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The synthesized MgTi2O4⋅TiO2⋅Zn2TiO4 nanomaterial was characterized by XRD (X‐Ray diffraction), SEM (Scanning electron microscopy), EDS (Energy dispersive x‐ray spectroscopy), FTIR (Fourier transform infrared spectroscopy) and PL (Photoluminescence) study. Particles size of MgTi2O4⋅TiO2⋅Zn2TiO4 nanomaterial was found to be 37.3 nm. PL and PLE (Photoluminescence excitation) spectra are showed several peaks including one red PL at 723 nm, when excited at 320 nm. Nanomaterial was subject to electrochemical sensor study. Thin layer of synthesized MgTi2O4⋅TiO2⋅Zn2TiO4 nanomaterials was fabricated onto the glassy carbon electrode (GCE) with conducting binder to result the working electrode of 4‐nitrophenylhydrazine (4‐NPHyd) sensor, which was applied successively to selectively detect the 4‐NPHyd in aqueous phase. The 4‐NPHyd chemical sensor exhibited high sensitivity with lower detection limit, long‐term stability in chemical environment and improved electrochemical responses during sensing performance. The linearity of calibration plot is obtained over the large linear dynamic range (LDR) from 0.1 nM to 0.1 mM of 4‐NPHyd. The sensitivity calculated from the slop of calibration plot (ratio of current to concentration of 4‐NPHyd) is 42.7215 μAmM−1cm−2 with detection limit (DL) of 0.02±0.001 nM at signal to noise ratio of 3(S/N). Therefore, the chemical sensor based on MgTi2O4⋅TiO2⋅Zn2TiO4 nanomaterials may be a promising highly sensitive sensor in electrochemical method for the effective detection of hazardous and carcinogenic chemicals in medical as well as biological sectors. [ABSTRACT FROM AUTHOR]