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; B. Cherry; J. L. Yarger; Q. Mou; W. Weber; S. R. Byrn

doi:10.1016/j.chemphys.2013.05.019

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, B. Cherry, J. L. Yarger, Q. Mou, W. Weber, S. R. Byrn

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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 language	English
Pages (from-to)	89-92
Number of pages	4
Journal	Chemical Physics
Volume	424
DOIs	https://doi.org/10.1016/j.chemphys.2013.05.019
State	Published - 2013

Funding

This research was supported by the US Department of Energy, Office of Science, Office of Basic Energy Sciences, under contract DE-AC02-06CH11357. We would like to thank Rick Spence at the Advanced Photon Source for his help in setting up the levitator equipment. JLY would like to acknowledge support from the National Nuclear Security Administration Carnegie/DOE Alliance Center (NNSA CDAC) Grant number DE-FC52-08NA28554 and the US National Science Foundation (NSF), Chemistry Division (CHE) under Grant CHE-1011937 .

Funders	Funder number
National Nuclear Security Administration Carnegie/DOE Alliance Center
National Science Foundation
U.S. Department of Energy
Division of Chemistry	CHE-1011937
Office of Science
Basic Energy Sciences	DE-AC02-06CH11357
National Nuclear Security Administration	DE-FC52-08NA28554

Keywords

Acoustic levitation
Amorphous pharmaceuticals
Glass
Keywords
Liquids
Neutron
X-ray

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10.1016/j.chemphys.2013.05.019

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

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.",

keywords = "Acoustic levitation, Amorphous pharmaceuticals, Glass, Keywords, Liquids, Neutron, X-ray",

author = "Weber, {J. K.R.} and Benmore, {C. J.} and Tailor, {A. N.} and Tumber, {S. K.} and J. Neuefeind and B. Cherry and Yarger, {J. L.} and Q. Mou and W. Weber and Byrn, {S. R.}",

year = "2013",

doi = "10.1016/j.chemphys.2013.05.019",

language = "English",

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AU - Weber, J. K.R.

AU - Benmore, C. J.

AU - Tailor, A. N.

AU - Tumber, S. K.

AU - Neuefeind, J.

AU - Cherry, B.

AU - Yarger, J. L.

AU - Mou, Q.

AU - Weber, W.

AU - Byrn, S. R.

PY - 2013

Y1 - 2013

N2 - 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.

AB - 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.

KW - Acoustic levitation

KW - Amorphous pharmaceuticals

KW - Glass

KW - Keywords

KW - Liquids

KW - Neutron

KW - X-ray

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SN - 0301-0104

VL - 424

SP - 89

EP - 92

JO - Chemical Physics

JF - Chemical Physics

ER -

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

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Keywords

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