The analysis of multi-phase pharmaceuticals, particularly when similar structures are involved (i.e. polymorphs, salts or hydrates), can often be a difficult task. Historically, x-ray powder diffraction (XRD) and differential scanning calorimetry (DSC) have been utilized to study pharmaceutical samples. Relative to other materials, diffraction data for pharmaceuticals are often complex due to the large number of diffraction maxima caused by the size of the molecule and/or the molecular symmetry. Multi-phase mixtures tend to have a large number of overlapping peaks which can hinder the difftactionist's ability to identify phases and interpret the data. When similar structures are analyzed calorimetrically, their thermal events may severely overlap (as will be shown), preventing accurate interpretation of the data. In addition there are several types of thermal events which may not be related to structural transitions. A common one in pharmaceuticals is the loss of solvent or absorbed (versus molecular) water.