摘要
报道了在碳糊电极上络合吸附阳极伏安法测定钯的新方法。在PH4．2的HAc-NaAc缓冲溶液中，钯（Ⅱ）与丁二酮肟（DMG）形成的络合物在0．20V（vs．SCE）搅拌富集60s，静止10S，然后在0．20～1.20V范围内以300mV／s的扫描速度线性扫描，在0．90V处产生灵敏的阳极吸附伏安峰。其二阶导数峰电流与钯（Ⅱ）的浓度在3．0×10～～8．0×10^-7mol／L范围内呈线性关系，富集120s，检出限达5．0×10^-10mol／L。本方法应用于催化剂中钯的测定，相对标准偏差为3．6％～4．7％，加标回收率在94％以上，结果与火焰原子吸收光谱法测定结果一致。
A sensitive complex adsorptive voltammetric method was developed for the determination of trace palladium at a carbon paste electrode（CPE）. The analysis was performed in HAc-NaAc buffer solution at pH 4.2 in the presence of dimethyl glyoxime （DMG）. A well defined anodic peak current was measured at 0. 90 V （vs. SCE）after stirring and accumulating for 60 s at 0. 20 V. The linear calibration range was 3.0×10^-9-8.0×10^-7 mol/L. The detection limit was 5.0×10^-10 mol/L for a 120 s preconcentration （S/N=3）. The proposed method was applied to the determination of Pd（Ⅱ） in catalyst samples with the RSD of 3.6%-4.7% and the recovery above 94%. The results are consistent with those obtained by FAAS.
出处
《冶金分析》
EI
CAS
CSCD
北大核心
2007年第10期23-26,共4页
Metallurgical Analysis
基金
中科院长春应化所电分析化学国家重点实验室基金(2005010)
湖南省教育厅基金(05B004)
关键词
钯
丁二酮肟
阳极吸附伏安法
碳糊电极
palladium
dimethyl glyoxime
anodic adsorptive voltammetry
carbon paste electrode
作者简介
黎拒难（1944-），男，教授，硕士，主要从事分析化学教学和科研工作，E-mail：junanli@xtu．edu．cn。
