Dönmez Koray B, Çetinkaya Ebru, Deveci Seda, Karadağ Sevinç, Şahin Yücel, Doğu Mustafa
Materials & Chemical Research Department, Mir Araştırma ve Geliştirme A.S, 34220, İstanbul, Turkey.
Faculty of Science and Art, Department of Chemistry, Yıldız Technical University, 34220, İstanbul, Turkey.
Anal Bioanal Chem. 2017 Aug;409(20):4827-4837. doi: 10.1007/s00216-017-0426-3. Epub 2017 Jun 29.
A simple and rapid analytical method of determining Pb and Cd in water samples using an electrochemically pretreated pencil-graphite electrode (EP-PGE) is proposed for the first time in the literature. An electrochemically pretreated pencil-graphite electrode was prepared by performing potential cycling between -0.3 V and 2.0 V in 0.1 mol L HPO solution to improve its ability to electrochemically sense Pb and Cd ions. Square-wave anodic stripping voltammetry (SWASV) was used as the electroanalytical method. The electroanalytical parameters that influence the stripping determination of Pb and Cd were optimized based on experimental results. The magnitude of the peak oxidation current was adjusted in order to optimize the value of each parameter. Applying the resulting disposable electrode under the optimized conditions led to good selectivity and sensitivity in the determination of Pb and Cd ions. Interference from coexisting ions was also investigated. The resulting sensor was successfully tested by applying it to a standard reference water sample. Under the optimized conditions, the limits of detection were 0.46 μg L for Pb and 1.11 μg L for Cd using the electrode. Relative standard deviations (%RSD) were 2.76 for Pb and 2.85 for Cd. The linear working ranges of the electrode for Pb and Cd ion detection were 5-45 μg L and 10-40 μg L, respectively. Graphical abstract Preparation of nanoporous pencil-graphite electrode by cyclic voltammetry and stripping voltammetric screening of Pb and Cd.
本文首次在文献中提出了一种使用电化学预处理铅笔石墨电极（EP-PGE）测定水样中铅和镉的简单快速分析方法。通过在0.1 mol/L HPO溶液中于-0.3 V和2.0 V之间进行电位循环来制备电化学预处理铅笔石墨电极，以提高其对铅和镉离子的电化学传感能力。采用方波阳极溶出伏安法（SWASV）作为电分析方法。根据实验结果优化了影响铅和镉溶出测定的电分析参数。调整峰氧化电流的大小以优化每个参数的值。在优化条件下应用所得的一次性电极，在铅和镉离子的测定中具有良好的选择性和灵敏度。还研究了共存离子的干扰。将所得传感器应用于标准参考水样进行了成功测试。在优化条件下，使用该电极时，铅的检测限为0.46 μg/L，镉的检测限为1.11 μg/L。铅的相对标准偏差（%RSD）为2.76，镉的相对标准偏差为2.85。该电极用于铅和镉离子检测的线性工作范围分别为5 - 45 μg/L和10 - 40 μg/L。图形摘要 通过循环伏安法制备纳米多孔铅笔石墨电极并对铅和镉进行溶出伏安法筛选
