A neutron-X-ray, NMR and calorimetric study of glassy Probucol synthesized using containerless techniques

J. K R Weber, C. J. Benmore, A. N. Tailor, S. K. Tumber, J. Neuefeind, Brian Cherry, Jeffery Yarger, Q. Mou, W. Weber, S. R. Byrn

Research output: Contribution to journalArticlepeer-review

13 Scopus citations

Abstract

Abstract Acoustic levitation was used to trap 1-3 mm diameter drops of Probucol and other pharmaceutical materials in containerless conditions. Samples were studied in situ using X-ray diffraction and ex situ using neutron diffraction, NMR and DSC techniques. The materials were brought into non-equilibrium states by supersaturating solutions or by supercooling melts. The glass transition and crystallization temperatures of glassy Probucol were 29 ± 1 and 71 ± 1 C respectively. The glassy form was stable with a shelf life of at least 8 months. A neutron/X-ray difference function of the glass showed that while molecular sub-groups remain rigid, many of the hydrogen correlations observed in the crystal become smeared out in the disordered material. The glass is principally comprised of slightly distorted Form I Probucol molecules with disordered packing rather than large changes in the individual molecular structure. Avoiding surface contact-induced nucleation provided access to highly non-equilibrium phases and enabled synthesis of phase-pure glasses.

Original languageEnglish (US)
Pages (from-to)89-92
Number of pages4
JournalChemical Physics
Volume424
DOIs
StatePublished - Jul 2 2013

Keywords

  • Acoustic levitation
  • Amorphous pharmaceuticals
  • Glass
  • Keywords
  • Liquids
  • Neutron
  • X-ray

ASJC Scopus subject areas

  • Physics and Astronomy(all)
  • Physical and Theoretical Chemistry

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