Abstract
For the new Flash DSC 1, the temperature windows-to-operate—the temperature ranges where the real, achieved scan rate is constant—have been determined for unloaded sensors under various conditions like purge gas and flow rate variations; cooling to −90 °C and heating to 450 °C; scan rates from 1 up to 20,000 °C s−1 in heating and 15,000 °C s−1 in cooling. Compared to nitrogen, helium purge gas offers better access to low-temperature transitions and enables faster cooling. Drawback is the decreased temperature window-to-operate in heating at the high-temperature side. The temperature calibration protocol according to the recent DIN SPEC 91127 for sample mass and scan rate was found to be useful. The correction factors are maximal −1.4 °C as measured for 1 μg at 1,000 °C s−1 heating. Using liquid crystalline substances it was proved that the Flash DSC 1 has symmetry, meaning that calibration data found in heating also can be applied in cooling.
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Acknowledgements
The authors like to acknowledge the contributions of the following members of the thermal analysis department of DSM Resolve: Wil van Eijk and Asifur Rahman. Support for SciTe from the Dutch Ministry of Economic Affairs/SenterNovem TSGE3009 is greatly acknowledged, as well as from the EU-FP7-NaPolyNet/Coordination Support Action NMP-2007-2.1-3/Characterization of nanostructured materials, see http://www.napolynet.eu.
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Poel, G.V., Istrate, D., Magon, A. et al. Performance and calibration of the Flash DSC 1, a new, MEMS-based fast scanning calorimeter. J Therm Anal Calorim 110, 1533–1546 (2012). https://doi.org/10.1007/s10973-012-2722-7
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DOI: https://doi.org/10.1007/s10973-012-2722-7