A solid phase extraction procedure using Amberlite XAD-1180/Pyrocatechol violet (PV) chelating resin for the determination of iron and lead ions in various environmental samples was established. The procedure is based on the sorption of lead(II) and iron(Ill) ions onto the resin at pH 9, followed by elation with 1 mol/L HNO3 and determination by name atomic absorption spectrometry. The influence of alkaline, earth alkaline and some transition metals, as interferents, are discussed. ne recoveries for the spiked analytes were greater than 95%. The detection limits for lead and iron by FAAS were 0.37 mu g/L and 0.20 mu g/L, respectively. Validation of the method described here was performed by using three certified reference materials (SRM 1515 Apple Leaves, SRM 2711 Montana Soil and NRCC-SLRS-4 Riverine Water). The procedure was successfully applied to natural waters and human hair.