先用恒电流电解重量法测定阳极铜中铜,然后通过原子吸收光谱法(AAS)测定电解残余液中铜,电感耦合等离子体原子发射光谱法(ICP-AES)测定沉积在铂阴极上的金、银等杂质元素,对电解重量法的测定结果进行修正.分别考察了电解条件、铂阴极干燥时间对分析结果的影响,结果表明,在设定电流为1.5 A时电解3.0~3.5 h后取出铂阴极,干燥3~5 min,可以获得较好的测定结果.按照实验方法测定阳极铜中铜,结果的相对标准偏差(RSD,n=11)小于 0.05%.方法用于铜合金标准物质IARM 71B中铜量的测定,测定值与认定值相一致.
The content of Cu in anode copper was firstly determined by constant current electrolytic gravimetry.Then, the content of Cu in residual electrolyte was determined by atomic absorption spectrometry.Moreover, the content of Au and Ag deposited on platinum cathode was measured by inductively coupled plasma atomic emission spectrometry to modify the determination results in electrolytic gravimetry.The influence of electrolysis conditions and dying time of platinum cathode on the analysis result was investigated.The results showed that the optimal testing conditions were obtained as follows: taking out the platinum cathode after electrolysis for 3.0-3.5 h when the current was 1.5 A followed by dying for 3-5 min.The content of Cu in anode copper was determined according to the experimental method.The relative standard deviations (RSD, n=11) were less than 0.05%.The proposed method was applied for the determination of Cu content in certified reference material of copper alloy (IARM 71B), and the found results were consistent with the certified values.
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