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高含量金样品均匀性的分析检验

         

摘要

利用王水溶样,残渣经氢氟酸、高氯酸分解-活性炭吸附-原子吸收光谱法测定了高含量金样品"哈测金-1"的15个子样中的全金量,并对子样进行了平行双份分析.考察了天平称量精度、玻璃器皿刻度精度和活性炭吸附率造成的测量不确定度,并估算出合成不确定度范围为2.5%~4.2%;论证了方法的可行性.对单个子样重复分析结果的可靠性及其算术平均值的极限误差进行了评估,计算出样品均匀性质量参数为0.70,依此判定该样品的均匀性质量等级为"良好".%15 samples, named "HACEAu-1", with high-content of gold were digested with aqua regia and the residues were decomposed with HF-HClO4. Gold in the sample solution was preconcentratcd by activated carbon adsorption and determined by FAAS. Duplicate analysis for 15 samples was carried out and the measurement uncertainty for the analytical results was evaluated. The main sources of measurement uncertainty came from sub-uncertainties of the analytical balance, scale accuracy of the analytical glassware, gold adsorption rate by activated carbon. The composed uncertainty was calculated with a range of 2.5% to 4.2%, which means that the method was feasible. The reliability for the results from duplicate analysis of single sample and the limiting error of its arithmetic mean value were also evaluated. The homogeneity quality coefficient of the sample was calculated as 0.70, which means that the sample was in "good" homogeneity quality grade.

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