巯基棉分离富集-电感耦合等离子体质谱法测定岩矿中痕量金和钯

Determination of trace gold and palladium in rock and mineral by inductively coupled plasma mass spectrometry after separation and enrichment with sulfhydryl cotton

岩矿样品经混合酸溶解后,在1.2 mol/L HCl介质中,采用巯基棉分离富集其中的Au和Pd,建立了电感耦合等离子体质谱法（ICP-MS）测定Au和Pd的方法。对样品分解、吸附、洗脱条件等进行了研究。实验表明,使用巯基棉分离富集和选择适当的同位素消除了质谱干扰,采用基体匹配法和以Re为内标元素校正了基体效应和仪器波动的影响。Au和Pd的方法检出限为0.13和0.22 ng/g。使用该法分析标准物质,分析结果与认定值一致,相对标准偏差为（RSD,n=9）4.8%~8.3%,可满足岩矿样品的分析测试要求。

After dissolved with mixed acids,gold and palladium in rock and mineral samples were separated and enriched by sulfhydryl cotton in 1.2 mol/L HCl solution.Consequently,a determination method of gold and palladium by inductively coupled plasma mass spectrometry（ICP-MS） was established.The experiment conditions about sample decomposition,adsorption and elution were discussed.Experiment results showed that the mass spectral interference was eliminated by sulfhydryl cotton separation and enrichment in combination with selecting appropriate analytical element.Then,the matrix effect and instrument fluctuation were corrected with matrix matching method and Re as the internal standard element.The detection limits of this method for gold and palladium were 0.13 and 0.22 ng/g respectively.When the method has been applied to determine certified reference materials,the results were consistent with the certified values with the relative standard deviations（RSD,n=9） of 4.8%-8.3%,which could meet the analysis and testing requirements for rock and mineral samples.