Microbial fuel cells (MFCs) are novel bioelectrochemical devices for spontaneous conversion of biomass into electricity through the metabolic activity of the bacteria. Microbial production of electricity may become an important source of bioenergy in future because MFCs offer the possibility of extracting electric current from a wide range of soluble or dissolved complex organic wastes and renewable biomass. However, the materials used in these devices are still not economic and researchers use different materials as cathode and anode in MFCs. This results in variable performance which is difficult to compare. We tested several commercially available materials for their suitability as anode in an acetate fed MFC. Besides, a novel non-platinized activated carbon (AC) based, gas porous air cathode was also tested. Both the anode and cathode were tested in a half cell configuration. Carbon cloth, graphite cloth and dynamically stable anode (DSA) served as ideal anode material with carbon cloth and graphite mesh reaching the open circuit voltage (OCV) of acetate oxidation (−500 mV vs. Ag/AgCl). The effect of increasing concentration of acetate on anode OCV was also investigated and results showed that on increasing the acetate concentration from 10 mM to 40 mM has no adverse impact on the anodic activity towards electrochemical oxidation of acetate. The AC cathode showed stable current (−1.2 mA/cm2) over a period of 100 days.