A procedure for simultaneous preconcentration and separation of traces of Zn(II) and Cd(II) has been described. It is based on the sorption on a chelating resin containing adenine moiety which has been synthesized by using microwave irradiation. The resulting resin was characterized by elemental analyses, infrared spectra and thermogravimetric analyses. The exchange capacity of the resulting resin for Zn(II) and Cd(II) was found to be 0.25 and 0.30 mmol g(-1) respectively at pH 1.0. In the column operation,the recoveries of Zn(II) and Cd(II) were 98.7+/-3.5 and 97.5+/-2.1% respectively at 97.5% confidence level for both. The detection limits were found to be 4.4 ng mL(-1) for Zn(II) and 9.0 ng mL(-1) for Cd(II). The loading half life (t(1/2)) periods were 14 and 12 min for Zn(II) and Cd(II) respectively. The mutual separation of Zn(II) and Cd(II) was carried out as a function of eluting agents. The reliability of the method has been tested by analysing NIES certified pond sediment sample. The developed method has been successfully applied in analysing industrial sludge samples.