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A new program for DSC purity analysis

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Abstract

DSC purity determinations have become very popular today [3]. The latest edition of the Mettler software package for thermal analysis, TA72.S GraphWare, now comprises a powerful purity evaluation program. It is based on the simultaneous calculation of the mole ratio of the sum of the eutectic impurities, the melting point of the pure component, the melting point of the substance present and the linearization term. The portion of the melting curve investigated is selected appropriately.

Experience has shown, that the applied heating rate is a very important parameter which influences the duration of the measurement and also the possible exposure to elevated temperature where decomposition can become a problem and last but not least the accuracy of the calculated impurity value.

Zusammenfassung

Die DSC-Reinheitsbestimmung ist heute eine weit verbreitete Methode, die mit einer einzigen Messung und unter Verwendung geeigneter Auswerteprogramme eine Bestimmung der absoluten eutektischen Reinheit einer Probe zulÄsst. Gleichzeitig können weitere thermodynamische Daten bestimmt werden, wie Schmelzpunkt der Probensubstanz und der reinen Hauptkomponente und die Schmelzenthalpie der Probe.

Durch experimentelle Befunde konnte gezeigt werden, dass die Wahl der Aufheizrate kritisch ist in bezug auf die Genauigkeit und die Signifikanz der ermittelten Daten.

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References

  1. E. Marti, Thermochim. Acta, 5 (1972) 173.

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  2. O. Heiber, Poster Session ICTA Bayreuth (1980).

  3. R. L. Blaineet al., Purity Determinations by Thermal Methods, ASTM Special Technical Publication 838 (1984).

  4. ASTM Test Method for Mol Percent Impurity by DSC, E928-83.

  5. E. Marti, Ciba-Geigy AG, Basel, private communication.

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Widmann, G., Scherrer, O. A new program for DSC purity analysis. Journal of Thermal Analysis 37, 1957–1964 (1991). https://doi.org/10.1007/BF01912228

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  • DOI: https://doi.org/10.1007/BF01912228

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