Urea-adduct process is commercially used to selectively separate n-alkanes from industrial hydrocarbon mixtures. Authors have explored application of this method for recovery of n-alkane based diluents from spent PUREX/UREX solvent. Traditionally this separation is performed by vacuum distillation, an energy-intensive process. The proposed method is simple and does not involve either exotic chemicals or complex processing steps. Application of urea-adduct process for recovery of diluent from spent solvent is reported here possibly first time in literature. Physical properties such as densities, viscosities and vapour pressure for irradiated organic solutions were also measured and reported.