Hydrogen peroxide sensing composite layers were prepared on Pt microwires by different approaches. A number of alternative preparation procedures were explored regarding not only changes in material and reagent composition but also different processing steps such as pretreatment, synthesis, polymerization and deposition of the sensing system constituents. Multiple-wall carbon nanotubes (CNT) and carbon black nanoparticles were used in this study. After optional oxidative pretreatment they were combined with ionic liquid, dispersion promoters and/or polymers and - essentially - with the Prussian Blue (PB) redox system, thus completing a hybrid layered structure. Various deposition techniques were employed: chemical, electrochemical (electropolymerization) or physical coating. Electroanalytical properties of the obtained microelectrodes were assessed by comparison of the cyclic voltammetry (CV) scans performed in physiological buffer solution (PBS) alone or with hydrogen peroxide added as the analyte.
The experimental results, showing correlations between observable electrocatalytic effects and structural properties of the composite layers resulting from their fabrication process, are comparatively displayed and briefly discussed. Cyclic voltammetric measurements confirmed that carbon nanomaterials improved and stabilized electrochemical parameters of the produced surface layers. The influence of CNT form (length, diameter) and surface modification resulting from covalent or non-covalent functionalization on their dispersion or interaction with the polymer matrix, metal substrate and the PB system could be also estimated. The structural effect is related to the facilitation of electron transport between the PB reaction centres and Pt substrate and stabilization of PB integrity within the layer.
The presented results have helped to select the promising microelectrodes for the assembly of the complete sensor for monitoring hydrogen peroxide level in biological systems.

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