TIC working electrode. Voltammetric characteristics and application for determination of lead traces by stripping voltammetry

被引:15
作者
Bas, B. [1 ]
Piech, R. [1 ]
Niewiara, E. [1 ]
Ziemnicka, A. [1 ]
Stobierski, L. [1 ]
Kubiak, W. W. [1 ]
机构
[1] AGH Univ Sci & Technol, Fac Mat Sci & Ceram, PL-30059 Krakow, Poland
关键词
titanium carbide; underpotential deposition; stripping voltammetry; lead; trace analysis; mercury-free electroanalysis;
D O I
10.1002/elan.200804229
中图分类号
O65 [分析化学];
学科分类号
070302 ; 081704 ;
摘要
The TiC working electrode was tested as a novel, potential electrode for anodic stripping voltammetric determination of lead(II) ions traces. To demonstrate the practical applicability of the TiC electrode, all underpotential deposition/dissolution (UPD) phenomena system in electrolyte without removal of oxygen was tested. The electrode was constructed be means of mounting a TiC. disk (circle divide = 3.5 mm) in a resin body. Three compositions of TiC were tested differing in stoichiometry, namely TiC0.6, TiC0.8, and TiC1.0, The key problem is the method of electrochemical activation of the TiC electrode. No or improperly activated electrode is not polarized and is unsuitable as a voltammetric sensor. The TiC electrode was used for the determination of Ph2+ 2 in concentrations ranging from I to WOW. The instrumental parameters, composition of supporting electrolyte and procedures of the electrode activation were optimized. The repeatability of DP ASV runs in synthetic solutions covering the entire concentration range is better than 3%. The calibration curve is characterized by a correlation coefficient of at least 0.999. The detection limit was 2 nM for an electrodeposition time of 30 s. ne method enables determination of Pb2+ in the presence of, among the others. high excesses of Cd, Cu, In, Sb, Se, and Tl ions as well as surfactants, Triton X-100 and humic acids. The analvsis of Ph2+ in synthetic solutions with and without surfactants, certified reference material and natural water samples have been performed. The voltammetric data were associated with the structural characterization of the electrode surface using scanning electron microscopy (SEM) and X-ray fluorescence spectroscopy (XRF).
引用
收藏
页码:1655 / 1664
页数:10
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