Microscopic and electrochemical characterization of lead film electrode applied in adsorptive stripping analysis

• Published in: Electrochimica acta Vol. 54; no. 28; pp. 7214 - 7221
• Main Authors: Bobrowski, Andrzej, Kalcher, Kurt, Kurowska, Katarzyna
• Format: Journal Article
• Language: English
• Published: Kidlington Elsevier Ltd 01-12-2009; Elsevier
• Subjects: Adsorptive stripping voltammetry; AFM; Analytical chemistry; Chemistry; Electrochemical methods; Exact sciences and technology; In situ; Lead film electrode; SEM; AFM; SEM; Adsorptive stripping voltammetry; Lead film electrode; In situ; Atomic force microscopy; Electrochemical enrichment; Cobalt; Electrochemical characteristic; Surface structure; Electrodes; Lead; Modified material; Electrode adsorption; Scanning electron microscopy; Transition metal; Buffer solution; Carbon; Electrochemical detector; Heavy metal; Ammonia; Analysis; Thin layer electrode; Morphology; Nickel; Glassy state
• ISSN: 0013-4686; 1873-3859
• DOI: 10.1016/j.electacta.2009.07.052

Lead film electrodes (PbFEs) deposited in situ on glassy carbon or carbon paste supports have recently found application in adsorptive stripping voltammetric determination of inorganic ions and organic substances. In this work, the PbFE, prepared in ammonia buffer solutions, was investigated using scanning electron microscopy, atomic force microscopy and various voltammetric techniques. The microscopic images of the lead films deposited on the glassy carbon substrate showed a considerable variability in microstructure and compactness of the deposited layer depending on the selected experimental conditions, such as the concentration of Pb(II) species, the nucleation and deposition potential, and the time applied. The catalytic adsorptive systems of cobalt and nickel in a solution containing 0.1 ammonia buffer, 2.5
×
10
−5
M nioxime and 0.25
M NaNO
2 were employed to investigate the electrochemical characteristics and utility of the in situ prepared lead films.
The optimal parameters, i.e. the lead concentration in the solution, the procedure of film removal, and the time and potential of lead nucleation and film deposition for the adsorptive determination of metal traces, were selected, resulting in the very good reproducibility (RSD
=
4.2% for 35 scans) of recorded signals. The voltammetric utility of the lead film electrode was compared to that of glassy carbon, mercury film and bismuth film electrodes, and was subsequently evaluated as superior.