电感耦合等离子体质谱法测定地球化学样品中痕量铑的干扰消除方法探讨

发布时间：2018-04-17 00:34

  本文选题：高压密闭消解 + 电感耦合等离子体质谱法　； 参考：《冶金分析》2017年09期

【摘要】：采用电感耦合等离子体质谱法(ICP-MS)测定地球化学样品中痕量Rh时,待测溶液的基体及分子离子干扰严重影响ICP-MS测定~(103)Rh的准确性。实验以10ng/mL的~(175)Lu消除基体干扰,以数学校正方程消除多原子离子~(87)Sr~(16)O~+、~(63)Cu~(40)Ar~+、~(86)SrOH、~(206)Pb~(2+)对~(103)Rh的干扰,最终实现了电感耦合等离子体质谱法测定地球化学样品中痕量Rh。分别详细考察了Cu、Sr、Pb对Rh测定的干扰情况,不仅有效消除了~(87)Sr~(16)O~+、~(63)Cu~(40)Ar~+、~(86)SrOH多原子离子对~(103)Rh的测定干扰,而且发现了双电荷离子~(206)Pb~(2+)对~(103)Rh的测定存在严重的质谱干扰。同时通过向不同浓度Rh的标准溶液中分别加入不同量的干扰元素Cu、Sr及Pb进行试验,得到了对~(103)Rh元素进行校正的数学校正方程。实验表明,Rh在0.050~100.0ng/mL范围内与其对应的信号强度呈良好的线性关系,线性相关系数为0.999 9,方法检出限(3σ)为0.014ng/g。采用实验方法对铂族元素地球化学一级标准物质中Rh进行分析,结果与认定值的相对误差(RE)为-7.27%~6.15%,相对标准偏差(RSD,n=12)均不大于8.6%。将实验方法应用于云南、四川、新疆等地区不同含量贵金属地球化学样品中Rh的测定,所得结果与锡试金方法符合性较好。
[Abstract]:In the determination of trace Rh in geochemical samples by inductively coupled plasma-mass spectrometry (ICP-MS), the accuracy of ICP-MS determination of Rh is seriously affected by the matrix and molecular ion interference of the solution to be determined.In this experiment, the matrix interference was eliminated by using 10ng/mL 175H Lu, and the interference of polyatomic ion Srm7O16O ~ ~ ~ () ~ ~ ~In this paper, the interference of Cu ~ (2 +) Sr ~ (2 +) Pb to the determination of Rh is investigated in detail. It not only effectively eliminates the interference caused by the polyatomic ion of Cu ~ (87) O ~ (16) O ~ (6) C ~ (6) C ~ (60) C ~ (60) O ~ (?) ~ (?) ~ (86) S ~ (OH) on the determination of Rh, but also finds that there is a serious mass spectrometry interference in the determination of Rh by the double charge ion (206Pbbbn2), which is not only effective in the determination of Rh, but also in the determination of Rh.At the same time, by adding different amounts of interference elements Cu-Sr and Pb into the standard solution of different concentrations of Rh, the mathematical correction equation for the correction of Rh is obtained.The experimental results show that Rh has a good linear relationship with the corresponding signal intensity in the range of 0.050~100.0ng/mL, with a linear correlation coefficient of 0.999 and a detection limit of 3 蟽) of 0.014 ng / g.The Rh in the primary reference material of platinum group element geochemistry is analyzed by experimental method. The relative error between the result and the determined value is -7.276.15, and the relative standard deviation (RSDN) is not greater than 8.6%.The experimental method has been applied to the determination of Rh in precious metal geochemical samples with different contents in Yunnan, Sichuan and Xinjiang.
【作者单位】： 河南省岩石矿物测试中心国土资源部贵金属分析技术重点实验室;河南省地质矿产勘查开发局第一地质勘查院;
【基金】：河南省“两权价款”地质科研项目(豫国土资发[2016]56号-4)
【分类号】：O657.63;P632
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