预富集电感耦合等离子体质谱法测定地下水中超痕量稀土元素及钪、钇

Determination of Trace Rare Earth Elements, Sc, and Yin Ground Water by Inductively Coupled Plasma Mass Spectrometry with Preconcerntration Method

以P50 7萃淋树脂为固定相 ,HCl EDTA为流动相 ,建立了地下水中超痕量稀土元素及钪、钇的ICP MS测定的新方法。详细探讨了稀土元素 (REEs)、Sc、Y与基体元素的分离、EDTA小体积洗脱的实验条件及ICP MS工作参数。在pH 2 .6时上柱 ,大部分Ca、Mg ,基体可不经淋洗而直接与REEs分离 ;以 10 0mmol的EDTA洗脱 ,5mL淋洗体积REEs、Y、Sc回收率为 96 %～ 98.5 %。详细考察了La、Ce、Pr的氧化物离子及氢氧化物离子的干扰及校正方法。分析方法的检测限为 0 .7～ 10 .1ng L ,加标回收率为 95 %～ 99%。用于实际地下水及人工模拟水样的分析 ,结果令人满意。

A method for the determination,of ultra-trace rare earth elements (REs), Sc and Y in ground water with inductively coupled plasma mass spectrometry (ICP-MS) was established with. 2-ethylhexyl hydrogen 2-ethylhexylphosphonate (P-507) resin as the stationary phase and HCl/EDTA as a mobile phased The separation-of REs, Sc, and Y from the matrix elements; experimental conditions for elution with small amount of EDTA and optimum parameters of ICP-MS were discussed. When the column is set at pH 2.6, most of the matrix,elements such as Ca and Mg were separated from M - without: elution. A complete separation was accomplished with elution of 5 mL 100 mmole EDTA. The detection limit for this determination is 0.7 similar to 10.1 ng/L. The recovery of standard addition is 95% similar to 99%. Satisfactory result was obtained for RES in both practical and simulated ground water.