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阳极溶出伏安法测定氯化锌-氯化铵电解制锌体系中铅和镉
Determination of lead and cadmium in zinc chloride-ammonium chloride electrolyte system by anodic stripping voltammetry
【摘要】 采用阳极溶出伏安法,建立了在ZnCl2-NH4Cl体系中,使用乙二胺四乙酸二钠(EDTA)和磺基水杨酸消除Cu2+对Pb2+测定的影响,不经预分离同时测定溶液中Pb2+和Cd2+的方法。在扫描电位为-0.80-0.30V、富集电位为-0.85V、富集时间为100s、扫描速率为0.015V/s的优化试验条件下,Pb2+和Cd2+分别在-0.48V和-0.68V处有灵敏的溶出峰。溶液中可能存在的常见离子不干扰测定。Pb2+、Cd2+浓度分别在9.7×10-92.4×10-4、1.8×10-88.9×10-5 mol/L范围内与其峰电流呈良好的线性关系,相关系数分别为0.995和0.998。方法中Pb2+、Cd2+的检出限分别为3.9×10-9、1.9×10-9 mol/L。采用实验方法测定了ZnSO4电解液和ZnCl2-NH4Cl电解液中的Pb2+和Cd2+,结果的相对标准偏差(RSD,n=6)分别为0.83%2.1%、0.56%0.75%,回收率分别为89%108%、92%104%。
【Abstract】 The simultaneous determination of Pb2+and Cd2+in ZnCl2-NH4 Cl system by anodic stripping voltammetry was established without pre-separation.The influence of Cu2+on the determination of Pb2+was eliminated using ethylene diamine tetraacetic acid(EDTA)and sulfosalicylic acid as masking agent.The optimal determination conditions were as follows:the scanning potential was-0.80-0.30 V,the enrichment potential was-0.85 V,the enrichment time was 100 s,and the scanning rate was 0.015V/s.Pb2+and Cd2+showed sensitive stripping peaks at-0.48Vand-0.68 V,respectively.The common ions in solution had no interference with the determination.The concentration of Pb2+and Cd2+in range of9.7×10-9-2.4×10-4 and 1.8×10-8-8.9×10-5 mol/L showed good linearity to the peak current.The correlation coefficient was 0.995 and 0.998,respectively.The detection limit of Pb2+and Cd2+was 3.9×10-9 and 1.9×10-9 mol/L,respectively.The content of Pb2+and Cd2+in ZnSO4 electrolyte and ZnCl2-NH4 Cl electrolyte was determined by the proposed method.The relative standard deviation(RSD,n=6)was 0.83%-2.1% and 0.56%-0.75%,and the recoveries were 89%-108% and 92%-104%,respectively.
【Key words】 anodic stripping voltammetry; zinc chloride; ammonium chloride; lead; cadmium;
- 【文献出处】 冶金分析 ,Metallurgical Analysis , 编辑部邮箱 ,2016年04期
- 【分类号】O657.1;TQ132.41
- 【被引频次】3
- 【下载频次】129