火焰原子吸收光谱法测定锡基合金中痕量银

摘要

With sample dissolved by HCl and HNO3 , a determination method of silver in tin-based alloy by flame atomic absorption spectrometry was established. The effect of HCl and HNO3 dosages on the recovery rate of Ag+ was investigated. The results showed that, when the concentration of Ag+ in solution was 0. 1-20 μg/mL and 10-20 mL of HCl and 3 mL of HNO3 were added, Ag+ and Cl- complexed most completely, which formed [AgCl4]3-. The recoveries were 98. 6 ％-107. 1 ％. In this study, the sample was dissolved with 10 mL of HCl and 3 mL of HNO3. The copper ion and other trace ions had no interference with the determination. The detection limit of method was 0. 00 6 μg/mL. Three tin-based alloy samples were determined, and the relative standard deviations (RSD) were 0. 29 ％-0. 31 ％. The determination results of this method were compared with those obtained by ICP-AES and the values were consistent.%采用HCl和HNO3溶解样品,建立了火焰原子吸收光谱法测定锡基合金中银的方法.考察了不同的盐酸、硝酸用量对Ag+回收率的影响,试验结果表明:当溶液中Ag+浓度在0.1～20μg/mL,加入10～20 mL HCl、3 mLHNO3时,Ag+与Cl-络合得最完全,生成[AgCl4]3-,回收率在98.6%～107.1%之间,实验选择加入10 mL HCl和3 mL HNO3溶解样品.样品中的铜离子及其它痕量离子不干扰测定,方法检出限为0.006μg/mL.对3个锡基合金样品进行测定,相对标准偏差在0.29%～0.31%之间;本法与ICP-AES法的测定值进行对照,结果相一致.