<p>Nanocrystalline nickel oxide (NiO) and copper oxide (CuO) have been synthesized in a water-in-oil microemulsion. The as-synthesized samples were characterized by X-ray diffraction (XRD), Electron Spin Resonance (E.S.R.), transmission electron microscopy (T.E.M.), and Specific Surface Area (S.S.A.). The particle size of nickel oxide and copper oxide can be controlled from 10.0 to 21.5 and 12.5 to 25.0 nm, respectively, at a different time of calcination temperature with a fixed proportion of water, surfactant, and oil in the microemulsion. Also, the results showed that the specific surface area (89.96 m² g^-1) and pore diameter (8.11 nm) of the prepared nano NiO are higher than the specific surface area (71.96 m² g^-1) and pore diameter (3.71 nm) of the prepared nano CuO. An adsorption test was carried out to show the efficiency of these prepared NiO and CuO nanoparticles for the Adsorption of T.N.T. in an aqueous solution. The removal efficiencies of both nano NiO and CuO were achieved at 90.06% and 77.0%, respectively.<strong></strong></p><p>Additionally, NiO and CuO nanoparticles were regenerated for five cycles. The Kinetic models of Pseudo first-order and pseudo-second-order were described. The results demonstrated that T.N.T. adsorption on both nano adsorbents follows the pseudo-second-order model.</p>