A flow injection analysis (FIA) system incorporation a microcolumn of immobilized oxine on surfactant-coated alumina had been devised for performing rapid thallium enrichment/matrix removal in flame atomic absorption spectrometry (FAA). The preconcentration is based on the deposition of thallium(I) on microcolumn and subsequent elution with 500 mu l of sodium thiosulfate (I mol 1(-1)). In the presence of EDTA, only TI(I) was retained on the microcolumn. Total thallium was determined after reduction of Tl(III) to Tl(I) by hydroxyl amine hydrochloride. A sample volume of 25 ml resulted in a preconcentration factor of 77. Precision at 30 mu g l(-1)` was 2.6% RSD (n = 10). With 25 ml sampling volume a detection limit of 2.5 mu g l(-1) was determined. The effect of potential interfering ions on the determination was studied. The method was applied for the determination of thallium in water, waste water, hair, nail, coal, and standard reference alloys. The accuracy was assessed through recovery experiment, independent analysis by Furnace-AAS, and analysis of certified reference alloys. 0 2007 Elsevier B.V. All rights reserved.