Recently, Coughlin et al. have shown that a redox couple involving the oxidation of coal and the reduction of H+at the cathode and primarily CO2at the anode. We have examined the electrochemical behavior of various Kentucky coals and H‐Coal liquids at platinum electrodes under voltammetric and electrolytic conditions, and found that the reported electrochemical process is not a general one, and that Fe++may yield a similar phenomenon. Thus, agueous 0.1M LiClO4slurries of most coals were found to yield characteristic voltammograms containing anodic waves starting at +0.4 volts vs. SCE and extending throughout the positive potential range. The resulting oxidation currents were proportional in magnitude to the coal concentration employed. Upon filtration, the bulk of the electro‐activity of the coal slurry was found to be retained in the filtrate while the remaining coal residue showed drastically diminished currents upon formation of a new slurry. Atomic absorption analysis of the filtrate revealed iron concentrations in the parts‐per‐thousand range. It was determined that the half‐wave potential of Fe2+occurred at +0.45 volts under the conditions employed. Also, acetonitrile coal slurries and acetonitrile solutions of H‐Coal liquids exhibited no larger electrolysis currents than were obtained with blank solutions.