Skip to main content
SpringerLink
Log in

Heat Capacity Measurements Using Temperature-modulated Heat Flux DSC with Close Control of the Heater Temperature

  • Published:
Journal of Thermal Analysis and Calorimetry Aims and scope Submit manuscript

Abstract

The determination of heat capacity data with sawtooth-type, temperature-modulated differential scanning calorimetry is analyzed using the Mettler-Toledo 820 ADSC™temperature-modulated differential scanning calorimeter (TMDSC). Heat capacities were calculated via the amplitudes of the first and higher harmonics of the Fourier series of the heat flow and heating rates. At modulation periods lower than about 150 s, the heat capacity deviates increasingly to smaller values and requires a calibration as function of frequency. An earlier derived correction function which was applied to the sample temperature-controlled power compensation calorimeter enables an empirical correction down to modulation periods of about 20 s. The correction function is determined by analysis of the higher harmonics of the Fourier transform from a single measurement of sufficient long modulation period. The correction function reveals that the time constant of the instrument is about 5 s rad−1 when a standard aluminum pan is used. The influence of pan type and sample mass on the time constant is determined, the correction for the asymmetry of the system is described, and the effect of smoothing of the modulated heat flow rate data is discussed.

This is a preview of subscription content, log in via an institution to check access.

Access this article

Log in via an institution

Price excludes VAT (USA)
Tax calculation will be finalised during checkout.

Instant access to the full article PDF.

Institutional subscriptions

Similar content being viewed by others

References

  1. M. Reading, B. K. Hahn and B. S. Crowe, U.S. Patent, Method and Apparatus for Modulated Differential Analysis, 5, 224, 775, July 6, 1993; P. S. Gill, S. R. Sauerbrunn and M. Reading, J. Thermal Anal., 40 (1993) 931; M. Reading, A. Luget and R. Wilson, Thermochim. Acta, 138 (1994) 295.

  2. B. Wunderlich, Thermal Analysis, Academic Press, New York 1990; for an update of the text see: Thermal Analysis of Materials, A computer-assisted lecture course published on the Internet (web.utk.edu/∼athas/courses/tham99.html), downloadable including presentation software, 2000.

    Google Scholar 

  3. A. Boller, Y. Jin and B. Wunderlich, J. Thermal Anal., 42 (1994) 307.

    CAS  Google Scholar 

  4. B. Wunderlich, Y. Jin and A. Boller, Thermochim. Acta, 238 (1994) 277.

    Article  CAS  Google Scholar 

  5. R. Androsch and B. Wunderlich, Thermochim. Acta, 333 (1999) 27.

    Article  CAS  Google Scholar 

  6. B. Wunderlich and I. Okazaki, ‘Temperature-Modulated Calorimetry of the Frequency Dependence of the Glass Transition of Poly(ethylene terephthalate) and Polystryrene’ in M. R. Tant and A. J. Hills, eds., ‘structure and Properties of Glassy Polymers’ ACS Symposium Series, 710 (1998) 103, Am. Chem. Soc., Washington, D.C.

    Google Scholar 

  7. R. Androsch, I. Moon, S. Kreitmeier and B. Wunderlich, Thermochim. Acta, in print.

  8. J. E. K. Schawe and W. Winter, Thermochim. Acta, 298 (1997) 9.

    Article  CAS  Google Scholar 

  9. I. Moon, R. Androsch and B. Wunderlich, Thermochim. Acta, accepted (1999); see also D. Dollimore (Ed.), Proceedings of the 26th NATAS Conference in Cleveland, OH, Sept. 13-15, 26 (1998) 134.

  10. Manual Mettler-Toledo STARe Software Version 5.1.

  11. R. Riesen, G. Wiedemann and R. Truttmann, Thermochim. Acta, 268 (1995) 1.

    Article  Google Scholar 

  12. B. Schenker and F. Stäger, Thermochim. Acta, 304/305 (1997) 219.

    Article  Google Scholar 

  13. K. Ishikiriyama and B. Wunderlich, J. Thermal Anal., 50 (1997) 337.

    Article  CAS  Google Scholar 

  14. A. Boller, I. Okazaki, K. Ishikiriyama, G. Zhang and B. Wunderlich, J. Thermal Anal., 49 (1997) 1081.

    Article  CAS  Google Scholar 

  15. R. Androsch, Polymer, 40 (1999) 2805.

    Article  CAS  Google Scholar 

  16. R. Androsch, J. Blackwell, S. N. Chvalun and B. Wunderlich, Macromolecules, 32 (1999) 3735.

    Article  CAS  Google Scholar 

  17. R. Androsch and B. Wunderlich, Macromolecules, 32 (1999) 7238.

    Article  CAS  Google Scholar 

  18. Operating Instructions, Dynamic Differential Scanning Calorimetry (DDSC) Accessory Kit, Perkin Elmer, Norwalk, 1995.

    Google Scholar 

  19. B. Wunderlich, R. Androsch, M. Pyda and Y. K. Kwon, Thermochim. Acta, submitted September 1999.

  20. J. Pak and B. Wunderlich, Thermochim. Acta, submitted October 1999.

  21. M. Pyda, Y. K. Kwon and B. Wunderlich, Thermochim. Acta, submitted October 1999.

  22. Y. K. Kwon, R. Androsch, M. Pyda and B. Wunderlich, Thermochim. Acta, submitted October 1999.

Download references

Author information

Authors and Affiliations

  1. Institute of Material Science, Martin Luther University Halle-Wittenberg, Geusaer Str, 06217, Merseburg, Germany

    R. Androsch

Authors
  1. R. Androsch
    View author publications

    You can also search for this author in PubMed Google Scholar

Rights and permissions

Reprints and permissions

About this article

Cite this article

Androsch, R. Heat Capacity Measurements Using Temperature-modulated Heat Flux DSC with Close Control of the Heater Temperature. Journal of Thermal Analysis and Calorimetry 61, 75–89 (2000). https://doi.org/10.1023/A:1010104406353

Download citation

  • Issue Date:

  • DOI: https://doi.org/10.1023/A:1010104406353

Search

Navigation