Yang X J
China Institute of Atomic Energy, Beijing, China.
Talanta. 1994 Nov;41(11):1807-13. doi: 10.1016/0039-9140(94)e0115-8.
An easily applicable separation method has been developed for the accurate and simultaneous determination of trace amounts of Al, Ca, Co, Cr, Cu, Mg, Mn, Ni, Pb and Zn in high purity europium oxide by inductively coupled plasma atomic emission spectrometry (ICP-AES) combined with extraction chromatography. Spectral interferences and europium matrix effects were examined. The chromatographic separation procedure was carried out with a di-(2-ethylhexyl) phosphoric acid (HDEHP)-Levextrel resin as the stationary phase, which retained the matrix europium, and dilute nitric acid as the mobile phase, which eluted the analyte of interest. The effect of nitric acid concentration on the adsorption of europium and the analyte ions on the resin, the eluting behaviour of these elements on the chromatographic column, and the capacity of the resin for europium oxide were investigated. The quantitative limits for determination (10 sigma), based on a 0.5-g amount of europium oxide, are between 0.36 microg/g for Mn and 6.4 microg/g for Pb. The method was applied to two spiked samples and a high purity europium oxide certified reference material. Results were obtained for recoveries of 93.2-112% and precision of 4-13%, expressed as the relative standard deviation and excellent agreement with the certified value with a relative error of <4%.
已开发出一种易于应用的分离方法，通过电感耦合等离子体原子发射光谱法（ICP-AES）结合萃取色谱法，准确同时测定高纯氧化铕中痕量的铝、钙、钴、铬、铜、镁、锰、镍、铅和锌。研究了光谱干扰和铕基体效应。色谱分离过程以二（2-乙基己基）磷酸（HDEHP）-Levextrel树脂为固定相，保留基体铕，以稀硝酸为流动相，洗脱目标分析物。考察了硝酸浓度对铕和分析物离子在树脂上吸附的影响、这些元素在色谱柱上的洗脱行为以及树脂对氧化铕的容量。基于0.5 g氧化铕的测定定量限（10σ），锰为0.36 μg/g，铅为6.4 μg/g。该方法应用于两个加标样品和一种高纯氧化铕标准物质。回收率为93.2% - 112%，精密度为4% - 13%（以相对标准偏差表示），与认定值的相对误差<4%，结果吻合良好。
