The main objective of the present study is to separate the rhenium and molybdenum as well as recovery of the targeted metal ion. The behavior of extraction, stripping and separation possibilities of rhenium and molybdenum from molybdenite roasting dust leaching solutions using tri-otyl-amine (TOA) as an extractant has been investigated. From the results, 5 vol% TOA dissolved in kerosene is found to be selective for extraction of rhenium as compared with molybdenum. It extracted, molybdenum with extraction efficiency of less than 30%, whereas rhenium with extraction efficiency of more than ³99%. The optimum extraction conditions have been determined as: 5 vol% TOA, 900 s of contact time, 298 K temperature, 250 rpm agitation speed, phase ratio (organic/aqueous = O/A) of 0.4 at equilibrium pH 0.0. Stripping (back extraction of loaded metal) of rhenium from loaded organic phase with 5 kmol/m 3 HNO 3 was proved as efficient and the rhenium stripping efficiencies were obtained about 99% under conditions of O:A ratio of 1, for 900 s time, at 298 K temperature, at the same experimental condition whereas molybdenum stripped ³31%.