In this study, a new chitosan derivative including vic-dioxime was synthesized by adding anti-monochloroglyoxime to chitosan (CS) at heterogeneous medium. The vic-dioxime-chitosan (v-DOCS) was characterized by elemental analysis (C, H, N), FT-IR and C-13 CP-MAS NMR spectroscopy. The degree of substitution (DS) of v-DOCS was evaluated by C-13 CP-MAS NMR spectroscopy and found to be 13.57%. As a result of the solubility test, unlike chitosan, v-DOCS were not dissolved in the aqueous solution of acetic acid. Metal complexes of v-DOCS with Co (II) and Cu (II) were synthesized and characterized by FT-IR and atomic absorption spectroscopy (AAS). Surface characterizations of CS, v-DOCS and v-DOCS-Copper (II) were performed by scanning electron. microscope (SEM). Thermal behaviors of the synthesized compounds were investigated by TG-DTA analysis. (C) 2007 Elsevier Ltd. All rights reserved.