The applicability of dispersion-free solvent extraction (DFSX), through rnicroporous hydrophobic membrane has been studied. The hollow fiber membrane contactor, with surface area of similar to 381 cm(2) was employed to extract U(VI) in macro concentration (35 dm(-3)) from aqueous acidic solutions. Prior to deployment of this technique for recovery of U(VI) from oxalate supernatant waste, chemical parameters such as extractant concentration, feed acidity, concentration of U(VI) in feed were studied. The Study revealed that 30% tri-n-biltyl phosphate (TBP) in n-dodecane as an extractant and feed in 3 M HNO3 gave an optimum extraction of U(VI) and it was possible to strip back utilizing 0.05 M HNO3. It was established to recover more than 90% of U(VI) from oxalate supernatant waste, which was often generated from nuclear chemical facilities. (C) 2007 Elsevier B.V. All rights reserved.