Mn, Ni, Cr, Cu, Ti, and Co) were measured. The detected values for the impurity elements were in agreement with the recommended values, which verified the method applicability .
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