高压消解-电感耦合等离子体质谱(ICP-MS)法测定地质样品中的铌和钽

Determination of Niobium and Tantalum in Mineral by High Pressure Dissolution-Inductively Coupled Plasma Mass Spectrometry

建立了运用硝酸-硫酸-氢氟酸体系高压消解样品,电感耦合等离子体质谱(ICP-MS)法测定地质样品中铌和钽含量的方法。研究了样品消解体系、样品消解时间、溶液的介质、内标元素等对测定的影响。Nb的方法检出限为0.027μg/g,Ta的方法检出限为0.015μg/g。Nb测定的相对标准偏差(RSD)为3.3%;Ta测定的相对标准偏差(RSD)为2.5%。经标准物质验证,分析结果令人满意,可适用于大批量地质样品中铌和钽的测定。

A methodfor the determination of niobium and tantalum contents in mineral by ICP-MS was established in this paper. The samples were dissolved in HF-HNO3-H2SO4 solution using high pressure digestion system. Effects of sample dissolution system, dissolution time, solution medium and internal standard element on determination results were studied. The detection limit of Nb was 0. 027 μg/g and the detection limit of Ta was 0. 015 μg/g. The relative standard deviation （RSD） of Nb is 3.3%; the RSD of Ta is 2.5%. The analytical results of the standard materials were satisfactory, which indicated that this method can be applied to analyze niobium and tantalum in large batches of geological samples.