A novel aminated chitosan was prepared with(NH4)2Fe(SO4)2 ·6H2O,NH4Fe(SO4)2·12H2O and chitosan base intermediate,through hydroxylpropyl and amination.The optimal conditions studied by orthogonal experiments were as follows: stirring speed was 1200r/min,the dosage of chitosan,epoxy chloropropane,ethylenediamine were 3.0g,5.0mL,2.5mL,respectively.The structure and morphology of magnetic microspheres were characterized by means of fluorescence microscopy.The results showed that Fe3O4 particles were embedded by aminated chitosan cayer.The magnetic microspheres' amine-group contents were 3.60mmol/g and they were paramagnetic and acid resistant sphereed with diameter 211.6nm.Finally,a test was done for the best possible conditions of the chitosan microspheres in the treatment of Cu2+ and Pb2+ capacity.