The batch removal of Cr(VI) ions from aqueous solution using binary composite microspheres of chitosan and nanoparticles of iron oxide under different conditions has been investigated in this study. The influences of initial chromium concentration, contact time, pH, temperature, and solid-liquid ratio have been reported. The adsorption data was fitted well in the Langmuir and Freundlich models and various static parameters were calculated. The mechanism of adsorption was studied by Fourier Transform Infrared spectroscopy (FTIR).