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本工作以Nafion树脂修饰玻碳电极为工作电极,饱和甘汞(SCE)为参比电极,铂片电极为对电极,考察了支持电解质、镀膜的厚度、富集电位、富集时间等实验条件对测量痕量银的影响并建立了差分脉冲溶出伏安法测定痕量银的方法。在0.1mol/LHNO3-0.1mol/LKNO3-0.001mol/LEDTA底液中,于-0.5V电位下富集300s,在+0.30V(vs.SCE)处有一灵敏的氧化峰。银的阳极溶出峰电流与银离子浓度在10~100μg/L范围内有良好的线性关系,检出限为0.05μg/L。将该方法用于钍中痕量银的分析,获得了满意的结果。
In this work, Nafion resin-modified glassy carbon electrode as working electrode, saturated calomel (SCE) as reference electrode and platinum electrode as counter electrode were used to investigate the experimental conditions of supporting electrolyte, coating thickness, enrichment potential and enrichment time The method of differential pulse stripping voltammetry was established for the determination of trace silver. In 0.1mol / L HNO3-0.1mol / LKNO3-0.001mol / LEDTA the bottom solution, enrichment of 300s at -0.5V potential, at + 0.30V (vs.SCE) at a sensitive oxidation peak. Silver anodic dissolution peak current and silver ion concentration in the 10 ~ 100μg / L range has a good linear relationship with a detection limit of 0.05μg / L. The method was applied to the analysis of trace silver in thorium and satisfactory results were obtained.