Synthesis and characterization of N,N,N',N'-tetrabutylsuccinamide (TBSA)was carried out and used for the extraction of U(VI) and Th(IV) from nitricacid solutions. Toluene was found to be the most suitable diluent for TBSAcompared with the other diluents tested. Extraction distribution ratios (D)of U(VI) and Th(IV) have been studied as a function of aqueous HNO 3 concentrations,NO3 – ion concentration, TBSA concentration and temperature.The results obtained indicated that U(VI) and Th(IV) are mainly extractedas UO2 (NO3 ) 2 . 2TBSA and Th(NO3 ) 4 . TBSA, respectively, and the IR spectra of the extractedspecies have been investigated. The values of thermodynamic functions havebeen calculated. Back-extraction of U(VI) and Th(IV) from organic phases wasalso studied.