Trace level voltammetric determination of lead and cadmium in sediment pore water by a bismuth-oxychloride particle-multiwalled carbon nanotube composite modified glassy carbon electrode

• Bi/MWCNT and BiOCl/MWCNT were synthesized and characterized by SEM and XRD.
• Bi/MWCNT and BiOCl/-MWCNT were applied as surface modifiers of glassy carbon electrode.
• Rapid, environmentally friendly, reliable trace level SWASV method was developed.
• BiOCl/MWCNT-GCE base method was tested for Pb2+ and Cd2+ determination in pore water.

Two multiwalled carbon nanotubes-based composites modified with bismuth and bismuth-oxychloride particles were synthesized and attached to the glassy carbon electrode substrate. The resultant configurations, Bi/MWCNT-GCE and BiOCl/MWNT-GCE, were then characterized with respect to their physicochemical properties and electroanalytical performance in combination with square-wave anodic stripping voltammetry (SWASV). Further, some key experimental conditions and instrumental parameters were optimized; namely: the supporting electrolyte composition, accumulation potential and time, together with the parameters of the SWV-ramp. The respective method with both electrode configurations has then been examined for the trace level determination of Pb2+ and Cd2+ ions and the results compared to those obtained with classical bismuth-film modified GCE. The different intensities of analytical signals obtained at the three electrodes for Pb2+ and Cd2+ vs. the saturated calomel reference electrode had indicated that the nature of the modifiers and the choice of the supporting electrolyte influenced significantly the corresponding stripping signals. The most promising procedure involved the BiOCl/MWCNT-GCE and the acetate buffer (pH 4.0) offering limits of determination of 4.0 μg L−1 Cd2+ and 1.9 μg L−1 Pb2+ when accumulating for 120 s at a potential of −1.20 V vs. ref. The BiOCl/MWCNT electrode was tested for the determination of target ions in the pore water of a selected sediment sample and the results agreed well with those obtained by graphite furnace atomic absorption spectrometry.

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