Afast method for the preconcentration of thallium and silver in nanogram quantities in fresh drinking waters (source, well, tap) and waters for irrigation using colloidal precipitate flotation is described. Lead(II) hexamethylenedithiocarbamate, Pb(HMDTC)2 played the role of flotation collector. The experimental conditions for the successful separation of thallium and silver (mass of Pb, amount ofHMDTC-, pHof the system, induction time, type of surfactant etc.) were optimized. After flotation separation from the mother liquor, the solid sublate containing traces of thallium and silver was dissolved and the analytes were determined by electrothermal atomic absorption spectrometry (ETAAS). The results of the ETAAS analysis are compared with those obtained by inductively coupled plasma-atomic emission spectrometry. The detection limit for thallium by this method is 0.027 mg/l, and for silver 0.005 microg/l.