Abstract
This work presents the development and validation of an electroanalytical method for Pb(II) determination in a single drop. The electrochemical sensors used were an unmodified screen-printed electrode (SPE) and a Bi-film SPE (BiFSPE). Anodic square wave stripping voltammetry (SWASV) was performed at an accumulation potential of −1.5 V vs. Ag/AgCl and an accumulation time of 60 s. Electroanalysis with an unmodified SPE did not yield satisfactory results, whereas the BiFSPE was a much better analysis method. The linear concentration using the BiFSPE was in the range of 138.8–162.5 µg/L. The accuracy and precision were evaluated for different spiked concentrations, but the method using the unmodified SPE was neither accurate nor precise. Using the BiFSPE, the method was found to be both accurate and precise for Pb(II) determination at a concentration of 140.0 μg/L, with recovery and relative standard deviation (RSD) of 106.6% and 12.1%, respectively. In addition, using the BiFSPE, LOD and LOQ values of 1.2 μg/L and 3.3 μg/L were obtained, respectively. The possible interference effect on Pb(II) stripping signal was checked in the presence of Cd(II), Zn(II), Cu(II), Sn(IV), Sb(III), Hg(II), Fe(III), As(V), K(I), I−, Ca(II), and NO3−. Electrochemical impedance spectroscopy measurements were also performed for the unmodified SPE and BiFSPE. The application of single drop Pb(II) analysis was tested by real water sample analysis.
Highlights
The signal S is the peak height, i.e., ∆iPb(II), and N is the background noise
A volume consisting of a 60-μL drop of supporting electrolyte was dropped on the screenprinted electrode (SPE) and the square wave stripping voltammetry (SWASV) measurement was performed, followed by 10-μL additions of the solution with a known Pb(II) mass concentration (γPb(II) )
The electrode modification of the Bi-film SPE (BiFSPE) was performed in situ with 0.5 mg/L Bi(III) in
Summary
Publisher’s Note: MDPI stays neutral with regard to jurisdictional claims in published maps and institutional affiliations. If only a small sample volume is available The latter became possible with the development of screen-printing technology. These screen-printed electrodes (SPEs) are promising for on-site analysis [1]. The analysis of a single drop has not yet been widely reported
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