The present paper proposes a preconcentration procedure for lead determination using flame atomic absorption spectrometry (FAAS). It is based on lead(11) ions extraction as brilliant cresyl blue (BCB) complex and its sorption onto Diaion HP-2MG, a methacrylic ester copolymer. The optimization step was carried Out using factorial design and the variables studied were pH, shaking time and reagent concentration. In the established experimental conditions, lead can be determinate with a limit of detection of 3.7 mug L-1 lead (N = 20) and a relative standard deviation of 7% for a lead concentration of 100 mug L-1. The accuracy was confirmed by analysis of a certified reference material, the stream sediment furnished by National Research Centre for Certified Reference Materials (NRCCRM), China (GBW 073 10). Effect of other ions in the procedure proposed was also Studied. The method was applied for lead determination in real samples of water, tea, soil and dust. Tests of addition/recovery in the experiments for lead determination in water samples revealed that the proposed procedure Could be applied satisfactorily for analysis of these samples. (C) 2004 Elsevier B.V. All rights reserved.