[en] A novel, highly sensitive, isotope-dilution analytical technique for the determination of technetium-99 has been developed around single ion-exchange bead mass spectrometry. Mass spectrometry is much more sensitive than direct counting for the low-energy, low-specific activity, Tc-99 isotope. Further, the point source provided by a single ion-exchange bead leads to a greater signal-to-noise ratio in the mass spectrometric measurement than does conventional application of a solution to the source filament. Recent results indicate a sensitivity greater than 0.1 picogram. Isolation of technetium from the samples occurs after addition of Tc-97 as a yield tracer. A combination of ion-exchange chromatography and ion-association solvent extraction provides decontamination from the potential interferences, Mo-97 and Ru-99. Subsequently, the technetium is loaded onto a pair of anion-exchange beads (diameter approx. 0.3 mm). The noncritical isolation and bead-loading scheme typically concentrates the technetium in the sample by a factor of about a million with overall recoveries exceeding 50%. A variety of environmental samples from the Savannah River Plant (SRP) has been analyzed by this method