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The combined techniques of thermomicroscopy, differential scanning calorimetry (DSC), thermomicrophotometry (TMP), and micro-Fourier transform infrared spectroscopy (FTIR) are essential for the unequivocal detection of polymorphism. The polymorphism ofp-hexadecylaminobenzoic acid (HABA), a pharmaceutical intermediate, is presented to illustrate the need to use a multitechnique approach.

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Kinetic applications of thermal analysis

A comparison of dynamic and isothermal methods

Journal of Thermal Analysis and Calorimetry
P. M. D. Benoit
R. G. Ferrillo
, and
A. H. Granzow

A study was undertaken to compare two computational methods of estimating kinetic parameters from thermoanalytical experiments. Examples illustrating the relationship between reaction complexity and validity of isothermalvs. non-isothermal kinetic analyses will be presented. Thermal decomposition of several compounds was studied both by isothermal and dynamic thermogravimetry (TG). For the isothermal runs, reaction order and activation energy were estimated using established methods. For the dynamic runs, the statistical method of nonlinear least squares was used to estimate all three kinetic parameters of the nth order decomposition reaction and their individual 95% confidence intervals. Both methods assumed Arrhenius temperature dependence.

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