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

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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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Authors and Affiliations

  1. DSM Resolve, Geleen, The Netherlands

    Geert Vanden Poel, Daniel Istrate & Agnieszka Magon

  2. Department of Chemistry, Rzeszów University of Technology, 35-959, Rzeszow, Poland

    Agnieszka Magon

  3. SciTe, Geleen, The Netherlands

    Vincent Mathot

Authors
  1. Geert Vanden Poel
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  2. Daniel Istrate
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  3. Agnieszka Magon
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  4. Vincent Mathot
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Correspondence to Geert Vanden Poel.

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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

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