A SAXS-WAXS study of the endothermic transitions in amorphous or supercooled liquid itraconazole

C. J. Benmore, Q. Mou, K. J. Benmore, D. S. Robinson, J. Neuefeind, J. Ilavsky, S. R. Byrn, Jeffery Yarger

Research output: Contribution to journalArticle

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Abstract

Small and wide angle high energy x-ray scattering experiments were performed upon cooling itraconazole from the melt to investigate the structural origin of the two transitions at ∼74 °C and ∼90 °C observed in DSC measurements. Slight changes to the main WAXS peak at Q = 1.33 ± 0.01 Å−1 were observed at 90 °C and are found to be inter-molecular in nature, suggesting a liquid to isotropic transition. This finding was supported by complementary wide angle neutron scattering measurements. For temperatures at and below ∼74 °C two strong rings appear in the 2D-SAXS pattern at Q = 0.24 ± 0.01 Å−1 and 0.43 ± 0.01 Å−1. The SAXS spectra were further deconvoluted into sharp and broad components. A narrowing of the broad component is associated with only minor changes in the packing arrangements of the itraconazole molecules below ∼90 °C, while the appearance of the sharp component below ∼74 °C is attributed to the formation of a polydomain lamellar phase.

Original languageEnglish (US)
Pages (from-to)1-5
Number of pages5
JournalThermochimica Acta
Volume644
DOIs
StatePublished - Nov 20 2016

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Itraconazole
Liquids
liquids
Neutron scattering
Scattering
x ray scattering
Cooling
X rays
Molecules
neutron scattering
cooling
Experiments
rings
Temperature
molecules
temperature
energy

ASJC Scopus subject areas

  • Instrumentation
  • Condensed Matter Physics
  • Physical and Theoretical Chemistry

Cite this

A SAXS-WAXS study of the endothermic transitions in amorphous or supercooled liquid itraconazole. / Benmore, C. J.; Mou, Q.; Benmore, K. J.; Robinson, D. S.; Neuefeind, J.; Ilavsky, J.; Byrn, S. R.; Yarger, Jeffery.

In: Thermochimica Acta, Vol. 644, 20.11.2016, p. 1-5.

Research output: Contribution to journalArticle

Benmore, CJ, Mou, Q, Benmore, KJ, Robinson, DS, Neuefeind, J, Ilavsky, J, Byrn, SR & Yarger, J 2016, 'A SAXS-WAXS study of the endothermic transitions in amorphous or supercooled liquid itraconazole', Thermochimica Acta, vol. 644, pp. 1-5. https://doi.org/10.1016/j.tca.2016.10.004
Benmore, C. J. ; Mou, Q. ; Benmore, K. J. ; Robinson, D. S. ; Neuefeind, J. ; Ilavsky, J. ; Byrn, S. R. ; Yarger, Jeffery. / A SAXS-WAXS study of the endothermic transitions in amorphous or supercooled liquid itraconazole. In: Thermochimica Acta. 2016 ; Vol. 644. pp. 1-5.
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