AbstractA fast and facile synthesis of TiO2‐ Al2O3 nanocomposite based on Microwave (MW) irradiation is presented. The nanocomposite development were corroborated by X‐ray photoelectron spectroscopy (XPS), scanning electron microscope (SEM), energy‐dispersive X‐ray (EDX),and Fourier transform infrared spectroscopy (FT‐IR)analysis. The XPS analyzed results affirmed that elements on the nanocomposite surface were Al and O. Electrochemical properties of the as prepared TiO2‐Al2O3 nanocomposites were studied thoroughly to determine the sensing activity of the nanocomposites towards 3,4‐Diaminotoluene (3,4‐DAT) which is a harmful or hazardous chemical using I−V method. Selective electrochemical sensor using TiO2‐Al2O3 nanocomposite onto glassy carbon electrode (GCE) was assembled and the details electrochemical investigation of 3,4‐Diaminotoluene (3,4‐DAT) was developed. It was calibrated using in range of 3,4‐DAT concentration and data were plotted as current versus concentration. Considering the highest linearity (r2=0.99)of calibrated range, the linear dynamic range (1.0 pM∼ 1.0 μM) was found. Employing the slope of calibration curve, the sensitivity (0.5024×103 μAμM−1cm−3) and detection limit (0.19 ± 0.01 pM) were estimated. Besides this, the selective 3,4‐DAT chemical sensor was shown long‐term stability and precious reproducibility with very short response time without any interference effect.