A very effective sorbent material which exhibits exceptional capture of hexavalent uranium from other actinides and lanthanides at mu g g(-1) level, features pyridine 2,6-dimethanol immobilized onto alumina. The maximum sorption capacity for dioxouranium(VI) was found as 1.96 mmol g(-1) at pH 3.0. The adsorbed uranium complex was eluted completely by 0.05 mol L-1 (NH4)(2)CO3 solution and the concentration of hexavalent dioxouranium ion was monitored spectrophotometrically using Arsenazo III. The structure of the chelated uranium complex has been confirmed by single crystal X-ray structure analysis and Fourier transform infrared red (FTIR) spectroscopy. Thermo gravimetric analysis/differential thermo gravimetric analysis (TGA/DTG) of the chelated uranium complex was performed. The method is reproducible with a relative standard deviation (RSD) of 1.2% (N = 10) and the three sigma detection limits (N = 15) 1.2 mu g mL(-1) respectively. A pre-concentration factor, almost 500, for uranium was achieved. Interferences from Th4+, Mn2+, Ni2+ and Cu2+ ions were masked with ethylene diamine tetra acetic acid (di-sodium salt) (Na(2)EDTA) in the aqueous phase. The developed method has been tested for uranium recovery and estimation in some certified reference materials and environmental samples. (C) 2010 Elsevier B.V. All rights reserved.