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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(ED‐TA)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9.7×10-9~2.4×10-4、1.8×10-8~8.9×10-5mol/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、1.9×10-9mol/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%。

T he simultaneous determination of Pb2+ and Cd2+ in ZnCl2‐N H4 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 0.015 V/s . Pb2+ and Cd2+ showed sensitive stripping peaks at -0.48 V and -0.68 V ,respectively .The common i‐ons in solution had no interference with the determination .The concentration of Pb2+ and Cd2+ in range of 9.7 × 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 cor‐relation 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‐NH4Cl 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 .

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