Neptunium and uranium behavior in extraction chromatography system, aiming the separation of microquantities of neptunium from uranyl nitrate solutions is described. Tri-n-octylamina (TOA), tri-n-butylphosphate (TBP), thenoyltrifluoroacetone (TTA) as stationary phase, alumina, Voltalef-UF-300, silica as support material were verified. The impregnation conditions as well as the best stationary phase/support material ratio were established. TBP/alumina, TBP/Voltalef and TOA/alumina system were selected to uranium and neptunium separation studies. In the system using TBP as extractant agent uranium and neptunium separation was reached by selective elution after the retention of both elements on the column. U-Np separation by selective retention of Np was possible with TOA system. The capacity of the column was the 66.6 mg U/mL and 191.6mg U/mL for the TBP/alumina and TBP/Voltalef systems, respectively. An application of extraction chromatography system in the final phase of irradiated uranium treatment process is proposed. (author).