Journal
THERMOCHIMICA ACTA
Volume 530, Issue -, Pages 64-72Publisher
ELSEVIER
DOI: 10.1016/j.tca.2011.12.001
Keywords
Fast-scanning calorimetry; Thermal lag; Zero-heating rate temperature calibration; Heat flow rate calibration; Liquid crystal
Funding
- Fund for Scientific Research-Flanders, Belgium (F.W.O. Vlaanderen)
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This paper presents the calibration and evaluation of a Rapid Heat-Cool DSC (RHC), a fast-scanning calorimeter capable of controlled heating rates of up to 2000 K min(-1). As the use of high scan rates increases the influence of thermal lag, a thorough analysis of the instrument performance was made. This encompasses a rigorous temperature calibration procedure, a study of the influence of sample mass and heating rate on the extrapolated onset temperature, and the analysis of the symmetry of the thermal lag in heating and cooling using phase transitions in liquid crystals. The calibration of the heat flow rate is evaluated using indium for a broad range of sample masses and heating rates, and verified by heat capacity measurements on polystyrene for a wide temperature range. The performance of the RHC proves to be very good, with estimated errors on temperature and heat flow rate (heat capacity) of 0.1 K and 2%, respectively. (C) 2011 Elsevier B.V. All rights reserved.
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