Abstract: A chitosancontaining glassy carbon electrode was found to give highly sensitive voltammetric wave for Pd(Ⅱ)-KCl-HCl system by anodic stripping voltammetry. Various conditions for the determination of trace Pd(Ⅱ) were studied. The optimum chitosan amount in glassy carbon was 1% 4 μL. In a solution of 0.02 mol/L KCl-HCl(pH=2), at 0.0 V, electrodeposited for 2 min or 1 min, scan rate was 0.1 V/s, the anodic stripping peak potential was at +0.67 V(vs.SCE). The peak current is proportional to the Pd(Ⅱ) concentration between 0.075-9.9 mg/L, r=0.999 3. 1.5 μg/L Pd(Ⅱ) was determined by electrodeposition for 10 min. The method was applied to the determination of palladium in catalyst. The possible mechanism of electrochemical reaction has been proposed by study of CV and UV.

Key words: chitosan, chemically modified electrode, palladium, anodic stripping voltammetry

摘要： 提出用脱乙酰壳多糖化学修饰电极为工作电极，阳极溶出伏安法测定痕量钯。在pH＝2的KCl-HCl底液中，+0.0V富集2min，以0.1V/s扫速阳极溶出，峰电位在0.67V(vs.SCE),Pd在0.075～9.9mg/L范围内与峰高呈良好的线性关系，相关系数r=0.9993。在富集10min时,可检测1.5μg/LPd，大大提高了测定灵敏度。样品测定结果满意。同时研究了该体系的电化学性质和电极过程机理。

关键词: 脱乙酰壳多糖, 化学修饰电极, 钯, 阳极溶出伏安法