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Related Concept Videos

X-ray Crystallography02:18

X-ray Crystallography

The size of the unit cell and the arrangement of atoms in a crystal may be determined from measurements of the diffraction of X-rays by the crystal, termed X-ray crystallography.
Diffraction
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X-ray diffraction or XRD is an analytical tool that utilizes X-rays to study ordered structures such as crystalline organic and inorganic samples, polycrystalline materials, proteins, carbohydrates, and drugs.
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X-ray Powder Diffraction in Conservation Science: Towards Routine Crystal Structure Determination of Corrosion Products on Heritage Art Objects
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Structural interpretation in composite systems using powder X-ray diffraction: applications of error propagation to

Michael D Moore1, Zhenqi Shi, Peter L D Wildfong

  • 1Duquesne University, Graduate School of Pharmaceutical Sciences, Pittsburgh, Pennsylvania 15282, USA.

Pharmaceutical Research
|September 3, 2010
PubMed
Summary

This study presents a new statistical method for analyzing powder X-ray diffraction (PXRD) data using pair distribution function (PDF) transforms. This approach enables accurate structural conclusions from composite systems, enhancing material characterization.

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Area of Science:

  • Materials Science
  • Crystallography
  • Analytical Chemistry

Background:

  • Powder X-ray diffraction (PXRD) is crucial for analyzing material structures.
  • Pair distribution function (PDF) analysis offers detailed structural insights from PXRD data.
  • Statistical inference from experimental errors in PDF transforms remains a challenge.

Purpose of the Study:

  • To develop a robust statistical method for drawing inferences from multiple experimental PDF transforms of PXRD data.
  • To establish a reliable error threshold for PDF analysis in composite systems.

Main Methods:

  • Monte Carlo simulations were employed to test error propagation algorithms on amorphous ketoconazole.
  • Physical mixtures and co-solidified products (felodipine:PVPva, terfenadine:PVPva) were prepared and analyzed using PXRD and PDF.
  • Differential scanning calorimetry (DSC) was used for complementary material characterization.

Main Results:

  • Monte Carlo simulations validated the appropriate manipulation of PXRD error estimates for PDF transforms.
  • An error threshold of ±3σ was established using a felodipine:PVPva physical mixture.
  • PDF analysis revealed complete miscibility in felodipine:PVPva co-solidified products and phase separation in terfenadine:PVPva, despite DSC suggesting otherwise for the latter.

Conclusions:

  • Statistically sound inferences can be reliably drawn from PDF transforms of PXRD data for composite systems.
  • The developed method provides a fundamental basis for structural conclusions in PDF studies.
  • The principles are adaptable to diverse material systems, enhancing structural analysis capabilities.