Cobalt oxide nanostructure (CoOxNS) deposited on the glassy carbon (GC) electrode surface is proposed as a novel electrocatalytic system for the reduction of para‐Nitrophenol. Cyclic voltammetry, electrochemical impedance spectroscopy, atomic force microscopy and scanning electron microscopy were used for characterization of deposited CoOxNS. CoOxNS deposited by cycling at positive potentials (0 to +1.3 V) show less charge‐transfer resistance (Rct) and more catalytic activity for the electroreduction of p‐nitrophenol compared to those CoOxNS obtained by scanning the applied potential throughout a negative V range. The GC/CoOxNS electrode showed good electrocatalytic activity toward the reduction of p‐nitrophenol at different pH values.
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