Polyvinylpyrrolidone (PVP) and poly(ethylene glycol) (PEG) solid dispersions with Felodipine or Hesperetin having up to 20 wt% drug were prepared using solvent evaporation method. Solid dispersions in comparison with their physical mixtures were studied using differential scanning calorimetry (DSC), wide-angle X-ray diffraction (WAXD), scanning electron microscopy (SEM) and hot stage polarizing light microscopy (HSM). PVP formulations with low drug load proved to be amorphous, since no crystalline Felodipine or Hesperetin drugs were detected using DSC and WAXD. Low and fast heating rates were applied for DSC study, to prevent changes in the samples caused during heating. Similarity between results of WAXD and DSC was also found in the case of physical mixtures, where the drug was in the crystalline state. However, though specific tests showed the high sensitivity of the DSC technique, it was difficult to arrive to reliable results for PEG solid dispersions or physical mixtures with low drug content by DSC, even by high heating rates. Crystalline drug could not be detected by DSC, leading to erroneous conclusions about the physical state of the drug, in contrast to WAXD. On the other hand, HSM proved the presence of small drug particles in the solid dispersions with PEG and the dissolution of the drug in the melt of PEG on heating. In such systems, in which a polymer with low melting point is used as drug carrier, DSC is inappropriate technique and must be used always in combination with HSM. The coupling of WAXD with thermal analysis, allowed complete physicochemical characterization and better understanding which is essential for a first prediction of dissolution characteristics of such formulations. (C) 2005 Elsevier B.V. All rights reserved.