Abstract
A study of single-run differential scanning calorimetry is presented considering baseline repeatability, crosstalk between the calorimeters, positioning of calorimeters, heating rate, sample mass, environment changes, sample pan mass, purge gas flow, instrument lags, and differences in heating rate between the calorimeters. The instrument considered was the du-Pont dual sample differential scanning calorimeter. The major errors are caused by environmental changes. All other errors seem to limit accuracy to±0.3%, a very respectable level. After optimizing all parameters, heat capacities of aluminum, sodium chloride, quartz, polystyrene and selenium were measured between 348 and 548 K. The root mean square error of all measurements on comparison with well established adiabatic calorimetry is±0.8%. This proves that single-run differential scanning calorimetry is possible, as predicted before, and improvements can still be made.
Zusammenfassung
Es wird eine Untersuchung eines single-run DSC vorgestellt, die tagendes berücksichtigt: Grundlinienreproduzierbarkeit, crosstalk zwischen Kalorimetern, Einstellung von Kalorimetern, Aufheizgeschwindigkeit, Probenmasse, Umweltver änderungen, Probenhaltermasse, Spülgasfluss, Instrumentträgheit und Unterschiede in der Aufheizgeschwindigkeit der Kalorimeter. Das fragliche Instrument war ein duPont Doppelproben DS-Kalorimeter. Die grössten Fehler werden durch Umwelteinflüsse verursacht. Alle anderen Fehler scheinen die Genauigkeit auf das akzeptierbare Mass von ±0.3% zu begrenzen. Nach einer Optimierung aller Parameter wurden bei Temperaturen zwischen 348 und 548 K die Wärmekapazitäten von Aluminium, Natriumchlorid, Quarz, Polystyrol, und Selen gemessen. Die Standardabweichung aller Messungen im Vergleich mit der relativ gut bekannten adiabatischen Kalorimetrie beträgt ±0.8%. Dies beweist, dass die single-run DSC, wie schon darauf hingewiesen, prinzipiell möglich ist, Verbesserungen aber noch möglich sind.
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On leave from the Dept. of Material Science, Fudan University, Shanghai, Chine
This work was supported by the National Science Foundation, Polymer 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 Systems, Inc. In addition, support by the duPont Company in acquisition of the instrumentation is acknowledged.
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Jin, Y., Wunderlich, B. Single run heat capacity measurements. Journal of Thermal Analysis 36, 765–789 (1990). https://doi.org/10.1007/BF01914526
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DOI: https://doi.org/10.1007/BF01914526