A separation-enrichment system based on adsorption of cadmium(II) and lead(II) ions as their 1-phenyl-1H-tetrazole-5-thiol chelates on Diaion SP-207 polymeric resin has been established. Flame atomic absorption spectrometry was used for the determination of cadmium and lead. Analytes were recovered ( >95%) on 0.5 g Diaion SP-207 at pH 6.5 and 4.5 mg of 1-pheny1-1H-tetrazole-5-thiol at 1.5 ml min(-1) flow rate. Cadmium and lead were desorbed by 10 ml of 1 M CH3COOH. The influences of some 1A and 2A group metals, transition metals on the recoveries of analyte were also investigated. Addition/recovery tests were performed. The accuracy was checked by the analysis of TMDA 54.4 fortified lake water certified reference material. The proposed procedure was applied for the analysis of analyte in real samples with successful results. (C) 2012 Production and hosting by Elsevier B.V. on behalf of King Saud University.