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Critical review of small sample calorimetry: improvement by auto-adaptive thermal shield control

MPG-Autoren
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Schnelle,  W.
Walter Schnelle, Inorganic Chemistry, Max Planck Institute for Chemical Physics of Solids, Max Planck Society;

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Gmelin,  E.
Max Planck Institute for Chemical Physics of Solids, Max Planck Society;

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Zitation

Schnelle, W., & Gmelin, E. (2002). Critical review of small sample calorimetry: improvement by auto-adaptive thermal shield control. Thermochimica Acta, 391(1-2), 41-49. doi:10.1016/S0040-6031(02)00162-4.


Zitierlink: https://hdl.handle.net/11858/00-001M-0000-0015-3113-D
Zusammenfassung
The paper reviews measuring and data computation procedures in heat-step calorimetry, for small samples (<100 mg mass) and at low temperatures (T < 100 K) under semi-adiabatic (isoperibol) measuring condition. In conjunction with an auto-adaptive heat- shield control, a method is described how the heat losses, occurring during an isoperibol measuring cycle, are correctly taken into account in order to achieve an absolute uncertainty of C-p of 1% or lower. The basic features of the method are strictly adiabatic condition at the beginning of each heat capacity measuring point, achieved by an extremely small temperature drift of the sample, and a very constant temperature of the heat-shield during the whole measuring cycle. (C) 2002 Elsevier Science B.V. All rights reserved.