We have synthesized Ni-ZnO nanoparticles (NPs) by a wet-chemical route using reducing agents. Thestructural and optical properties of Ni-ZnO NPs were investigated by various conventional methods. Theanalytical potential of the Ni-ZnO NPs was studied for a selective detection of toxic Pb(II) ion usingrecognized ICP-OES method for environmental remediation. Data obtained from the selectivity studyindicated that the selectivity of Ni-ZnO NPs phase was the most toward Pb(II) ion. However, theadsorption isotherm data of Pb(II) on Ni-ZnO NPs phase was good-match with the Langmuir-Adsorption-Isotherm, strongly supporting that the adsorption process was mainly monolayer on homogeneousadsorbent surfaces.