Application of Powder X-ray Diffraction in Studying the Compaction Behavior of Bulk Pharmaceutical Powders  Rebanta Bandyopadhyay, Jon Selbo, Gregory E. Amidon, Michael Hawley  Journal of Pharmaceutical Sciences  Volume 94, Issue 11, Pages 2520-2530 (November 2005) DOI: 10.1002/jps.20415 Copyright © 2005 Wiley-Liss, Inc. Terms and Conditions

Figure 1 A schematic representation of the effects of crystal lattice deformation on the X-ray diffraction peak position. adapted from reference 19 Journal of Pharmaceutical Sciences 2005 94, 2520-2530DOI: (10.1002/jps.20415) Copyright © 2005 Wiley-Liss, Inc. Terms and Conditions

Figure 2 The relationship between δd/δθ and δd/δθ with 2θ and d. The plots are based on Eq. 2a and b assuming ‘n’ to be unity. Journal of Pharmaceutical Sciences 2005 94, 2520-2530DOI: (10.1002/jps.20415) Copyright © 2005 Wiley-Liss, Inc. Terms and Conditions

Figure 3 Optical photomicrographs showing the crystal morphologies of the three model compounds (A) PNU-288034, (B) PNU-177553, and (C) PNU-141659. Journal of Pharmaceutical Sciences 2005 94, 2520-2530DOI: (10.1002/jps.20415) Copyright © 2005 Wiley-Liss, Inc. Terms and Conditions

Figure 4 The powder X-ray diffraction (PXRD) patterns from compressed (2000lb) and uncompressed (A) PNU-288034, (B) PNU-177553, and (C) PNU-141659 powders. Journal of Pharmaceutical Sciences 2005 94, 2520-2530DOI: (10.1002/jps.20415) Copyright © 2005 Wiley-Liss, Inc. Terms and Conditions

Figure 5 Effect of compaction on peak intensity for the various diffraction peaks of PNU-288034. The peaks are identified by their 2θ positions in the bulk PXRD pattern. Journal of Pharmaceutical Sciences 2005 94, 2520-2530DOI: (10.1002/jps.20415) Copyright © 2005 Wiley-Liss, Inc. Terms and Conditions

Figure 6 The changes in 2θ peak positions for PNU-288034 plotted against the corresponding peak positions for the uncompressed, bulk powder. Since the change is calculated as the peak position of the bulk powder—the peak position of the compact, a negative shift depicted in the plot, represents a shift towards larger 2θ upon compression. Journal of Pharmaceutical Sciences 2005 94, 2520-2530DOI: (10.1002/jps.20415) Copyright © 2005 Wiley-Liss, Inc. Terms and Conditions

Figure 7 The change in interplanar d-spacing after compression of PNU-288034 expressed as a fraction of the d-spacing in the uncompressed, bulk powder shown plotted against the d-spacing of the bulk powder. Convention used: a positive strain in the plot represents a decrease in the interplanar d-spacing following compaction. Journal of Pharmaceutical Sciences 2005 94, 2520-2530DOI: (10.1002/jps.20415) Copyright © 2005 Wiley-Liss, Inc. Terms and Conditions

Figure 8 The change in interplanar d-spacing after compaction of PNU-177553 expressed as a fraction of the d-spacing in the uncompressed, bulk powder shown plotted against the d-spacing of the bulk powder. Convention: a positive strain represents a decrease in the interplanar d-spacing following compaction. Journal of Pharmaceutical Sciences 2005 94, 2520-2530DOI: (10.1002/jps.20415) Copyright © 2005 Wiley-Liss, Inc. Terms and Conditions

Figure 9 The change in interplanar d-spacing after compaction of PNU-141659 expressed as a fraction of the d-spacing in the uncompressed, bulk powder. Convention: the negative value of the strain in the figure represents an increase in the interplanar d-spacing following compaction. Journal of Pharmaceutical Sciences 2005 94, 2520-2530DOI: (10.1002/jps.20415) Copyright © 2005 Wiley-Liss, Inc. Terms and Conditions

Figure 10 The change in interplanar d-spacing expressed as a fraction of the d-spacing in the uncompressed, bulk powder after size reduction of PNU-141659 crystals by grinding. Convention: the negative value of the strain in the figure represents an increase in the interplanar d-spacing following compaction. Journal of Pharmaceutical Sciences 2005 94, 2520-2530DOI: (10.1002/jps.20415) Copyright © 2005 Wiley-Liss, Inc. Terms and Conditions

Figure 11 Plot showing the relationship between the compressed lattice strain and the square of the lattice d-spacing of the uncompressed powder for (A) PNU-288034 (B) PNU-177553 and (C) PNU-141659. Journal of Pharmaceutical Sciences 2005 94, 2520-2530DOI: (10.1002/jps.20415) Copyright © 2005 Wiley-Liss, Inc. Terms and Conditions