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In this work, two Tc radiochemical isolation methods—a conventional method by Triskem TEVA® resin and a rapid method by Empore™ Tc Rad Disk—are compared in the field of nuclear decommissioning and 99Tc assessment. The conventional method results more selective than the rapid one, being able to remove almost 100% of the main radiological interferers with the exception of the 90Y; however, the rapid method obtains higher chemical yields (97% vs. 80%) and slightly lower detection limits (0.025 Bq vs. 0.030 Bq) than the conventional. Both methods are similar with regards to equipment and reagent costs. [ABSTRACT FROM AUTHOR]