Removal of Cu(II) and Ni(II) from aqueous solutions by a novel xanthated carboxymethyl chitosan (XCC) was investigated. XCC obtained was characterized by FTIR, SEM, EDX, and XRD. The adsorption ability of chitosan and XCC toward Cu(II) and Ni(II) was compared. The effect of pH (2.0-7.0), contact time (5-60min), and adsorption isotherms on adsorption were also investigated. It was observed that the modified chitosan XCC showed a remarkable increase in Cu(II) and Ni(II) adsorption as compared to chitosan and displayed a quick adsorption performance. Further, The Langmuir isotherm was found to provide the best correlation of the experimental data and the adsorption capacity obtained from the Langmuir model was 174.2mg/g and 128.4mg/g for Cu(II) and Ni(II), respectively. FTIR and UV spectra suggested that the amino groups, carboxyl groups, and xanthate groups of XCC participated in the adsorption.