Due to rapid industrialization, the presence of heavy metals in water and wastewater is a matter of environmental concern. Though some of the metals are essential for our system but if present beyond their threshold limit value (TLV), they are harmful and their treatment prior to disposal becomes inevitable. The present communication has been addressed for the removal of Cr (VI) from aqueous solutions by synthesized zinc aluminate novel nano-materials doped with copper (II); loaded and non-loaded with carbon spheres (CSs) using the co-precipitation technology. The as-prepared precursors of Cu(x)Zn(1-x)Al2O4 were annealed at 1000 oC for 2 h. The characterization of the samples nanoparticles were implemented by X-ray fluorescence (XRF), X-ray diffraction (XRD), transmission electron microscopy (TEM) analysis, photoluminescence spectra (PL) as well as the optical properties was demonstrated by UV–visible–near IR spectrophotometer. The optical properties of the prepared nano-materials and their catalytic performances are well discussed. Batch experiments were adopted for the adsorption of Cr (VI) from its solutions. The effect of doped copper ions and Cu (II) / CSs co-dopants on the behavior of ZnAl2O4 on removal of chromium was studied using inductively coupled plasma (ICP) analysis that had been used to measure removed and remaining Cr (VI) from its water polluted samples.