ICP-AES法测定二氧化镎粉末中的杂质元素

Determination of Impurity Element in Neptunium Dioxide Powder by ICP-AES

建立了采用电感耦合等离子体发射光谱(ICP-AES)法测定二氧化镎粉末中Ca、Be、Cd等12种金属杂质元素含量的分析方法。采用HNO_3-HF混酸体系于聚四氟乙烯坩埚中溶解二氧化镎粉末样品,样品溶液进行调价后再用TEVA树脂柱进行预处理,接收的样品测试液采用ICP-AES法进行测量。结果表明,最佳分析条件为:取样量30 mg、样品溶解液采用过氧化氢在常温下调价约5 min、5 mol/L硝酸为淋洗液。在此条件下,元素的收率大于95%,各元素测量值的相对标准偏差为0.6%～4.8%(n=6),方法的加标回收率为93%～108%、检测限为0.07～8μg/g。

The determination method of impurity metal elements in the neptunium dioxide powder was built by ICP-AES, which could detect twelve impurity metal elements such as calcium, beryllium, cadmium, etc. In this work, a HNO3-HF acid system was used to dissolve the neptunium dioxide powder in polytetrafluoroethylene crucible, then the solution was dealt with TEVA resin column after valence adjustment, and the sample test solution was detected by ICP-AES. The results show that the optimum analytical conditions are as follows: Sample dissolution adjusted with hydrogen peroxide about 5 min, sample amount of 30 mg, and 5 mol/L nitric acid as eluent. Under these conditions the recoveries of most elements are more than 95%, the relative standard deviations(n=6) are between 0.6% and 4.8% with 93%-108% recoveries, and the detection limits of this method are 0.07-8 μg/g.