By Robert L. Snyder (auth.), Camden R. Hubbard, Charles S. Barrett, Paul K. Predecki, Donald E. Leyden (eds.)
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Extra info for Advances in X-Ray Analysis: Volume 26
HUBBARD TABLE 1. 533 *Corrected for thermal expansion. 2 °c. t-~9 . 40345 x 10 Table 2. Observed and Calculated 29 (Si sample 11115, a. 004 48 I. ACCURACY IN X-RAY POWDER DIFFRACTION x-ray exposure, humidity and heat. The powder is purposely of large crystallite size «200 mesh) to enhance preferrential orientation in packed mounts. A well oriented sample can be prepared by front loading and pressing with a microscope slide. Parafocusing diffractometer measurements from such a sample will yield only OO!
INTRODUCTION The large majority of publications on accuracy in powder diffraction deal with diffraction angle and lattice parameter determinations. This paper describes a preliminary study of a number of factors that contribute to the accuracy of the intensities. Accurate intensity data are required in a number of applications such as quantitative phase analysis, crystal structure refinement, line profile determination and similar studies. The introduction of the counter tube diffractometer 35 years ago greatly improved the accuracy over film methods but it remains surprisingly difficult to make accurate measurements even now.
In most quantitative analyses the situation is reversed and great accuracy in the d-value is generally not required, except in those cases where one is trying to correlate changes in unit cell dimension with compositional variations. An accurate intensity measurement is generally a critical first step in any quantitative analytical scheme, and the final accuracy in calculated phase concentration obtained is invariably limited by the accuracy of the measured intensity. It is thus clear that for powder work in general, the analyst must be able to control the accuracies of 25 I.