The paper reports a new rapid radioanalytical procedure for the determination of plutonium (Pu) in sediments by solid phase extraction chromatography (SPEC) using Bis-(2-ethylhexyl) carbamoyl methoxy phenoxy-bis-(2-ethylhexyl) grafted resin, abbreviated as Benzodioxodiamide (BenzoDODA) grafted resin. The resin was synthesized and evaluated for its sorption behaviour towards Pu in batch and column mode to determine its efficacy for selective recovery of Pu from sediment samples. The analytical procedure was based on the radiochemical separation of samples by acid digestion, followed by preconcentration of actinides by co-precipitation with Fe (OH)₃ and finally selective recovery of Pu by SPEC using a column filled with BenzoDODA grafted resin. Pu was then radiometrically assayed by preparing alpha disc sources with electro-deposition followed by alpha spectrometry. The method was further validated with IAEA reference materials. This method gives reliable and reproducible results for the activity concentration of Pu in sediment samples within 24 h.