【摘要】 研究了不经基体分离,膜去溶-ICP-MS法直接测定高纯CeO2中14种痕量稀土杂质的分析方法,讨论了Ce基体产生的多原子离子对被测元素的质谱干扰,并且对影响多原子离子产率的因素进行了分析,同时建立了Pr,Gd,Tb和Yb数学校正方程。通过使用膜去溶雾化器和优化ICP-MS参数,消除了CeH+,CeO2+和CeO2H+产生的质谱干扰,将CeO/Ce产率降为0.008%,同时结合数学校正方程彻底消除了CeO+,CeOH+和CeOH2+的质谱干扰。Pr,Gd,Tb和Yb的方法测定下限分别为0.08,0.1,0.15和0.008μg.g-1,14种稀土杂质方法测定下限和为0.75μg.g-1。99.999%高纯CeO2实际样品测定加标回收率为96%~103%,RSD为1.2%~4.3%。更多还原

【Abstract】 A method for the direct determination of 14 trace rare earth impurities in high purity CeO2,without of separation impurities from Ce matrix,by inductively coupled plasma mass spectrometry with membrane desolvation(MD-ICP-MS) was developed.The mass spectra isobaric interferences of polyatomic ions from Ce matrix to the analyte were discussed,and the factors that,which influenced the production ratio of polyatomic ions also analyzed.The algebraic correction equations of Pr,Gd,Tb and Yb were developed.By utilizing membrane desolvation and optimizing the operation conditions of ICP-MS,the polyatomic ion interferences from CeH+,CeO2+and CeO2H+ were eliminated,and the production ratio of CeO/Ce was reduced to 0.008%.Combining with algebraic correction equations,the polyatomic ion interferences from CeO+,CeOH+ and CeOH2+ was eliminated completely.The determination limits for Pr,Gd,Tb and Yb were 0.08,0.1,0.15 and 0.008 μg·g-1,respectively.The total determination limit for 14 rare earth impurities was 0.75 μg·g-1.The recoveries of spiked 99.999% high-purity CeO2 sample for 14 REEs were 96%~103% with the precision of 1.2%~4.3% RSD.更多还原