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Single run heat capacity measurements

III. Data analysis

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Abstract

An outline for the data analysis of single-run heat capacity measurments by dual sample DSC is presented with the following features: 1. Heat flow correction by subtracting the contribution due to the sample pan, including correction for mismatched pan masses. 2. Heat flow and temperature correction with a nonlinear temperature calibration, temperature lag correction, and heating rate correction. 3. Calculation of the cell constants for both cell positions and evaluation of the asymmetry factor between cell positions A and B. 4. Heat capacity calibration and calculation with slope and asymmetry correction. 5. Calculation of heat capacity for multiple runs. 6. Data curve fitting for heat capacity.

Zusammenfassung

Es werden die Grundzüge für die Datenanalyse von Wärmekapazitätsmessungen durch Doppelproben- DSC mit Einfachdurchgängen beschrieben: 1. Korrektion des Wärmeflusses durch Subtraktion des Beitrages des Probenbehälters, einschließlich der Korrektion nicht angeglichener Behältermassen. 2. Korrektion des Wärme flusses und der Temperatur mit einer nichtlinearen Temperaturkalibrierung, Korrektion von Temperaturverzögerung und Aufheizgeschwindigkeit. 3. Berechnung der Zellen-konstanten für beide Zellenpositionen und Ermittlung des Asymmetriefaktors zwischen den Zellenpositionen A und B. 4. Kalibrierung der Wärmekapazität und Berechnung mit Anstiegs- und Asymmetriekorrektion. 5. Berechnung der Wärmekapazität für Mehrfachdurchgänge. 6. Kurvenanpassung für die Wärmekapazität.

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Authors and Affiliations

  1. Department of Chemistry, University of Tennessee, 37996-1600, Knoxville, TN

    Y. Jin & B. Wunderlich

  2. Chemistry Division, Oak Ridge National Laboratory, 37831-6197, Oak Ridge, TN, USA

    Y. Jin & B. Wunderlich

Authors
  1. Y. Jin
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  2. B. Wunderlich
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Additional information

‘The submitted manuscript has been authored by a contractor of the U.S. Government under contract No. DE-AC05-840R-21400. Accordingly, the U.S. Government retains a nonexclusive, royalty-free license to publish or reproduce the published form of this contribution, or allow others to do so, for U.S. Government purposes.’

This work was supported by the Division of Materials Research, National Science Foundation, Polymers Program, Grant # DMR 8818412 and the Division of Materials Sciences, Office of Basic Energy Sciences, U.S. Department of Energy, under Contract DE-AC05-84OR21400 with Martin Marietta Energy Systems, Inc. Thanks are given to TA Instruments, Inc. (New Castle, DE) for providing the commercial heat capacity software and helping with the acquisition of the calorimeter.

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Jin, Y., Wunderlich, B. Single run heat capacity measurements. Journal of Thermal Analysis 38, 2257–2272 (1992). https://doi.org/10.1007/BF02123979

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  • DOI: https://doi.org/10.1007/BF02123979

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