By using a new adsorbent (sepiolite) an adsorption-elution and atomic absorption spectrometric method has been developed for the preconcentration and determination of Fe and Pb. Recoveries of the analytes were 82 +/- 3% for Fe and 91 +/- 2% for Pb at 95% confidence level. For Cu it was only 5 +/- 1%. The recovery of iron could be increased to about 97 +/- 1% by complexing with EDTA, the recovery of copper only to 57 +/- 2%. The optimised method was applied to the determination of lead in metal materials (e.g. brass).