Phase change material (PCM) selection for particular applications mainly depends on its phase change temperature and latent heat, which were commonly measured by the differential scanning calorimetry (DSC). However, the DSC instruments are not absolute measuring devices and calibration is extremely important to ensure the accuracy of determined data. Meanwhile, the PCM with melting temperature between 0 and 65 °C is the most common interest for energy saving in buildings. This study, therefore, calibrated the DSC produce (NanoTechnology Inc.) by the high-purity metals with various regression methods for low melting temperature PCM thermal properties analysis. In the end, the paraffin n-eicosane was introduced to evaluate the accuracy of the temperature and latent heat measurements of the DSC. The experimental results showed that the accuracy of calibration could be improved by higher-order and more reference materials in a broad temperature range. However, the measurement results of n-eicosane proved that the 0-order regression method could offer good accuracy with only one suitable calibrant in a particular temperature range. Therefore, this research suggests the selection of reference materials for DSC calibration should consider the target of measurement temperature range as well as the thermal stabilities of calibrants.