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Dynamic purity determinations. I. Location of the solidus by nuclear magnetic resonance

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Abstract

The error in purity determinations by differential scanning calorimetry has been studied on two different kinds of systems, metallic and organic, the latter with different types of impurities added. The organic systems have been corrected for solid-solubility error by a nuclear magnetic resonance technique.

The impurities chosen for the organic systems were either quite dissimilar to the matrix or similar enough to render solid solution probable. This solid solution leads to deviations from the equation used for dynamic purity determinations. The nuclear magnetic resonance determination of the solidus establishes the proper starting temperature for area summation on a DSC curve.

Zusammenfassung

Der Fehler in Reinheitsbestimmungen mittels Differential-Scanning-kalorimetrie wurde an zwei verschiedenartigen Systemen untersucht, metallisch und organisch, wobei zu letzteren verschiedentliche Verunreinigungen zugefügt wurden. Der durch Feststoff-Feststofflöslichkeit verursachte Fehler in den organischen Systemen wurde mittels einer kernmagnetischen Resonanzmethode korrigiert.

Die für die organischen Systeme gewählten Verunreinigungen waren entweder sehr verschieden von der Matrix, oder aber genügend ähnlich, um feste Lösungen wahrscheinlich zu machen. Diese festen Lösungen führen zu Abweichungen von der für dynamische Reinheitsbestimmungen angewendeten Gleichung. Die Bestimmung der kernmagnetischen Resonanz des Feststoffs ermöglicht die Bestimmung der richtigen Anfangstemperatur für die Flächen-summierung auf der DSC-Kurve.

Резюме

С помощью ДСК была изу чена ошибка при определении чистоты двух различных систем: металлическо й и органической. При э том последняя система из учалась с различного рода при месями. С помощью мето да ЯМР для органических систем была учтена ошибка твердо тельной растворимос ти. Примеси, взятые для органичес ких систем, или полностью отлича лись от исходного орг анисеского вещества, или же были в такой степени подобн ы, что могли образовыв ать твердый раствор. Твердый раст вор вызывал отклонения о т уравнения, исыользо ванного для динамического опред еления чистоть. Определение солидуса методом ЯМР позволило установить начальну ю температуру для итоговой поверхн оти ДСК-кривой.

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Authors and Affiliations

  1. The University of Akron, 44325, Akron, Ohio, USA

    B. Kawalec, J. J. Houser & P. D. Garn

Authors
  1. B. Kawalec
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  2. J. J. Houser
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  3. P. D. Garn
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Additional information

On leave from The Institute for Physical Chemistry, Polish Academy of Science, Warsaw, Poland.

The authors are grateful to the National Science Foundation for its support through Research Grant CHE 76-08765, and to S. E. Walter for assistance with some calculations.

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Kawalec, B., Houser, J.J. & Garn, P.D. Dynamic purity determinations. I. Location of the solidus by nuclear magnetic resonance. Journal of Thermal Analysis 25, 259–270 (1982). https://doi.org/10.1007/BF01912951

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  • DOI: https://doi.org/10.1007/BF01912951

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