采用高温高压酸溶,同位素稀释电感耦合等离子体质谱法,以铂族多元素标准溶液和铂族单元素标准溶液标定了^99Ru、^105Pd、^191Ir、^198Pt稀释剂溶液的浓度。根据最佳稀释比和最佳测量比,配制了三组待标定稀释剂溶液,所得浓度结果不确定度在1%左右。建立了一套溶解金属Ru、Ir的方法,同时确定了测量Ru、Pd、Ir、Pt时检测器死时间。用标准溶液测得各元素的多组同位素比值和质量数,拟合出Ru、Pd、Pt的分馏系数方程,通过分馏系数校正丰度测量中的质量分馏。
A method for the preparation and calibration of mixed isotope spike solutions for simultaneous determination of platinum-group elements(PGEs) by ID-ICPMS is described in this paper. ^99Ru and ^191Ir isotope spike solutions are prepared by digestion of metal spikes undue high temperature and high pressure. And the concentration of spike solutions of ^99 Ru, ^105 Pd, ^191ir and ^198 Pt are calibrated with single and mixed PGEs standards. On the basis of optimization of dilution ratios and signal intensity ratios, which can cover a wide range of PGEs contents in the samples, three sets of mixed spike solutions are prepared with uncertainty of about 1%. Through the experiments, the dead time of the ICPMS instrument is optimized for mass bias calibration. And equations for mass fractionation factor calculation of Ru, Pd and Pt are established by fitting the data of isotope ratios and masses from the determination of standard solutions of these elements and have been applied to the mass fractionation calibration in isotope abundance measurements.