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

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

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To copyright. 45 Not subject 46 I. ACCURACY IN X-RAY POWDER DIFFRACTION standards are needed which fall into three general categories: internal standards, pure phase standards, and solid solution standards. To meet these needs the National Bureau of Standards (NBS) initiated a program to develop XRD standards. The first standard, SRM640 silicon powder, was certified by NBS in 1975 (Hubbard, Swanson and Mauer). Since then over 850 units have been sold through the Office of Standard Reference Materials and the stock has been depleted.

4. 5. 6. 7. 8. 9. 10. 11. 12. A. Brown, J. W. Edmonds and C. M. Foris, "Reproducibility and Precision of Guinier Patterns Using Powdered Silicon Calibrant", Adv. X-ray Anal. 24 111 (Edited by Deane K. Smith, Plenum Press, 1981)~ A. Brown and C. M. Foris, "Precision and Reproducibility of Lattice Parameters from Guinier Powder Patterns: Followup and Assessment". (For publication in Adv. X-ray Anal. 1983). C. R. Hubbard, H. E. Swanson and F. A. Mauer, "A Silicon Powder Diffraction Standard Reference Material", J.

4 Correction for Residual Errors: A consistent difference was observed between lattice parameters obtained from calibrated Guinier patterns and values for the same samples as given by diffractometer measurements. Thus for Gonio 1 these parameters were greater than the Guinier values such that K ~ 4, while for Gonio 2 the discrepancy was somewhat larger but negative. 005°. For Gonio 1 the best agreement for these two materials 16 I. 02°. The absolute encoder was reset by this amount, and the specimens were made up again and re-run to check the effectiveness of the correction.

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