A preconcentration/separation procedure is presented for the solid phase extraction of trace cadmium and lead ions as their 1-(2-pyridylazo) 2-naphthol (PAN) chelates in environmental samples on Chromosorb-106 resin, prior to cadmium and lead determinations by atomic absorption spectrometry. The preconcentration procedure was optimized by using model solutions containing cadmium and lead ions. The influences of pH of the model solutions, amounts of PAN, eluent type and volume etc. were investigated. Also the effects of the matrix constituents of the samples were also examined. Separation of cadmium and lead from real samples was achieved quantitatively. The procedure presented was checked with the analysis of microwave-digested standard reference materials (IAEA-336 Lichen and SRM 1515 Apple leaves). The preconcentration procedure was applied for the lead and cadmium contents of the natural water samples, some salts with satisfactory results (recoveries > 95 %, relative standard deviations < 8 %). © 2005 Elsevier B.V. All rights reserved.