This paper describes an investigation of the reduction of nitrobenzene to p-aminophenol by the use of CV, RDE and preparative electrolysis with Cu and Cu(Hg) electrodes. The preparative electrolyses of nitrobenzene were carried out at controlled current and controlled potential conditions using copper and amalgamated copper using a new semipilot (laboratory) scale system in the absence of an organic cosolvent. The effects of redox reagents and the concentration of nitrobenzene in catholyte added to the medium were also examined. The best results were obtained with 2.3% BiCl3 at nitrobenzene concentration of 0.144 g cm(-)3 catholyte. The most suitable electrode material was found to be amalgamated copper and the reduction of nitrobenzene to p-aminophenol was found to follow an ECE mechanism.