集合式屑状标准物质校正-激光烧蚀电感耦合等离子体质谱法分析镍基高温合金中痕量元素

全面优化了激光烧蚀电感耦合等离子体质谱法(LA-ICP-MS)分析镍基高温合金的工作参数;考察了激光进样的质谱干扰问题;选择合金元素Ti作内标;尝试并比较了多种屑状标准物质固定方式,即采用胶粘方式将屑样固定在平板玻璃上的集合式标准物质来代替块状标样进行定量分析,较好地解决了由于缺乏基体匹配的块状标准物质而限制LA-ICP-MS应用于定量分析的问题。所建立了LA-ICP-MS法应用于高温合金标准物质中B、Mg、Al、Cu、Zn、Ga、Ge、As、Se、Ag、Cd、In、Sn、Sb、Te、Tl、Pb、Bi等18种痕量元素的分析,B、Mg、P、Se的测定下限小于10μg/g,其他元素的测定下限小于1μg/g,大多数元素的RSD值均小于15%。应用于一组高温合金样品中B、Zn、As、Ag、Bi等10种痕量元素的分析,测定结果与参考值吻合较好。

Determination of trace elements in nickel-base superalloy by laser ablation inductively coupled plasma mass spectrometry with correction of aggregated reference material chips

Laser-ablation conditions and plasma conditions have been optimized for the analysis of nick-el-base superalloy sample. Spectral interferences of laser ablation inductively coupled plasma massspectrometry(LA-ICP-MS) were investigated. Titanium was chosen as the internal standard. Several manners have been attempted and evaluated to fix up superalloy chips. The aggregated chips on a plate glass by double-sided adhesive could be a good substitute of bulk reference materials. As a result, the correction limitation caused by the lack of matrix-matched bulk reference materials was gotten over. The method was applied to analyze eighteen trace elements (B, P, Sc, Cu, Zn, Ga, Ge, As, Se, Ag, In, Sn, Sb, Te, Hf, Tl, Pb and Bi) in CRM of superalloy, and the determination limits of most ele-ments were lower than 1 μg/g except B, Mg, P and Se lower than 10 μg/g. For most of trace ele-ments in CRMs, RSDs were smaller than 15 %. Furthermore, ten trace elements in four samples were quantitatively analyzed by the method, and the quantitative results agreed well with the certified val-ues.