Chloromethylated polystyrene-divinylbenzene copolymer has been functionalized with 2-aminothiazole by using microwave irradiation. The resulting resin has been characterized by elemental analysis, thermogravimetric analysis, infrared spectra, water regain and metal sorption capacity. Various parameters like pH, equilibriation rate and sorption and desorption of metal ions, and effect of diverse ions have been studied. The maximum sorption capacities for Cd(II) and Hg(II) are 0.15 (pH 1) and 0.51 mmol(.)g(-1) (pH 6) respectively. The concentration of Cd(II) was measured by flame atomic absorption spectrometry while Hg(II) was measured by cold vapor atomic absorption spectrometry. The limits of quantification (10 sigma) values were found to be 5.70 and 0.14 ng mL(-1) for Cd(II) and Hg(II) respectively. The procedure has been applied to the determination of cadmium and mercury in certified biological samples after their dissolution by microwave-assisted treatment. The method is simple, rapid and free from interference and can be used routinely.