Abstract

The simultaneous detection of oxygen (O2) and hydrogen peroxide (H2O2) in neutral media was investigated by cyclic voltammetry using a two-working modified glassy carbon (GC) electrode system. Both electrodes were functionalized either by electrodeposited or by chemically-prepared gold nanoparticles (AuNPs). AuNPs electrodeposition was achieved by constant potential electrolysis either at 0.5 or ‐0.5 V/SHE in acidic HAuCl4 solution. Colloidal AuNPs were obtained according four different procedures (type A to D) derived from the classical Turkevich synthesis and further drop-casted on GC. The kinetics of H2O2 oxidation was studied by recording steady-state voltammograms in a deaerated NaCl/NaHCO3 pH 7.4 neutral solution on all the functionalized electrodes and favorably compared to unmodified GC and bare gold electrodes. Both Koutecky-Levich and Tafel treatment of the current-potential curves showed that the highest anodic transfer coefficient αn (0.78 ± 0.14) was obtained with the electrodeposited AuNPs/GC electrode using the most cathodic deposition potential of ‐0.5 V which provided the highest average number of nanoparticles per square micrometer (555 ± 49 µm-2) of very little average size (25 ± 12 nm) NPs. The simultaneous detection and quantification of O2 and H2O2 was achieved only with electrodes functionalized using D-type Turkevich synthesis. In this case H2O2 was detected at the anode while current corresponding to O2 reduction was selectively recorded at a potential close to ‐0.3 V without interference from H2O2.

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