微柱分离-ICP-MS测定高纯氧化铈中14个稀土杂质

Determination of 14 Rare Earth Impurities in High-purity CeO_(2) with ICP-MS after Micro-column Separation

研究了微柱分离-ICP-MS法测定高纯CeO_(2)中Gd、Tb含量的基体分离条件。建立了高纯CeO_(2)中分离Ce后测定Gd、Tb以及内标补偿法直接测定其它12种稀土杂质的ICP-MS分析方法。方法测定下限为0.2μg/g~0.5μg/g,加标回收率为93.5%~107.5%,RSD为2.4%~6.0%,精密度好。本方法可满足快速测定99.999%氧化铈中14个稀土杂质的要求。

A method for separation of Gd and Tb from the CeO_(2)matrix to eliminate the mass spectral interference of the matrix was developed by using a micro-column separation.Gd and Tb were determined with ICP-MS after separation,whereas the other 12 REE impurities were determined directly with ICP-MS by using internal standard method to eliminate the matrix effects.The determination limits for REE were 0.2μg/g to 0.5μg/g,the recoveries of standard addition were 93.5%to 107.5%and the RSDs of the determinations were 2.4%to 6.0%.The method was rapid and easy to operate.It has been applied to the determination of 14 REE impurities in 99.999%CeO_(2).