Performance and calibration of the Flash DSC 1, a new, MEMS-based fast scanning calorimeter

Autor: Agnieszka Magon, Geert Vanden Poel, Daniel Istrate, Vincent Mathot
Rok vydání: 2012
Předmět:
Zdroj: Journal of Thermal Analysis and Calorimetry. 110:1533-1546
ISSN: 1572-8943
1388-6150
DOI: 10.1007/s10973-012-2722-7
Popis: 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.
Databáze: OpenAIRE