Methane was electrochemically activated at room temperature to CH3OH, HCHO, CO and HCOO- and other low molecular weight oxygenates at room temperature using CO32- as an oxygen-donating species over a NiO-ZrO2 bifunctional electrocatalyst. Products were identified using Mass Spectrometry and H-1-Nuclear Magnetic Resonance Spectroscopy. O-2 and CO2 were also observed as products resulting from carbonate electrolysis and/or the oxygen evolution reaction.. Methane was adsorbed and activated by NiO while CO32- was adsorbed onto non-conducting ZrO2. Oxygen was then abstracted and donated from CO32- to electrocatalytically active sites to form new C-O or O-H bonds. This proposed low temperature electrochemical partial oxidation of methane may provide a new pathway for the synthesis of complex oxygenates and long chain hydrocarbons. (C) 2013 The Electrochemical Society, All rights reserved.