Lead at trace concentrations is quantitatively extracted with 4.7 x 10(-4) M of cryptand 222B in tolune at pH 5.5 in the presence of 5 x 10(-4) M eosin as the counter ion. Lead from the organic phase is stripped with 1 M hydrochloric acid and determined by atomic absorption spectroscopy at 217 nm. Lead is separated from calcium, magnesium, zinc, copper which are associated within aquatic environment. It has been also separated from the multicomponent mixtures containing lead, cadmium, zinc; lead, cadmium, potassium, magnesium; and lead, cadmium, caesium and zinc. The method has been extended for the separation of lead from environmental samples containing effluents, sediments and aerosols.