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Related Experiment Videos

Indexing powder patterns in physical form screening: instrumentation and data quality.

Alastair J Florence1, Bruno Baumgartner, Chris Weston

  • 1Department of Pharmaceutical Sciences, University of Strathclyde, Glasgow G4 0NR, UK. alastair.florence@strath.ac.uk

Journal of Pharmaceutical Sciences
|September 2, 2003
PubMed
Summary

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Two powder diffractometers effectively screen physical forms using foil transmission geometry. This method provides high-quality data for pattern recognition and indexing, enabling efficient analysis of multiple samples.

Area of Science:

  • Materials Science
  • Crystallography
  • Analytical Chemistry

Background:

  • Physical form screening is crucial for pharmaceutical development.
  • Powder X-ray diffraction (PXRD) is a key technique for characterizing solid-state materials.
  • Efficient and accurate PXRD data collection is essential for high-throughput screening.

Purpose of the Study:

  • To evaluate two laboratory powder diffractometers for pattern indexing in physical form screening.
  • To assess the effectiveness of foil transmission geometry, monochromated radiation, and position-sensitive detectors for PXRD analysis.
  • To determine the suitability of the evaluated systems for rapid and reliable crystallographic analysis.

Main Methods:

  • Evaluation of two multisample laboratory powder diffractometers.

Related Experiment Videos

  • Utilizing foil transmission geometry, primary monochromated radiation, and a position-sensitive detector.
  • Data collection for six model compounds and analysis using the DICVOL-91 indexing program and DASH software for preferred orientation estimation.

    • Main Results:

    • Excellent angular resolution (FWHM as low as 0.06 degrees) was achieved.
    • Accurate lattice parameters were obtained for all tested compounds.
    • Preferred orientation was observed in specific compounds (clomipramine hydrochloride, famotidine) but did not impede overall data quality.
    • Data compared favorably with reference capillary data.

    Conclusions:

    • The combination of foil transmission geometry, monochromated radiation, and a position-sensitive detector is highly effective for PXRD pattern indexing and physical form screening.
    • This setup enables the analysis of 20-30 samples per day with high-quality data crucial for pattern recognition and indexing.
    • The collected data also present opportunities for crystal structure determination.