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

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. © Akadémiai Kiadó, Budapest, Hungary 2012.

Jaar van publicatie:2012