Metal oxide semiconductor is widely used as the sensing material for different gases. In this work Nickel Oxide (NiO) nanomaterialis used as the sensing layer for detecting Acetone gas. Acetone gas is proven to be the breath marker for diabetes. The Nickel Oxide nanomaterial is synthesized through microwave assisted Sol-gel process. The structural characterization of the NiO samples obtained were studied using X-ray diffractometer (XRD) and Scanning Electron Microscope (SEM). The gas sensing responseof the synthesized NiO nanostructures to 500 ppm acetone gas at room temperature was analyzed. The current of the sensing layer was observed decreasing, which indicates that acetone is a reducing gas. The response time, recovery time and the response of the sensor were also observed.