In situ electrochemical generation of gold nanostructured screen-printed carbon electrodes. Application to the detection of lead underpotential deposition

In the present work, an electrochemical method for the reproducible and stable generation of gold nanostructures on the surface of screen-printed carbon electrodes was developed. This technique is based on the application of a constant current over an appropriate time interval. Gold nanostructured screen-printed carbon electrodes were characterized using both SEM and electrochemical methods. The mean diameter and the dispersion of gold nanoparticles that were generated electrochemically depended on the gold concentration, the time deposition and the current intensity. Smaller diameters and better distribution of nanoparticles were obtained when a shift of potential to −0.70 V occurred during the gold electrodeposition process. Moreover, the underpotential deposition (UPD) of lead on these nanostructured surfaces was studied, as was their behavior as array electrodes. The best results, using UPD combined with square wave stripping voltammetry, were obtained for gold nanostructured surfaces with a mean diameter of 78 ± 24 nm and a density of 4.4 × 107 nanoparticles/mm2. These gold nanostructured screen-printed carbon electrodes were obtained by applying a current intensity of −100 μA for 300 s using a gold concentration of 0.5 mM. The reproducibility and limit of detection obtained using these nanostructured electrodic surfaces were 2.4% (in terms of RSD) and 0.8 ng/mL, respectively.