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Advances in X-Ray Analysis: Volume 26 by Robert L. Snyder (auth.), Camden R. Hubbard, Charles S.

By Robert L. Snyder (auth.), Camden R. Hubbard, Charles S. Barrett, Paul K. Predecki, Donald E. Leyden (eds.)

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287, 5). The NBS silicon powder used was prepared from a large single crystal and each particle is a single crystal fragment so that the particle and crystallite sizes are the same. The study was made with a series of specimens prepared from the five particle size ranges described above. The crystallite size effect can be observed by rotating the specimen around the axis normal to the center of the specimen surface while the diffractometer is set at the peak position, and recording the intensity on a strip chart, Fig.

ACCURACY IN X-RAY POWDER DIFFRACTION Correction functions for these errors can, in principle at least, be applied relatively easily with the modern computer-controlled diffractome~er since they can all be described in terms of known parameters. The only term really in any doubt is the axial divergence term which was first described by Pike. 3 It seems, at least intuitively, that there must be a problem with the Pike axial divergence term at low angles since it involves cot and csc functions which become infinite as 26 approaches zero.

A square was used to see if the surface was flat and normal to the axis. Once the specimen was prepared the particles were tightly bonded and the surfaces stable. All specimens were examined with a binocular microscope and given the X-ray test described below. PRECISION OF METHOD The inherent precision of the data collection and reduction methods was determined with carefully controlled conditions. 04° steps and 1 second count time per step. The specimen was not moved between runs and the experimental time was about three minutes for the four reflections.

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