Cyclic voltammetry (CV) and preparative electrolysis techniques were used to investigate the reduction of nitrobenzene into (NB) p-aminophenol (p-Ap). The electrodes used in CV experiments were glassy carbon (GC), TiO2/Ti, Sn and Pb. The preparative electrolyses were carried out by the use of Pb, Sn, carbon cloth and TiO2/Ti electrodes. The CV data were evaluated according to Nicholson-Shain criteria, and it was deduced that the reductions on TiO2/Ti and GC electrodes were irreversible and monitored by an electrochemical-chemical-electrochemical mechanism. No reduction peak was observed with Sn and Pb electrodes. Preparative electrolyses were carried out under current-control led conditions in the presence and absence of solvent. The best yield of (p-Ap) was obtained with a circulating neat NB electrolysis system on a TiO2/Ti electrode.