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中国无机分析化学:2021,11(2):51-56
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激光剥蚀-电感耦合等离子体质谱法测定纯钌中19种杂质元素
贾贵发1, 李秋莹2, 甘建壮2, 马媛3, 杨辉3
(1.贵研铂业股份有限公司;2.贵研检测科技(云南)有限公司;3.贵研铂业股份有限公司,稀贵金属综合利用新技术国家重点实验室)
Determination of 19 impurity elements in pure ruthenium by laser denudation-Inductively coupled plasma mass spectrometry
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投稿时间:2020-08-17    修订日期:2020-08-25
中文摘要: 建立了激光剥蚀-电感耦合等离子-体质谱法(LA-ICP-MS)法测定纯钌中Mg、Al、Fe、Ni、Cu、Zn、Rb、Rh、Pd、Mo、Ag、Cd、Sn、Ba、Ir、Pt、Au、Pb和Si等19种杂质元素的分析方法。优化了仪器参数:给出了激光能量为60%,剥蚀孔径为110 μm,扫描速率为50 μm/s,脉冲频率为10Hz,载气流量为0.74L/min条件下,信号强度和稳定性最佳。由于钌标准样品难以获得,本文选择用纯钌粉样品,高温高压溶解后,采用ICP-MS定值所测元素(除硅外)。根据钌粉样品的ICP-MS定值结果确定了测定元素的相对灵敏度因子(RSF),对归一法结果进行较正,提高了方法准确度。方法的检出限为:0.001~12.81μg/g,相对标准偏差(RSD)为:10%~30%。采用本方法测定纯钌中杂质元素,结果与ICP-MS测定的结果吻合。
Abstract:A method for the determination of twenty-four impurity elements Mg, Al, Fe, Ni, Cu, Zn, Rb, Rh, Pd, Mo, Ag, Cd, Sn, Ba, Ir, Pt, Au, Pb and Si in pure Iridium by Laser Ablation inductively coupled plasma-mass spectrometry(LA-ICP-MS)was developed.The instrument parameters have been optimized: Gives a laser energy of 60%,denudation pore size 110μm,the scan rate is 50μm/s,Pulse rate of 10 Hz and the carrier gas flow rate is 0.74 L / Min, Optimum signal strength and stability. Because ruthenium standard sample is difficult to obtain, in this paper, the ruthenium powder was dissolved at high temperature and high pressure, Elements other than silicon determined by ICP-MS ,The relative sensitivity factor (RSF) of ruthenium powder was determined by ICP-MS.The results of the normalization method are correct and the accuracy of the method is improved. The detection limit of the method was 0.007μg/g~12.81μg/g, and the relative standard deviation (RSD) was 10% ~ 30%. The method was applied to the quantitative determination of impurity elements in pure iridium, The results were in good agreement with those obtained by ICP-MS glow discharge mass spectrometry.
文章编号:     中图分类号:    文献标志码:
基金项目:国家重点研发计划项目(No.2017YFB0305405)
引用文本:
贾贵发,李秋莹,甘建壮,马媛,杨辉.激光剥蚀-电感耦合等离子体质谱法测定纯钌中19种杂质元素[J].中国无机分析化学,2021,11(2):51-56.
JIA Fa-gui,LI Qiu-ying,GAN Jian-zhuang,MA Yuan,YANG Hui.Determination of 19 impurity elements in pure ruthenium by laser denudation-Inductively coupled plasma mass spectrometry[J].Chinese Journal of Inorganic Analytical Chemistry,2021,11(2):51-56.

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