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Quantitative Analysis by Thermogravimetry-Mass Spectrum Analysis for Reactions with Evolved Gases
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Published on: October 29, 2018

Quantitative analysis of solid-state processes studied with isothermal microcalorimetry.

Luis Almeida E Sousa1, Naziha Alem, Anthony E Beezer

  • 1School of Pharmacy, University of London, 29-39 Brunswick Square, London, WC1N 1AX, United Kingdom.

The Journal of Physical Chemistry. B
|September 28, 2010
PubMed
Summary
This summary is machine-generated.

New mathematical methods enable direct calculation of total heat change (Q) from partial isothermal microcalorimetric data. This facilitates quantitative analysis of solid-state processes and determination of reaction mechanisms.

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Area of Science:

  • Physical Chemistry
  • Materials Science
  • Chemical Engineering

Background:

  • Quantitative analysis of solid-state processes using isothermal microcalorimetry typically requires data for the entire process.
  • Determining the total heat change (Q) is crucial for analyzing calorimetric data as a function of fraction reacted (α).
  • Q determination is challenging when initial or final data are missing due to fast or slow process kinetics.

Purpose of the Study:

  • To introduce novel mathematical methods for directly calculating the total heat change (Q) from partial microcalorimetric data.
  • To enable direct determination of reaction mechanism descriptors (m and n) and rate constants (k).
  • To apply these methods to real-world solid-state processes, such as the crystallization of indomethacin.

Main Methods:

  • Development of several mathematical methods based on the Pérez-Maqueda model for calculating Q from incomplete data.
  • Utilizing simulated calorimetric data to validate the accuracy and reliability of the proposed methods.
  • Introduction of a graphical method for generating solid-state power-time data.

Main Results:

  • The developed methods successfully recovered the total reaction enthalpy (16.6 J) for the crystallization of indomethacin.
  • Analysis indicated that the crystallization process followed an Avrami model.
  • Rate constants for crystallization were consistently determined across the different methods (3.98–4.13 × 10⁻⁶ s⁻¹).

Conclusions:

  • The introduced mathematical methods provide a robust approach for quantitative analysis of solid-state processes even with incomplete microcalorimetric data.
  • These methods facilitate direct determination of reaction kinetics and mechanisms, overcoming limitations of traditional analysis.
  • The successful application to indomethacin crystallization demonstrates the practical utility of these techniques in materials science research.