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The use of the High-Temperature Gas-Balance (HTGB) for thermogravimetric measurements

Thermal analysis detecting equilibrium conditions

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Abstract

Several methods are established in thermal analysis to investigate phase formation, phase transition, and decomposition reactions. The analysis of phase equilibria with volatile components is particularly feasible by using standard method of thermogravimetry. Hardly any investigations of phase formation reactions are possible to realize if one of the components is lost by vaporization. By using the “High-Temperature Gas-Balance” (HTGB), the vapor phase is enclosed in a silica ampoule and thus forms an equilibrium gas phase in permanent contact with the solid phase. The measurement signal Δm meas is caused by change of the leverage of the horizontal balance support during evaporation and condensation. The application of the HTGB allows the analysis of solid–gas equilibria in the working range from 0.01 till 15 bar at temperatures up to 1,100 °C. The first comparison of evaporation reactions determined by standard thermogravimetric analyses and by measurements using the HTGB is given for the inorganic systems: P, As, SeO2, PtI2, and Hg/I.

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Acknowledgements

The authors greatly acknowledge the financial support by the Priority program—Schwerpunktprogramm 1415 of the German research funding organization—Deutsche Forschungsgemeinschaft (DFG). The high-temperature materials and furnaces specialist HTM Reetz (http://www.htm-reetz.de/en/index.asp) is gratefully acknowledged for the technical support in construction and optimization of the High-Temperature Gas-Balance.

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Authors and Affiliations

  1. Faculty of Sciences, Inorganic Solids and Materials, Lausitz University of Applied Science, P.O. Box 101548, 01958, Senftenberg, Germany

    Peer Schmidt

  2. Department of Inorganic Chemistry, Technische Universität Dresden, Helmholtzstrasse 10, 01069, Dresden, Germany

    Michael Schöneich

  3. Institute for Inorganic and Analytical Chemistry, WWU Münster, Corrensstraße 30, 48149, Münster, Germany

    Melanie Bawohl

  4. Department of Chemistry, Technische Universität München, Lichtenbergstr. 4, 85737, Garching, Germany

    Tom Nilges

  5. Institute for Inorganic Chemistry, Universität Regensburg, Universitätsstr. 31, 93040, Regensburg, Germany

    Richard Weihrich

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  1. Peer Schmidt
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  2. Michael Schöneich
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  3. Melanie Bawohl
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  4. Tom Nilges
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  5. Richard Weihrich
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Correspondence to Peer Schmidt.

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Schmidt, P., Schöneich, M., Bawohl, M. et al. The use of the High-Temperature Gas-Balance (HTGB) for thermogravimetric measurements. J Therm Anal Calorim 110, 1511–1521 (2012). https://doi.org/10.1007/s10973-011-2107-3

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  • DOI: https://doi.org/10.1007/s10973-011-2107-3

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