摘要
建立了激光剥蚀-电感耦合等离子体质谱(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110μm,扫描速率为50μm/s,脉冲频率为10 Hz,载气流量为0.74 L/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,因此选择用纯钌粉样品,高温高压溶解后,采用ICP-MS法定值所测元素(除硅外)。根据钌粉样品的ICP-MS法定值结果确定了测定元素的相对灵敏度因子(RSF),采用相对灵敏度因子(RSF)对所测结果进行校正,方法准确、快速,检出限为0.007~12.8μg/g,相对标准偏差(RSD)为10%~30%。测定纯钌中杂质元素,结果与ICP-MS法测定的结果吻合。
A method for the determination of nineteen impurity elements Mg,Al,Fe,Ni,Cu,Zn,Rb,Rh,Pd,Mo,Ag,Cd,Sn,Ba,Ir,Pt,Au,Pb and Si in pure ruthenium by Laser Ablation Inductively Coupled Plasma-Mass Spectrometry(LA-ICP-MS)was developed.The instrument parameters have been optimized:Giving a laser energy of 60%,denudation pore size 110μm,the scan rate 50μm/s,pulse rate of 10 Hz and the carrier gas flow rate of 0.74 L/min,signal strength and stability is optimum.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 relative sensitivity factor(RSF)is used to correct the measured results,the method is accurate and quick.The detection limit was 0.007—12.8μg/g,and the relative standard deviation(RSD)was 10%—30%.The method was applied to the quantitative determination of impurity elements in pure ruthenium.The results were in good agreement with those obtained by ICP-MS glow discharge mass spectrometry.
作者
贾贵发
李秋莹
甘建壮
马媛
杨辉
JIA Guifa;LI Qiuying;GAN Jianzhuang;MA Yuan;YANG Hui(State Key Laboratory of Advanced Technologies for Comprehensive Utilization of Platinum Metals,Sino-Platinum Metals Co.,Ltd.,Kunming,Yunnan 650106,China;Guiyan Detection Technology (Yunnan) Co.,Ltd.,Kunming,Yunnan 650106,China)
出处
《中国无机分析化学》
CAS
北大核心
2021年第2期51-56,共6页
Chinese Journal of Inorganic Analytical Chemistry
基金
国家重点研发计划项目(2017YFB0305405)。
