An extraction chromatographic separation scheme has been developed using impregnated resin for the processing of actual plutonium contaminated solid analytical assorted waste. The effluent obtained on anion exchange chromatography during plutonium purification step was processed by tri-n-butyl phosphate (TBP) and tetra 2-ethylhexyl diglycolamide (T2EHDGA) augmented XAD-4 resin to remove uranium and americium, respectively, while Ag ion was electrochemically separated further. The augmentation of TBP and T2EHDGA functionalities on XAD-4 have been evidenced by FTIR spectroscopy, TG and DSC analysis. The modification in surface morphology on augmentation has been investigated by SEM, while elemental mapping and EDS heteroatom analysis indicated the successful functionalization/impregnation of the resin. In case of U removal by TBP augmented XAD-4 resin, starting from 3 gL À 1 feed in 7.2 M HNO 3 , a maximum of 93 % U was found to be loaded on the column, which can quantitatively be back extracted by 0.01 M HNO 3 . Despite ∼ 10 % reduction in loading capacity during the 3 rd consecutive cycle, the efficacy of this column chromatographic separation of U has been demonstrated successfully. The raffinate of this step was used as feed for Am 3 + separation using T2EHDGA-XAD-4. A maximum of 98 % loading and almost quantitative elution have been observed during this step and the performance recyclability has been checked for three consecutive cycles. The loading of U and Eu (Am analogue) has been evidenced by elemental mapping and energy-dispersive X-ray spectroscopy (EDS)analyses of loaded resin.