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Micro X‐ray diffraction on capillary powder samples: a novel and effective technique for overcoming preferred orientation
Author(s) -
Bergese P.,
Bontempi E.,
Colombo I.,
Depero L. E.
Publication year - 2001
Publication title -
journal of applied crystallography
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 1.429
H-Index - 162
ISSN - 1600-5767
DOI - 10.1107/s0021889801012237
Subject(s) - powder diffraction , diffraction , orientation (vector space) , materials science , amorphous solid , detector , capillary action , x ray crystallography , crystallography , optics , analytical chemistry (journal) , composite material , chromatography , chemistry , mathematics , physics , geometry
In past years, both experimental and analytical approaches have been developed for eliminating preferred orientation effects on powder X‐ray diffraction patterns. The state of the art does not allow one to face the problem without difficult sample treatments, mechanical randomization, pole‐figure study or pattern fitting based on the Rietveld approach. These methods are time consuming or need the knowledge of all the structural parameters, and, moreover, must be managed by specialized operators. Besides, none of the above techniques can be applied to powder samples of drugs loaded into polymeric carriers, the diffraction patterns of which present a structured amorphous halo from which the crystalline drug peaks rise up. In this paper, it is shown that micro X‐ray diffraction on capillary powder samples, combined with a two‐dimensional detector, is a promising solution to preferred orientation problems, since it provides easy and rapid preparation of randomly oriented powder samples, fast measurements (acquisition times of a few minutes) and correct powder diffraction patterns.