Polyaniline-rhodium based electrocatalysts for the aqueous hydrogenation of organic compounds have been developed via two di screte methodologies. Sequentially deposited polyaniline/rhodium electrocatalysts, produced a polymer film which contained highl y dispersed rhodium particles. The activity of these polyaniline/rhodium electrocatalysts was found to be comparable to pure rhodium electrodes of a similar surface area. Under potentiostatic conditions, the catalysts were found to be active towards reduction of many simple hydrocarbon-based organic compounds and produced relatively high conversions over a period of ti me. The selectivity of this type of catalyst differed from that of pure rhodium electrodes, which has been attributed to the presence of the polyaniline. The method of producing co-deposited polyaniline(rhodium) electrocatalysts is currently novel, and creates a polymer with an extremely high level of dispersion of the rhodium within the polymer matrix. Activity of this type of electrocatalyst compared favorably with the sequentially deposited electrocatalysts only when the pH of the catholyte solution was maintained and the polymer film was thick. Several organic functionalities were tested on the most active electrocatalyst and it was found that a reasonable selectivity and activity for most organic functionalities was achievable under optimim conditi ons.