Correction of Errors in DSC Measurements Using Detailed Modeling of Thermal Phenomena in Calorimeter-Sample System

Measurements of quantities by differential scanning calorimetry (DSC) are influenced by intrinsic factors given by the construction limits of particular DSC devices. The position of temperature sensors outside the samples causes the produced experimental outputs to suffer from signal delay or partial signal consumption. Differences in sample mass and heating rate belong to other typical sources of errors that cannot be fully eliminated even by the experimental calibration. In this article, a computational method involving detailed modeling of thermal phenomena in the calorimeter-sample system is used for the correction of inaccuracies in DSC measurements. The applied model is able to extract pure data related to the sample itself, which is free of distortion. In a practical application of the method, lime hydrate samples of various mass are analyzed at first experimentally, while several different heating rates are used, and the influence of varying parameters on the obtained outputs is recorded. The experimental data are then reconstructed using computational modeling of thermal phenomena in the calorimeter-sample system. The corrected specific heat power values are found to be up to 9% higher and can be attributed to the heat capacity of inner parts of the device that consumes a part of the heat. The highest agreement between experimental and computational outputs is achieved when a sample filling one half of the crucible's volume is heated at 7 K · min
^-1
. Such a parameter choice shows a low-temperature shift (<; 5 °C), and the specific heat power difference is only 0.09 mW · mg
^-1
(3.4%).