Electrochemical Characterization of Modified Glassy Carbon Electrodes for Non-Enzymatic Glucose Sensors

The diversity of materials proposed for non-enzymatic glucose detection and the lack of standardized protocols for assessing sensor performance have caused considerable confusion in the field. Therefore, methods for pre-evaluation of working electrodes, which will enable their conscious design, are currently intensively sought. Our approach involved comprehensive morphologic and structural characterization of copper sulfides as well as drop-casted suspensions based on three different polymers-cationic chitosan, anionic Nafion, and nonionic polyvinylpyrrolidone (PVP). For this purpose, scanning electron microscopy (SEM), X-ray diffraction (XRD), and Raman spectroscopy were applied. Subsequently, comparative studies of electrochemical properties of bare glassy carbon electrode (GCE), polymer- and copper sulfides/polymer-modified GCEs were performed using electrochemical impedance spectroscopy (EIS) and voltammetry. The results from EIS provided an explanation for the enhanced analytical performance of Cu-PVP/GCE over chitosan- and Nafion-based electrodes. Moreover, it was found that the pH of the electrolyte significantly affects the electrocatalytic behavior of copper sulfides, indicating the importance of OH_ads in the detection mechanism. Additionally, diffusion was denoted as a limiting step in the irreversible electrooxidation process that occurs in the proposed system.