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

Schnelle, W.; Gmelin, E.

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

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Schnelle, W.
Former Scientific Facilities, Max Planck Institute for Solid State Research, Max Planck Society;

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Gmelin, E.
Former Scientific Facilities, Max Planck Institute for Solid State Research, Max Planck Society;

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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.

Cite as: https://hdl.handle.net/21.11116/0000-000E-EF93-F

Abstract

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.