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In this study, the influence of oxygen diffusion on the physical properties of Ti–6Al–2Sn–4Zr–2Mo–0.1Si was examined. Measurements were carried out directly on sample cross sections which were preoxidized at high temperature. The lattice parameter evolution was measured using synchrotron X-ray diffraction and was coupled with microhardness and electron probe microanalyzer results with the aim of highlighting their relationships. The results show that the hardness and oxygen gradients along the oxygen diffusion zone in the alloy are similar to the evolution of the α-phase unit-cell volume quantified by X-ray diffraction. Linear relationships were found between these three parameters.