电感耦合等离子体质谱(ICP-MS)法工作参数对灵敏度和氧化物干扰的实验研究  

Study on the Interference of ICP-MS Operating Parameters on Sensitivity and Oxide

作　　者：张鹏鹏 胡梦颖 徐进力[1,2] 刘彬 张灵火[1,2] 白金峰 ZHANG Pengpeng;HU Mengying;XU Jinli;LIU Bin;ZHANG Linghuo;BAI Jinfeng(Institute of Geophysical and Geochemical Exploration,Chinese Academy of Geological Sciences,Langfang,Hebei 065000,China;Key Laboratory of Geochemical Exploration,Ministry of Natural Resources,Langfang,Hebei 065000,China)

机构地区：[1]中国地质科学院地球物理地球化学勘查研究所,河北廊坊065000 [2]自然资源部地球化学探测重点实验室,河北廊坊065000

出　　处：《中国无机分析化学》2023年第4期396-406,共11页Chinese Journal of Inorganic Analytical Chemistry

基　　金：中国地质科学院基本科研业务专项(AS2020J04)。

摘　　要：改变电感耦合等离子体质谱仪的仪器工作条件实验,得出功率、雾化气流量、氦气流量和采样深度对灵敏度和氧化物的产率产生较大的影响,而改变扫描次数、驻留时间、冷却气流量和辅助气流量等条件,各元素的灵敏度和氧化物的产率基本无变化。采用氢氟酸-高氯酸-硫酸-硝酸-盐酸来消解样品,选择仪器的最佳条件,得出La、Ce、Pr、Nd、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb、Lu和Y的方法检出限分别为0.01、0.01、0.003、0.02、0.004、0.002、0.004、0.001、0.004、0.001、0.003、0.001、0.002、0.001和0.03 ng/g。三个标准物质的稀土元素方法精密度均小于6.0%,经多个标准物质进行验证,所测稀土元素相对误差基本都小于10%,满足多目标地球化学样品测试的精密度和准确度要求。As the most important instrument for inorganic element analysis, ICP-MS plays a key role in production and scientific research.Through the experiment of changing the instrument working conditions of ICP-MS in the determination process, it is concluded that the power, atomization gas flow rate, helium flow rate, and sampling depth have a great impact on the sensitivity and oxide yield, while the sensitivity of each element and oxide yield basically remain unchanged by changing the scanning times, residence time, cooling gas flow rate, and auxiliary gas flow rate.Using HF-HClO4-H2SO4-HNO3-HCl to digest the samples, and the best conditions of the instrument were selected.The detection limits of La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu and Y were 0.01,0.01,0.003,0.02,0.004,0.002,0.004,0.001,0.004,0.001,0.003,0.001,0.002,0.001 and 0.03 ng/g, respectively.The precision of the rare earth element method of the three reference materials is less than 6.0%.Verified by multiple reference materials, the relative error of the measured rare earth elements is basically less than 10%,which meets the precision and accuracy requirements of multi-target geochemical sample testing.

关 键 词：电感耦合等离子体质谱法 灵敏度 氧化物 产率 稀土元素 

分 类 号：O657.63[理学—分析化学] TH843[理学—化学]