Removal of perchloroethylene using combined granular active carbon (GAC) adsorption and electrolysis is evaluated in this research. There is an interest in the regeneration of GAC using methanol solutions, because this process can obtain the almost complete desorption of the pollutant retained during the treatment of gaseous flows. In this work, the electrolysis of perchloroethylene (used not only as a hazardous pollutant but also as a model of organic pollutant) in methanol media containing sodium chloride and sodium hydroxide is evaluated and results are compared to those obtained during the electrolysis of this pollutant in aqueous media. Results demonstrate the feasibility of this treatment technology, which does not only remove the raw molecule but it is also capable to remove all the intermediates detected by GC-ECD, allowing the possibility of the reuse of the methanol solution for further regeneration steps.