Different fields such as archaeology, biomedicine, forensic science, and pathology involve the analysis of burned bones. In this work, the effects of successive thermal treatments on pig long bones, measured by photothermal radiometry and diffuse reflectance are reported. Measurements were complemented by X-ray diffraction and infrared spectroscopy. Samples were thermally treated for 1 h within the range of 25 • C to 350 • C. The thermal diffusivity and reflectance increase in the low-temperature range, reaching a maximum around 125 • C and decaying at higher temperatures. These results are the consequence of complex modifications occurring in the inorganic and organic bone structure. For lower temperatures dehydration, dehydroxilation, and carbonate loss processes are dominant, followed by collagen denaturing and decompositions, which have an influence on the bone microstructure.