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

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 similar to 74 degrees C and similar to 90 degrees C observed in DSC measurements. Slight changes to the main WAXS peak at Q=1.33 +/- 0.01 angstrom(-1) were observed at 90 degrees 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 similar to 74 degrees C two strong rings appear in the 2D-SAXS pattern at Q= 0.24 +/- 0.01 angstrom(-1) and 0,43 +/- 0.01 angstrom(-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 degrees C, while the appearance of the sharp component below similar to 74 degrees C is attributed to the formation of a polydomain lamellar phase.

Authors:
 [1];  [2];  [3];  [4];  [5];  [4];  [6];  [2]
+ Show Author Affiliations
  1. Argonne National Lab. (ANL), Argonne, IL (United States); Arizona State Univ., Tempe, AZ (United States)
  2. Arizona State Univ., Tempe, AZ (United States)
  3. Univ. of Sheffield, Sheffield (United Kingdom)
  4. Argonne National Lab. (ANL), Argonne, IL (United States)
  5. Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)
  6. Purdue Univ., West Lafayette, IN (United States)
Publication Date:
Research Org.:
Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States). Spallation Neutron Source (SNS); Argonne National Lab. (ANL), Argonne, IL (United States)
Sponsoring Org.:
USDOE Office of Science (SC), Basic Energy Sciences (BES)
OSTI Identifier:
1329117
Alternate Identifier(s):
OSTI ID: 1364641; OSTI ID: 1396821
Grant/Contract Number:  
AC05-00OR22725; AC02-06CH11357; AC02-06CH1135
Resource Type:
Accepted Manuscript
Journal Name:
Thermochimica Acta
Additional Journal Information:
Journal Volume: 644; Journal Issue: C; Journal ID: ISSN 0040-6031
Publisher:
Elsevier
Country of Publication:
United States
Language:
English
Subject:
36 MATERIALS SCIENCE

Citation Formats

Benmore, C. J., Mou, Q., Benmore, K. J., Robinson, D. S., Neuefeind, J., Ilavsky, J., Byrn, S. R., and Yarger, J. L. A SAXS-WAXS study of the endothermic transitions in amorphous or supercooled liquid itraconazole. United States: N. p., 2016. Web. doi:10.1016/j.tca.2016.10.004.
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Benmore, C. J., Mou, Q., Benmore, K. J., Robinson, D. S., Neuefeind, J., Ilavsky, J., Byrn, S. R., & Yarger, J. L. A SAXS-WAXS study of the endothermic transitions in amorphous or supercooled liquid itraconazole. United States. doi:10.1016/j.tca.2016.10.004.
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Benmore, C. J., Mou, Q., Benmore, K. J., Robinson, D. S., Neuefeind, J., Ilavsky, J., Byrn, S. R., and Yarger, J. L. Fri . "A SAXS-WAXS study of the endothermic transitions in amorphous or supercooled liquid itraconazole". United States. doi:10.1016/j.tca.2016.10.004. https://www.osti.gov/servlets/purl/1329117.
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@article{osti_1329117,
title = {A SAXS-WAXS study of the endothermic transitions in amorphous or supercooled liquid itraconazole},
author = {Benmore, C. J. and Mou, Q. and Benmore, K. J. and Robinson, D. S. and Neuefeind, J. and Ilavsky, J. and Byrn, S. R. and Yarger, J. L.},
abstractNote = {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 similar to 74 degrees C and similar to 90 degrees C observed in DSC measurements. Slight changes to the main WAXS peak at Q=1.33 +/- 0.01 angstrom(-1) were observed at 90 degrees 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 similar to 74 degrees C two strong rings appear in the 2D-SAXS pattern at Q= 0.24 +/- 0.01 angstrom(-1) and 0,43 +/- 0.01 angstrom(-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 degrees C, while the appearance of the sharp component below similar to 74 degrees C is attributed to the formation of a polydomain lamellar phase.},
doi = {10.1016/j.tca.2016.10.004},
journal = {Thermochimica Acta},
number = C,
volume = 644,
place = {United States},
year = {2016},
month = {10}
}
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Journal Article:
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DOI:  10.1016/j.tca.2016.10.004
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Works referencing / citing this record:

Organic glasses with tunable liquid-crystalline order through kinetic arrest of end-over-end rotation: the case of saperconazole
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  • DOI: 10.1039/c9sm02180a

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journal, September 2019

  • Bishop, Camille; Thelen, Jacob L.; Gann, Eliot
  • Proceedings of the National Academy of Sciences, Vol. 116, Issue 43
  • DOI: 10.1073/pnas.1908445116
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