萃取分离基体-电感耦合等离子体质谱法测定高纯二氧化锆中痕量稀土杂质

Determination of trace rare earth impurities in high purity zirconium dioxide by inductively coupled plasma mass spectrometry after separation by solvent extraction

建立了1-苯基-3-甲基-4-苯甲酰基-吡唑酮[5]（PMBP）萃取分离基体-电感耦合等离子质谱法（ICP-MS）测定高纯二氧化锆中痕量稀土杂质的方法。结果表明，在2mol／L HNO3介质中，基体锆的萃取率为99．7％，而待测稀土元素则完全留在水相中。考察了影响萃取和测定的主要因素。在优化实验条件下，方法的测定下限为1．8～5．7ng／g，回收率在89．0％～110％之间，相对标准偏差（RSD）小于14％。

A method was developed for the determination of trace rare earth impurities in high purity zirconium dioxide by inductively coupled plasma mass spectrometry（ICP-MS） after separation by solvent extraction. 1-phenyl-3-methyl-4-benzoyl-5-pyrazone（PMBP） was used as extractant. In 2 mol/L HNO3 medium,it was found that more than 99.7% of the Zr matrix was removed.The main factors affecting the extraction and determination,including acidity,PMBP amount and matrix concentration were investigated in detail. In the optimal conditions, the determination limits are 1.8-5.7 ng/g in solid ZrO2 with the relative standard deviations less than 14 % and recoveries of 89.0%-110 % for 14 rare earth impurities.