Amidoximated bagasse (Am-B) was prepared by treating sugarcane bagasse fibers with acrylonitrile in the presence of sodium hydroxide followed by aqueous hydroxyl amine. Adsorption of some heavy metal ions, namely, Cu(II), Hg(II), Ni(II), Cr(III), and Pb(II) on the prepared Am-B at different metal ion concentration, intervals, and temperatures was studied. Also, the selectivity of the prepared Am-B toward adsorption of the aforementioned metal ions in an equimolar mixture was studied. The effect of regeneration of Am-B using ethylenediamine tetraacetic acid disodium salt (EDTA), up to five times, on its adsorption capacity of the aforementioned metal ions was investigated.