Thermal Analysis and X-Ray Diffraction are – each one in its area – powerful methods for characterizing active pharmaceutical ingredients, excipients and formulations. However, the informative value of measurements can become even higher when these techniques are commonly applied. Thermal analysis is a widely used screening tool for determining temperature-induced changes in phases (DSC) and composition (TGA) and thus identifies temperature ranges worthy of being further investigated. There, X-ray Powder Diffraction (XRPD) can then be used to specifically inspect whether the structure of the material has changed and what kind of transformation has taken place. After a short introduction into the analytical methods, experts from both Malvern Panalytical and NETZSCH will provide practical guidance on how this powerful combination can be fully utilized.