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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。
The rock samples were separated and enriched with mercapto cotton in 1.2 mol / L HCl solution. The ICP and MS were used to determine Au and Pd. The sample decomposition, adsorption, elution conditions were studied. Experiments show that the use of mercapto cotton to enrich and select the appropriate isotopes to eliminate the interference of mass spectrometry, matrix matching method and the use of Re as an internal standard to correct the matrix effects and instrument fluctuations. The detection limits of Au and Pd were 0.13 and 0.22 ng / g, respectively. The method was used to analyze the standard materials. The analysis results were consistent with the certified values. The relative standard deviation (RSD, n = 9) was 4.8% ~ 8.3%, which met the analytical requirements of rock samples.