电感耦合等离子体质谱法测定高纯氧化镨中稀土杂质

Determination of Rare Earth Element Impurities in High Purity Pr_6O_11 by Inductively Coupled Plasma Mass Spectrometry

深入考察了ICP-MS法测定高纯氧化镨时基体对稀土杂质测定的影响,研究了P_(507)萃淋树脂分离大量基体Pr_6O_(11)的实验条件,建立了采用内标补偿直接测定大部分稀土杂质和经P_(507)萃淋树脂分离基体后测定被干扰离子Tb相结合测定高纯Pr_6O_(11)中稀土杂质的ICP-MS分析方法.方法检出限为0.005～0.021mg/L;加标回收率为89.1～102%;测定精度RSD为0.76%～3.2%.本法适用于纯度为99.99%～99.9999%的高纯Pr_6O_(11)中稀土杂质的分析.

A method for the determination of rare earth element (REE) impurities in high purity Pr6O11 by ICP-MS was reported. The interference form the matrix of Pr6O11 on the ICP-MS determination was studied. Matrix induced signal suppression effect was compensated by internal standardization and the P507 extraction chromatographic column was used to separate Tb from the matrix, which is seriously suffered from the spectra overlap of polyatomic ions connected with matrix. By combining the direct ICP-MS determination with matrix removal with extraction chromatographic separation, 14 REE impurities in high purity Pr6O11 were determined, detection limits for Rees were 0.02-0.09 μg/g. Recoverier of standard addition were 89. 1 % -105% with precision of 0.8% -3.2% RSD. The method has been applied to the determination of REE impurities in Pr6O11 samples with purity of 99.99% - 99.999% .