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A novel technique combining high-resolution synchrotron x-ray microtomography and x-ray diffraction for characterization of micro particulates

DOI: 10.1088/0957-0233/22/11/115703 DOI Help

Authors: David Merrifield (University of Leeds) , Vasuki Ramachandran (University of Leeds) , Kevin Roberts (University of Leeds) , Wes Armour (Diamond Light Source) , Danny Axford (Diamond Light Source) , Mark Basham (Diamond Light Source) , Gwyndaf Evans (Diamond Light Source) , Katherine Mcauley (Diamond Light Source) , Robin Owen (Diamond Light Source) , James Sandy (Diamond Light Source) , Thomas Connolley (Diamond Light Source)
Co-authored by industrial partner: No

Type: Journal Paper
Journal: Measurement Science And Technology , VOL 22 (11)

State: Published (Approved)
Published: November 2011

Abstract: The processing of solids, such as crystals, is strongly influenced by the surface properties of the material. In recent years the pharmaceutical industry has shown great interest in identifying, or chemically speciating, the molecular components of crystal faces. Formerly, characterization of the molecular identity of crystal faces was restricted to the study of large single crystals. This would have been primarily for structure determination as part of the drug registration process. Diamond Light Source in Oxfordshire is a new synchrotron facility in the UK, having 18 operational beamlines with 4 more in the construction phase. Beamlines at this medium energy light source enable the study of micron-sized objects in great detail. It is well known that x-ray microtomography (XMT) can be used to investigate the external morphology of a crystal whereas x-ray diffraction (XRD) is used to study the molecular orientation, structure and packing within the crystal. The objective of this research is to assess the feasibility of, and thereby develop a new methodology for, characterizing the molecular identity of a particular face of a crystalline particle at a scale of scrutiny of 20–50 ?m by combining these two powerful techniques. This work demonstrates the application of XMT and XRD to investigate respectively the shape and crystalline phase/orientation of relevant test crystals. This research has applications in the pharmaceutical industry in that when the exact molecular nature of a particular face is known, the important physico-pharmaceutical properties stemming from that can be better understood. Some initial data are presented and discussed.

Journal Keywords: Synchrotron Radiation; X-Ray Diffraction; X-Ray Microtomography; Single Particle; Crystallization

Subject Areas: Biology and Bio-materials


Instruments: I02-Macromolecular Crystallography , I03-Macromolecular Crystallography , I04-Macromolecular Crystallography , I24-Microfocus Macromolecular Crystallography