The first application of tritium NMR spectroscopy to the direct observation of proton-exchange kinetics is described; this technique allows the study of milligram amounts of substrates and for substrates with multiple exchangeable positions. The examples include benzene and the ring and methyl positions of p-xylene reacting with cesium cyclohexylamide in cyclohexylamine, and the enolate positions of cyclohexanone and methyl 7,12-dihydroxy-3-ketocholan-24-oate reacting with heptafluorobutyric acid in dioxane.