The separation behaviour of Mo and W from sulfuric acid solution by solvent extraction with Alamine 336 was investigated as a function of solution pH and extractant concentration. Selective extraction of Mo over W by Alamine 336 was obtained in the pH range of 3-5 with low amine concentration. The mixture of Alamine 336 and acidic extractants improved the separation factor between Mo and W and was in the following order: D2EPHA > PC88A > Decanol > Versatic acid. The stripping efficiency of Mo and W from the loaded mixture of Alamine 336 and D2EHPA was very poor, while complete stripping of Mo and W was possible from the mixture of Alamine 336 and Decanol by using a mixture of NH4OH and NH4Cl.