摘要
建立了电感耦合等离子体质谱法（ICP-MS）同时测定生铁中的硼、锌、钴、钼、铅、砷、锡、锑、铋的方法.讨论了样品溶解方法、质谱干扰与同位素选择、基体效应及内标的校正作用.确定了用硝硫混酸溶解样品,11B、66Zn、59Co、98Mo、208Pb、75As、118Sn、121Sb、209Bi作为待测元素的测量同位素.通过以高纯铁粉进行基体匹配和采用Sc作为质量数小于100的元素的内标,In作为质量数在100～130的元素的内标,Tl作为质量数大于130的元素的内标来消除基体效应和仪器信号漂移的影响.方法应用于生铁标准样品中各元素的测定,测定值与认定值吻合,除了Bi因含量较低其相对标准偏差（RSD,n=8）为16.5％外,其余元素的RSD（n=8）都小于10.0％.方法应用于实际样品分析,测得结果与电感耦合等离子体原子发射光谱法吻合.
A method for the simultaneous determination of trace elements including B, Zn, Co, Mo, Pb, As, Sn, Sb and Bi in pig iron by inductively coupled plasma mass spectrometry was developed. The sample dissolution method, interference of mass spectrometry, selection of determination isotopes as well as the matrix effect and the correction effect of internal standard were discussed. The mixed acid of nitric acid and sulfuric acid was used for sample dissolution. ^11B, ^66Zn, ^59Co, ^98Mo, ^208Pb, ^75As, ^118Sn, ^121Sb, and ^209Bi were selected as testing isotopes. The matrix and instrument signal drift effects were eliminated by matrix matehing with highly pure iron powder and using Se, In and T1 as the internal standards of the determined elements whose mass numbers were smaller than 100, be- tween 100 and 130 and larger than 130 respectively. This method was applied to determine the ele- ments in pig iron standard samples and the results were consistent with the certified values. The rela- tive standard deviations （RSDs, n=8） for all elements were smaller than 10.0% except for Bi whose RSD （n=8） was 16.5% ,because the content of Bi was comparatively lower than the others. When this method was applied to practical sample analysis, its results was consistent with those obtained by inductively coupled plasma atomic emission spectrometry.
出处
《冶金分析》
CAS
CSCD
北大核心
2014年第8期27-31,共5页
Metallurgical Analysis
关键词
电感耦合等离子体质谱法
生铁
痕量元素
inductively coupled plasma mass spectrometry
pig iron
trace element
