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提出了硫酸亚铁电位滴定金的方法,研究了贵金属合金的微波消解和预处理方法,讨论了提高滴定Au的准确度和精密度的条件,比较了本法与原《国家标准》和火试金分析方法。结果表明:用HCl-H2O2试剂通过微波加热可快速消解金、铂、钯合金样品。CuCl预分离大量的Pt、Pd、Rh、Ir和Sn等干扰元素后,在稀HCl介质中,用FeSO4电位滴定法测定质量分数3%~99.5%的Au,相对标准偏差为0.02%~0.22%,与库仑法和火试金法的分析结果吻合。方法已成功地应用于金、铂、钯等贵金属合金、金粉、首饰、自然金、溶液、冶金物料等试样中Au的测定。
The method of potentiometric titration of ferrous sulfate was proposed. The methods of microwave digestion and pretreatment of noble metal alloy were studied. The conditions of improving the accuracy and precision of titration of Au were discussed. Compared with the original “national standard” and fire test Gold analysis method. The results show that samples of gold, platinum and palladium alloy can be rapidly digested with HCl-H2O2 reagent by microwave heating. CuCl pre-separation of a large number of interfering elements such as Pt, Pd, Rh, Ir and Sn, measured in dilute HCl medium FeSO4 potentiometric titration of 3% to 99.5% by mass of the Au, the relative standard deviation of 0.02% to 0.22% , Consistent with the results of coulometry and fire assay. The method has been successfully applied to the determination of Au in the samples of precious metals such as gold, platinum and palladium, gold powder, jewelry, natural gold, solution and metallurgical materials.