Adsorption of Pb(II) was studied using a novel xanthated carboxymethyl chitosan (XCC). The XCC was synthesized using the xanthation reaction of N-carboxymethyl chitosan (NCMC). The chemical structure of XCC was characterized by UV–visible spectra. The effects of initial pH value of the solutions, contact time and adsorption isotherms on adsorption of Pb(II) were investigated. Moreover, the possible adsorption mechanism was identified using Fourier transform infrared spectroscopy (FTIR) and X-ray photoelectron spectroscopy (XPS). The experimental results showed XCC experienced a high adsorption capacity. The adsorption isotherm followed the Langmuir model. The maximum adsorption capacity obtained from the Langmuir model was 520.8 mg/g. Thermodynamic studies revealed a spontaneous and exothermic adsorption process. FTIR and XPS studies showed that the carboxyl groups, nitrogen atoms and sulfur atoms participated in the adsorption of Pb(II).