Gas sensing properties of ZnO nanobelts synthesized using carbothermal reduction method has been investigated. At room temperature (28 °C), the sensor films exhibit an appreciable response towards H2S and NO and response of these two gases were studied as a function of concentration. For NO the sensor films exhibit a complete reversible curve for the concentration range between 1 and 60 ppm. However, for H2S a complete recovery was obtained for concentration <5 ppm and for higher concentration a partial recovery of the baseline resistance was observed. The reason for the incomplete recovery was investigated using X-ray photoelectron spectroscopy (XPS) and X-ray diffraction (XRD) studies of the sample before and after the H2S exposure. After exposure, appearance of an additional peak at 26.6° corresponding to the formation of ZnS was observed in XRD. Formation of additional phase was further corroborated using the results of XPS. H2S exposure causes decrease in the intensity of O 1s peak and appearance of sulphide peaks at binding energies of 162.8 and 161.8 eV corresponding to S-2p peaks – 2p3/2 and 2p1/2, confirms the formation of ZnS upon exposure.