The introduction of tritium (T), with an initial kinetic energy of 2.7 MeV into the cavity of C60 using recoil implantation is studied in a 6Li(n,α)T activated homogenized compound matrix of Li2CO3 and C60. Radioactive endohedral T@C60 could be detected through the liquid scintillation spectrometry coupled with high-pressure liquid chromatography (HPLC). Fast atom bombardment mass spectrometry provided evidence for the retainment of C60 cage as against radiation damage. Solid state temperature-programmed desorption based on evolved gas showed the desorption of 3He gas (as a β− decay product from T) from the endohedral C60 cage at a higher temperature than the T2 and T2O trapped species at the defect sites and from the ordered crystallographic network of Li2CO3, respectively. The non-isothermal kinetics of the helium desorption, as a function of temperature evidenced a diffusion controlled process.