Abstract
We describe the construction, operation and performance of a fully automated low temperature differential micro-calorimeter for heat capacity measurements on small samples (m < 100 mg) in the temperature range from 15 K to 300 K. The instrument is operated using different calorimetric methods, in particular adiabatic differential scanning. Its reliability is demonstrated by measuring the heat capacity of 23 mg of copper and 37 mg of cyclopentane with an error of less than 2%.
Zusammenfassung
Es wird der Aufbau, die Funktions- und Arbeitsweise eines vollautomatisierten Differential-Mikrokalorimeters für Wärmekapazitätsmessungen kleiner Proben (m < 100 mg) im Temperaturbereich 15–300 K beschrieben. Die Funktionsweise des Gerätes beruht auf verschiedenen kalorimetrischen Methoden, insbesondere aufadiabatischem Differential-Scanning, Seine Zuverlässigkeit wird durch die Messung der Wärmekapazität einer 23 mg-Kupferprobe und einer 37 rag-Cyclopentanprobe mit einem Me\fehler von kleiner als 2% demonstriert.
Similar content being viewed by others
References
P. F. Sullivan and G. Seidel, Phys. Rev., 173 (1968) 679.
D. R. Bachmannet al., Rev. Sci. Instrum., 43 (1972) 205.
R. Marx, Rev. Sci. Instrum., 55 (1984) 1310.
R. W. Jones, G. S. Knapp and B. W. Veal, Rev. Sci. Instrum., 44 (1973) 807.
W. Brill and E. Gmelin, J. of Thermal Analysis, 33 (1988) 365.
D. Bertolini, M. Cassettari, G. Salvetti, E. Tombari and S. Veronesi, Rev. Sci. Instrum., 61 (1990) 2416.
S. Riegel and G. Weber, J. Phys. E, 19 (1986) 790.
R. W. Willekers, H. C. Meijer, F. Mathu and H. Postma, Cryogenics, 31 (1991) 168.
M. Regelsberger, R. Wernhardt and M. Rosenberg, J. Phys. E, 19 (1986) 525.
J. M. de Puydt and E. D. Dahlberg, Rev. Sci. Instrum., 57 (1986) 483.
E. Gmelin, Thermochimica Acta, 29 (1979) 1, and Refs therein.
E. Gmelin and P. Rödhammer, J. Phys. E, 14 (1981) 233.
D. L. Martin, Can. J. Phys., 38 (1960) 17; J. F. Cochran, G A. Schiffmann and J. E Neighbor, Rev. Sci. Instrum., 37 (1966) 499.
R Lagnier, J. Pierre and M. J. Mortimer, Cryogenics 17 (1977) 349.
A. Junod, J. Phys. E, 12 (1979) 945, and Refs therein.
M. Rajeswari and A. K. Raychaudhuri, J. Phys. E, 21 (1988) 1017.
A. K. Bandyopadhyay, P. Maruthikumar, G. L. Bhalla, S. K. Agarwal and A. V. Narlikar, Physica C, 165 (1990) 29.
E. Gmelin, Thermochimica Acta, 110 (1987) 183.
CRYOVAC GmbH, D-5210 Troisdorf, FRG
E. Gmelin and K. Ripka, Cryogenics, 21 (1981) 117.
M. Wun and N. E. Philips, Cryogenics, 15 (1975) 36, and Refs therein.
T. D. Cheung, W. K. Chan and J. S. Kouvel, Rev. Sci. Instrum., 53 (1982) 880.
D. L. Martin, Rev. Sci. Instrum., 58 (1987) 639 and Refs therein.
Recommendations of the GEFTA task group ‘Calibration of Dynamic Calorimeters’; see this conference and Part II to be published in Thermochim. Acta (1991); Part I: G. W. H. Höhne, H. K. Cammenga, W. Eysel, E. Gmelin and W. Hemminger, Thermochim. Acta, 160 (1990) 1.
J. G. Aston, H. L. Fink and S. C. Schumann, J. Amer. Chem. Soc., 65 (1943) 7; G. J. Szasz, J. A. Morisson, E. L. Pace and J. G. Aston, J. Chem. Phys., 15 (1947) 562.
Author information
Authors and Affiliations
Rights and permissions
About this article
Cite this article
Rahm, U., Gmelin, E. Low temperature micro-calorimetry by differential scanning. Journal of Thermal Analysis 38, 335–344 (1992). https://doi.org/10.1007/BF01915498
Issue Date:
DOI: https://doi.org/10.1007/BF01915498