Calibration of magnitude and phase angle of TMDSC: Part 2. Calibration practice

In the first part of this paper we have discussed the influence of heat transfer in temperature-modulated differential scanning calorimetry (TMDSC) and its influence on the measured signals, in particular, magnitude and phase angle of effective complex heat capacity. Fundamentals of transfer theory were given within the framework of linear response. On this basis different calibration methods were suggested which enable to correct the influence of heat transfer on the measured (effective) complex heat capacity in TMDSC. In the second part of the paper, we apply the different calibration methods to a single set of experimental data to compare the results with the expected ones, and to draw conclusion concerning the calibration method in question and the frequency range where the calibration algorithm works. The example has shown that the more simple calibration procedures lead to nearly the same uncertainties of the results in everyday measurements as the more sophisticated “third order” calibration procedure does. However, we recommend the “third order” calibration procedure in all cases where the heat transfer conditions could change during the measurement.