Sb-doped SnO2/Ti anode was prepared in our lab with thermal decomposition method, and in the same time, the effect of heat treatment on the properties of the electrode also was studied. Scanning electron microscopy (SEM) was used to study the surface characterization of the electrodes. X-ray photoelectro-spectroscopy (XPS) measurements were carried out to study the chemical state of elements, Sn and Sb. The potentiodynamic polarization behaviors of the two anodes in different solutions were performed. Galvanostatic electrolyses were carried out at 5 mA/cm2 to study the electrocatalytic activity of the two anodes in removing organic pollutant. SEM showed that the electrodes had the same well-known cracked-mud structure, while the electrode annealed in O2 [SnO2/Ti(O2)] had more larger surface area than the electrode annealed in the air [SnO2/Ti(air)]. XPS measurements showed that the binding energies of both Sn3d(5/2) and Sb3d(5/2) of SnO2/Ti(O2) were 0.15 eV smaller than what of the SnO2/Ti(air) film. Both of the electrochemical measurements and electrolyses results confirmed that SnO2/Ti(O2) was more active in the degradation of organic pollutant. The galvanostatic electrolyses lasted until the solutions were decoloured throughly, 76.3% of total organic carbon (TOC) was removed with SnO2/Ti(O2), compared with 63.3% of SnO2/Ti(air). The similar exponential rules were driven for the variations of residual TOC concentration with two anodes.