The paper describes a new method for the rapid determination of Technetium (Tc) in sediment samples using solid-phase extraction chromatography (SPEC) with a novel methyl triphenyl phosphoniumnitrate (MTPN) resin. The effectiveness of the resin in selectively recovering Tc was evaluated in both batch and column mode and exploited for rapid analysis of ’Tc’. The procedure involves the acid digestion of samples, pre-concentration of fission products in supernatant and co-precipitation of actinides with Fe(OH)3, followed by selective recovery of Tc by SPEC using a column filled with MTPN resin. The recovered Tc was then radiometrically assayed using beta counting. The method was validated using IAEA certified reference materials and was found to provide reliable and reproducible results for the activity concentration of Tc-99 in sediment samples within 24 h.