A new simultaneous DSC/X-ray measurement system was developed for the purpose of combining X-ray scattering data and calorimetric data. The DSC/X-ray measurement system was equipped with a conventional wide-angle X-ray diffractometer (WAXD). The phase transition behavior of pure hexatriacontane was measured by the DSC/WAXD, both on heating and cooling. The accuracy and reproducibility of the simultaneous DSC/X-ray instrument were comparable with the conventional DSC.