The electrochemical regeneration of an activated carbon, previously saturated with toluene by gas phase adsorption, was studied. Cathodic and anodic regeneration methods were analyzed using a small batch electrochemical cell. In both cases, a stripping efficiency close to 100% was obtained under appropriate conditions of potential, current, and time of electrolysis. Successive loading and regeneration cycles of the activated carbon were performed under cathodic conditions without loss of the adsorption properties of the activated carbon, thus achieving a high regeneration efficiency (close to 99%). This electrochemical method is very effective for regeneration of activated carbon compared to conventional thermal regeneration as it does not modify the porous texture of the material.