A simple and rapid technique for the separation and preconcentration of lead in water and biological samples has been devised. Preconcentration is based on the deposition of analyte onto a column packed with dithizone immobilized on sodium dodecyl sulfate coated alumina at pH ≥ 3. The trapped lead is eluted with 5 mL of 4-M nitric acid and determined by flame atomic absorption spectroscopy. A sample of 1 L, results in a preconcentration factor of 200, and the precision at 20 µg L −1 is 1.3% (n = 8). The procedure is applied to tap water, well water, river water, vegetable extract and milk samples, and accuracy is assessed through recovery experiments and by independent analysis by furnace atomic absorption.