Crystallographic Structure of Powder Beds from X-ray Microscopy
Introduction

Crystallographic Structure of Powder Beds from X-ray Microscopy

Researchers successfully use LabDCT to study 3D crystallographic information.

The vast majority of pharmaceutical formulations involve polycrystalline materials in some form. The interactions between different crystals can be important for the behavior of the formulation and necessary to assess manufacturability and performance. Surprisingly, there is an absence of methods and techniques for 3D crystallographic information for organic materials and a clear need for techniques that provide non-destructive granular information of organic materials in powders.

Dr. Parmesh Gajjar, a research associate at the University of Manchester, United Kingdom, recently published how he used the ZEISS Xradia Versa X-ray microscope with LabDCT to investigate crystalline powder bed structure.

  • 3D visualizations of all the different crystals within the powder identified by LabDCT, each colored according to their orientation.
    3D visualizations of all the different crystals within the powder identified by LabDCT, each colored according to their orientation.

    3D visualizations of all the different crystals within the powder identified by LabDCT, each colored according to their orientation.

    3D visualizations of all the different crystals within the powder identified by LabDCT, each colored according to their orientation.

  • Several groups of crystals, highlighting crystal-crystal interactions.
    Several groups of crystals, highlighting crystal-crystal interactions.

    Several groups of crystals, highlighting crystal-crystal interactions.

    Several groups of crystals, highlighting crystal-crystal interactions.

  • Orientational color bar, with sketches showing what each orientation means in terms of a hexamine crystal. Image reproduced from Gajjar et al. under a CC-BY license.
    Orientational color bar, with sketches showing what each orientation means in terms of a hexamine crystal. Image reproduced from Gajjar et al. under a CC-BY license.

    Orientational color bar, with sketches showing what each orientation means in terms of a hexamine crystal. Image reproduced from Gajjar et al. under a CC-BY license.

    Orientational color bar, with sketches showing what each orientation means in terms of a hexamine crystal. Image reproduced from Gajjar et al. under a CC-BY license.

Crystal Morphology and Interactions Unveiled with LabDCT

Previously, Dr. Gajjar had shown that LabDCT, an analytical module of the ZEISS Xradia Versa X-ray microscope, could be successfully used to study 3D crystallographic information, including grain centroid, orientation and shape, for metals, metalloids and minerals. Next, he wanted to test if this technique could be used for organic materials.

In this paper, he shows how LabDCT does indeed work for organic materials and he experimentally proves the crystal morphology as well as reveals the nature of interactions between individual crystals within the powder bed.

Dr. Parmesh Gajjar, University of Manchester, United Kingdom

These results have significance for the pharmaceutical industry and, more broadly, fine chemical industries, where a firm knowledge of the chemical basis behind powder bed structuring is of utmost importance for manufacturing and performance.

Dr. Parmesh Gajjar

Research Associate, University of Manchester, United Kingdom


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