The solid-sate electrochemistry of organosulfur compounds existing in petroleum and its derived matrices is described using the voltammetry of immobilized microparticles methodology. Cyclic and square wave voltammogrammetric responses of sulfur compounds responsible of aging of asphalt pavements, namely, thiophenes, disulfides, sulfides, sulfoxides and sulfones were determined at compound-modified graphite electrodes in contact with 0.10 M H2SO4. The electrochemical oxidation/reduction products were characterized by attenuated total reflectance Fourier transform infrared spectroscopy (ATR-FTIR) and scanning electron microscopy with energy dispersion x-ray detection (SEM-EDX) coupled to electrolysis experiments. Different types of voltammetric response were detected depending on the solubility of the parent compounds and their products of oxidation/reduction, in several cases resulting in significant crystal re-structuring. Under the studied conditions, the oxidation of thiophenes, disulfides and sulfides yields sulfonic acid, sulfone compounds and some sub products in dissolution while sulfones can be reduced to thiols which experience subsequent oxidation processes.