Hu Chengguo, Wu Kangbing, Dai Xuan, Hu Shengshui
Department of Chemistry, Wuhan University, Wuhan 430072, China.
Talanta. 2003 May 28;60(1):17-24. doi: 10.1016/S0039-9140(03)00116-4.
A simple and effective chemically modified carbon paste electrode (CMCPE) for the simultaneous determination of lead(II) and cadmium(II) was developed in this work. The electrode was prepared by the addition of diacetyldioxime into a carbon paste mixture. Pb(2+) and Cd(2+) were preconcentrated on the surface of the modified electrode by complexing with diacetyldioxime and reduced at a negative potential (-1.10 V). Then the reduced products were oxidized by differential pulse stripping. The fact that two stripping peaks appeared on the voltammograms at the potentials of -0.65 V (Cd(2+)) and -0.91 V (Pb(2+)) demonstrates the possibility of simultaneous determination of Pb(2+) and Cd(2+). Under the optimized working conditions, calibration graphs were linear in the concentration ranges of 1.0x10(-7)-1.5x10(-5) mol l(-1) (Pb(2+)) and 2.5x10(-7)-2.5x10(-5) mol l(-1) (Cd(2+)), respectively. For 5 min preconcentration, detection limits of 1x10(-8) mol l(-1) (Pb(2+)) and 4x10(-8) mol l(-1) (Cd(2+)) were obtained at the signal noise ratio (SNR) of 3. To evaluate the reproducibility of the newly developed electrode, the measurements of 5x10(-7) mol l(-1) Pb(2+) and Cd(2+) were parallel carried out for six times at different electrodes and the relative standard deviations were 2.9% (Pb(2+)) and 3.2% (Cd(2+)), respectively. Interferences by some metals were investigated. Only Ni(2+) and Hg(2+) apparently affected the peak currents of Pb(2+) and Cd(2+). The diacetyldioxime modified carbon paste electrode was applied to the determination of Pb(2+) and Cd(2+) in water samples. The results indicate that this electrode is sensitive and effective for the simultaneous determination of Pb(2+) and Cd(2+).
在本工作中,开发了一种用于同时测定铅(II)和镉(II)的简单有效的化学修饰碳糊电极(CMCPE)。该电极通过将二乙酰二肟添加到碳糊混合物中制备而成。Pb(2+)和Cd(2+)通过与二乙酰二肟络合而在修饰电极表面预富集,并在负电位(-1.10 V)下还原。然后,还原产物通过差分脉冲溶出法进行氧化。伏安图上在-0.65 V(Cd(2+))和-0.91 V(Pb(2+))电位处出现两个溶出峰,这表明同时测定Pb(2+)和Cd(2+)是可行的。在优化的工作条件下,校准曲线在1.0×10(-7)-1.5×10(-5) mol l(-1)(Pb(2+))和2.5×10(-7)-2.5×10(-5) mol l(-1)(Cd(2+))的浓度范围内呈线性。对于5分钟的预富集,在信噪比(SNR)为3时,Pb(2+)的检测限为1×10(-8) mol l(-1),Cd(2+)的检测限为4×10(-8) mol l(-1)。为了评估新开发电极的重现性,在不同电极上对5×10(-7) mol l(-1)的Pb(2+)和Cd(2+)进行了六次平行测量,相对标准偏差分别为2.9%(Pb(2+))和3.2%(Cd(2+))。研究了一些金属的干扰。只有Ni(2+)和Hg(2+)明显影响Pb(2+)和Cd(2+)的峰电流。二乙酰二肟修饰的碳糊电极应用于水样中Pb(2+)和Cd(2+)的测定。结果表明,该电极对于同时测定Pb(2+)和Cd(2+)灵敏且有效。