Wide potential windows were found at carbon nanotube film electrodes in neutral solutions after being treated with nitric acid and mixed acid. Electrochemical reversibility was investigated at carbon nanotube films with different pretreatments for ferri/ferrocyanide and quinone /hydroquinone. Carbon nanotube film electrodes presented quasi-reversible electrochemical behavior for both electrolytes. In the range of scan rate, carbon nanotube film electrodes treated with acids showed heterogeneous electron-transfer properties, which was mainly controlled by its electron state density on the surface of the film. On the whole, the carbon nanotube electrode with nitric acid treatment presented the best electrochemical behaviors, so we chose it as an analytical electrode to determine the trace compound in dilute solution. The results demonstrated that this new electrode material exhibits superior performance characteristics for the detection of azide anion. Wide potential windows were found at carbon nanotube film electrodes in neutral solutions after being treated with nitric acid and mixed acid. Electrochemical reversibility was investigated at carbon nanotube films with different pretreatments for ferri / ferrocyanide and quinone / hydroquinone. Carbon nanotube film electrodes presented quasi- reversible electrochemical behavior for both electrolytes. In the range of scan rate, carbon nanotube film electrodes treated with acids showed heterogeneous electron-transfer properties, which was mainly controlled by its electron state density on the surface of the film. On the whole, the carbon nanotube electrode with nitric acid treatment presented the best electrochemical behaviors, so we chose it as an analytical electrode to determine the trace compound in dilute solution. The results said that this new electrode material exhibits superior performance characteristics for the detection of azide anion.