Abstract: Three TiDxTy films made on Mo substrates with about 5 m thickness were analyzed by using proton backscattering (PBS) method. The spectra show that the tritium profile can get an accurate analysis result, and the deuterium profile has a big bias due to the interference of the signal coming from the proton multi-scattered from the Mo substrate. The analysis results show that the T content and concentration measured by PBS method are coincident with the measurement results got in the samples during preparing process, and the tritium has an even distribution in Ti film. It is proved that the PBS method can be applied in T content and concentration analysis in materials.