The preparation of polymer carbon electrocatalysts by the controlled pyrolysis of polyfurfuryl alcohol polymer is described. Potentiostatic testing in oxygen-saturated KOH electrolytes is performed, and electrokinetic properties of the electrodes prepared from the electrocatalysts are presented and discussed. It is revealed that a pure polymer carbon electrode pyrolysed in powder form possesses a very high active area, displaying higher catalytic activity than a polymer pyrolysed in bulk. Suitable reduction mechanisms are proposed.