In this study, we used a new simple chemical method to synthesise nanostructured magnesium aluminate (NMA) powder. Sol gel technique followed by sonication was used to develop different sensor samples namely NMA573, NMA873, and NMA1073 by calcination at temperatures of 573, 873, and 1073 K respectively. Average crystallite size of 18-27 nm and specific surface area of 68.09 to 61.84 m(2) g(-1) was obtained for the sensor samples. The existence of functional groups at 800 and 550 cm(-1) corresponding respectively to A106 group and the lattice vibration of MgO4 stretching were confirmed through FTIR studies; SEM/EDX confirm the spherical morphology with elemental composition Mg, Al and 0 at different calcination temperatures. UV-Vis absorption spectra show band gap energy as 3.50, 3.48, and 3.44 eV for the sensor samples NMA573, NMA873, and NMA1073 respectively. The effect of polyethylene glycol on the gas-sensing behaviour was studied in all the sensor samples. In particular, NMA1073 was found to have better resistance and sensor response for CO gas than NMA573 and NMA873. The effect of increase in calcination temperature of the sensor samples on the structural, morphological, optical, and gas response properties were carried out extensively to explore its gas sensing applications.