电感耦合等离子体质谱法(ICP-MS)测定水系沉积物中的铌钽锆铪

Determination of Nb,Ta,Zr and Hf in stream sediment by inductively coupled plasma mass spectrometry(ICP-MS)

建立电感耦合等离子体质谱法（ICP-MS）测定水系沉积物中铌、钽、锆、铪四种元素的分析方法。将样品与氢氧化钠、过氧化钠混合物放入高温炉中,熔融分解完全,用热水提取,过滤后弃去滤液,将滤纸及沉淀用酒石酸-盐酸溶液溶解,稀释至刻度测定。方法检出限（3s）为：LD（Nb）=0.08μg/g,LD（Ta）=0.04μg/g,LD（Zr）=0.5μg/g,LD（Hf）=0.04μg/g,精密度（RSD%,n=6）为：0.84%~4.21%。该测定方法具有灵敏度高、精密度好、分析速度快、线性范围宽、操作性强等优势。采用该方法对国家一级标准物质进行测定表明,其结果与标准值吻合。此方法已在实际地质调查样品分析中得到应用。

This paper intended to make use of inductively coupled plasma mass spectrometry （ICP-MS）as an analytical method for the determination of Nb,Ta,Zr,Hf in stream sediment.The samples were put in a high temperature furnace with mixture of sodium hydroxide and sodium peroxide until they were decomposed completely.Through hot water extraction,filtering and removal of the filtrate,the filter paper and precipi-tation were dissolved by tartaric acid and hydrochloric acid solution,and they were diluted to the scale for de-termination.The detection limit （3s）was LD（Nb）=0.08μg/g,LD（Ta）=0.04μg/g,LD（Zr）=0.5μg/g, LD（Hf）=0.04μg/g.The precision was 0.84%-4.21% （RSD%,n=6）.This determination method was characterized by high sensitivity,good precision,fast analysis,wide linear range,maneuverability and other advantages.GBW materials of Chinese standard were tested by this method,and the results indicated agree-ment with the standard values.The method has been applied to the analysis of a great many of samples from field geological survey.