The renovated silver ring electrode in determination of lead traces by differential pulse anodic stripping voltammetry
- 作者：Bogusł ; aw Baś ; Mał ; gorzata Jakubowska
- 关键词：Silver electrode ; Underpotential deposition ; Stripping voltammetry ; Mercury-free electroanalysis ; Trace analysis ; Lead
- 刊名：Analytica Chimica Acta
- 出版年：2008
- 期刊代码：2_00032670
- 类别：ch
- 出版时间：12 May 2008
- 卷：615
- 期：1
- 页码：39-46
- 文件大小：547 K
摘要
The study of a new type of working electrode – the renovated silver ring electrode (RSRE) – for lead ions detection via differential pulse anodic stripping voltammetry (DP ASV) without removal of oxygen is reported. The only four constituents of the RSRE: a specially constructed silver ring electrode, a silver sheet used as silver counter/quasi-reference electrode and a silicon O-ring, are fastened together in a polypropylene body. The renovation of this electrode is carried out through mechanical removal of solid contaminants and electrochemical activation in the electrolyte which fills the RSRE body. Excellent repeatability and reproducibility – also in organic samples solutions – were reached in a period of a few weeks through the renovation of the electrode surface before each measurement. The reduction and stripping of lead on silver electrode under the DP ASV conditions are underpotential deposition/dissolution phenomena. The RSRE is used for the determination of Pb ions in concentrations ranging from 1 × 10−9 to 1 × 10−7 M. The repeatability of DP ASV runs in synthetic solutions covering the entire concentration range is better than 2%. Obtained calibration curves are represented by a correlation coefficient of at least 0.999. The detection limit (LOD) for the time of electrodeposition equal to 60 s is 0.2 × 10−9 M. LOD for Pb2+ detection at the RSRE is similar to this reported for a rotating silver electrode in subtractive anodic stripping voltammetry (E. Kirowa-Eisner, et al., Anal. Chim. Acta, 385 (1999) 325). The analysis of Pb2+ in synthetic solutions with and without surfactants, certified reference materials and natural water samples have been performed.