We have developed a facile and efficient tritium labelingmethod using a Pd/C−HTO−H2 system. This method canprovide multitritium-labeled compounds in highly dilutedHTO under T2 gas-free conditions, and is environmentallybenign since purification by silica gel column chromatography is not necessary, which causes a large quantity ofradioactive waste such as silica gel and eluent.