Transient nuclear magnetic resonance (NMR) measurements on3He, generated by &bgr; decay and contained in aging titanium tritide (TiH1.8), have been carried out. The experiments were conducted over a period of about three years during which the rate of helium evolution from the sample abruptly increases. Qualitative analysis of the temperature dependence of the3He NMR correlates the onset of rapid increase in release rate with the precipitation of large bubbles within the solid. Further consideration suggests these bubbles are preliminary stages for release, since only a small fraction (<10%) of the3He in TiH1.8is ever observed in this configuration. This is the first data which directly infers3He bubbles at the time of release, although blisters have been observed in earlier experiments.