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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 (November 2005) DOI: /jps.20415 Copyright © 2005 Wiley-Liss, Inc. Terms and Conditions
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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 , DOI: ( /jps.20415) Copyright © 2005 Wiley-Liss, Inc. Terms and Conditions
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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 , DOI: ( /jps.20415) Copyright © 2005 Wiley-Liss, Inc. Terms and Conditions
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Figure 3 Optical photomicrographs showing the crystal morphologies of the three model compounds (A) PNU , (B) PNU , and (C) PNU Journal of Pharmaceutical Sciences , DOI: ( /jps.20415) Copyright © 2005 Wiley-Liss, Inc. Terms and Conditions
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Figure 4 The powder X-ray diffraction (PXRD) patterns from compressed (2000lb) and uncompressed (A) PNU , (B) PNU , and (C) PNU powders. Journal of Pharmaceutical Sciences , DOI: ( /jps.20415) Copyright © 2005 Wiley-Liss, Inc. Terms and Conditions
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Figure 5 Effect of compaction on peak intensity for the various diffraction peaks of PNU The peaks are identified by their 2θ positions in the bulk PXRD pattern. Journal of Pharmaceutical Sciences , DOI: ( /jps.20415) Copyright © 2005 Wiley-Liss, Inc. Terms and Conditions
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Figure 6 The changes in 2θ peak positions for PNU 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 , DOI: ( /jps.20415) Copyright © 2005 Wiley-Liss, Inc. Terms and Conditions
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Figure 7 The change in interplanar d-spacing after compression of PNU 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 , DOI: ( /jps.20415) Copyright © 2005 Wiley-Liss, Inc. Terms and Conditions
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Figure 8 The change in interplanar d-spacing after compaction of PNU 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 , DOI: ( /jps.20415) Copyright © 2005 Wiley-Liss, Inc. Terms and Conditions
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Figure 9 The change in interplanar d-spacing after compaction of PNU 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 , DOI: ( /jps.20415) Copyright © 2005 Wiley-Liss, Inc. Terms and Conditions
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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 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 , DOI: ( /jps.20415) Copyright © 2005 Wiley-Liss, Inc. Terms and Conditions
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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 (B) PNU and (C) PNU Journal of Pharmaceutical Sciences , DOI: ( /jps.20415) Copyright © 2005 Wiley-Liss, Inc. Terms and Conditions
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