TODGA负载硅藻土分离-ICP-MS法测定钕中铽、镝和钬量

TODGA Loaded Diatomite Separation-ICP-MS Determination of Terbium,Dysprosium and Holmium in Neodymium

采用硝酸低温溶解试样,通过将TODGA负载到硅藻土上制成色谱柱分离钕基体,然后使用ICP-MS测定铽、镝和钬量。确定在2.0 mL/min的流速,2.4%盐酸淋洗分离钕基体,淋洗体积不小于50 mL条件下分离基体后,选择2.0 mL/min的流速,pH=0.48盐酸反洗铽、镝、钬,收集的待测元素溶液使用ICP-MS测定铽、镝和钬量,测定下限为0.39μg/g、0.17μg/g和0.13μg/g。经精密度和加标回收试验,方法精密度即RSD分别为5.6%、5.8%和6.9%,加标回收率分别为106.0%、99.4%和96.4%。

In this paper,the samples were dissolved in nitric acid at low temperature,then TODGA was loaded on diatomite to make a chromatographic column to separate neodymium matrix.The content of terbium,dysprosium and holmium was determined by ICP-MS.After the neodymium matrix was separated with 2.4%hydrochloric acid at a flow rate of 2.0 mL/min,and the elution volume not less than 50 mL,the flow rate of 2.0 mL/min and pH=0.48 hydrochloric acid were selected to backwash terbium,dysprosium and holmium.The amounts of terbium,dysprosium and holmium were determined by ICP-MS with the lower limits of 0.39μg/g,0.17μg/g and 0.13μg/g,precisions of RSD were 5.6%,5.8%and 6.9%,and the recoveries of standard addition were 106.0%,99.4 and 96.4%,respectively.