Abstract: Partition behavior of the coordination complex formed by Mo(Ⅵ) and 3,5-dibromosalicylflurone (DBSAF) between aqueous-salt phase and ethanol phase in an aqueous ethanol solution was studied. Under the optimum conditions of ① pH 1-6,② concn. of (NH4)SO4: 0.35 g·mL-1,③ volume ratio of ethanol to H2O in the test solution: 3 to 7,④ amount of 1×10-4mol·L-1 DBSAF solution added: 2.0 mL and ⑤ total volume of test solution: 10 mL,Mo(Ⅵ) was effectively separated from several common co-existing cations,e.g. Co(Ⅱ),Zn(Ⅱ),Ni(Ⅱ),Cu(Ⅱ),Mn(Ⅱ),Fe(Ⅲ) and W(Ⅵ). The rate of extraction of Mo(Ⅵ) was found achieving to values over 97%,while the extraction rates of co-existing cation were less than 5%.