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

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. Lastly, 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.
Authors:
 [1] ;  [2] ;  [3] ;  [4] ;  [5] ;  [4] ;  [6] ;  [2]
  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:
Grant/Contract Number:
AC05-00OR22725; AC02-06CH11357; AC02-06CH1135
Type:
Accepted Manuscript
Journal Name:
Thermochimica Acta
Additional Journal Information:
Journal Volume: 644; Journal Issue: C; Journal ID: ISSN 0040-6031
Publisher:
Elsevier
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) (SC-22)
Country of Publication:
United States
Language:
English
Subject:
36 MATERIALS SCIENCE
OSTI Identifier:
1329117
Alternate Identifier(s):
OSTI ID: 1364641; OSTI ID: 1396821