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7mol/L,油水相比为1.5,萃取时间为2min时,萃取率达到最大。各种待测元素方法的检出限为0.4~2.7ng/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。
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.
作者
张坤鹏
刘宏
徐进勇
ZHANG Kunpeng;LIU Hong;XU Jinyong(Chengdu University of Technology,Chengdu,Sichuan 610000,China)
出处
《中国无机分析化学》
CAS
2018年第1期37-40,共4页
Chinese Journal of Inorganic Analytical Chemistry
基金
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
