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Introduction of a Nist Instrument Sensitivity Standard Reference Material for X-Ray Powder Diffraction

Published online by Cambridge University Press:  06 March 2019

James P. Cline
Affiliation:
National Institute of Standards and Technology Gaithersburg, MD 20899
Susannah B. Schiller
Affiliation:
National Institute of Standards and Technology Gaithersburg, MD 20899
Ron Jenkins
Affiliation:
National Institute of Standards and Technology Gaithersburg, MD 20899
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Abstract

Improvements in sample preparation methods have resulted in increased accuracy in x-ray powder diffraction intensity measurements. This improvement has focused scrutiny on the instrument as a potential source of error. NIST Standard Reference Material, SRM, 1976 consists of a sintered α alumina, corundum, plate certified with respect to 12 relative intensity values from 25 to 145 degrees 2θ. Its function is to allow for standardization of powder diffraction intensity as a function of 2θ angle (instrument sensitivity). An increase in the accuracy of interlaboratory comparisons of diffraction intensity and related determinations will result. Utilization of the SRM requires the user to collect intensity data from the test instrument in a manner which conforms to that used in the certification. Graphical interpretation of the ratio of these data to those on the certificate will allow for appropriate judgment as to the condition of the test instrument. Discontinuities in the data indicate a malfunctioning or misaligned instrument. Systematic bias, introduced by design characteristics of the test instrument, manifests itself in terms of a pattern in the data other than a horizontal straight line with value of one. This bias may be removed with the calculation and application of a correction curve.

Type
VI. XRD Instrumentation, Techniques and Reference Materials
Copyright
Copyright © International Centre for Diffraction Data 1991

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References

1) Crystallographic Databases, publication of IUCR, 1937, Chester UK, section 3.3 “Powder Diffraction File”, Jenkins, R. and smith, D.K., pp 158177 Google Scholar
2) Jenkins, R., Schreiner, W., and Dismore, P., Characterization of Powder Diffractometer Sensitivity, to be submitted to Powder DiffractionGoogle Scholar
3) Cline, J., S, Schiller, and Jenkins, R., In WorksGoogle Scholar
4) The SRM material was donated to MIST by International Business Machines Corporation, East Fishkill, N.Y. facility, through the efforts of Ron AndersonGoogle Scholar
5) Hubbard, C.R., Robbins, C.R., and Snyder, R.L., “XRD Quantitative Phase Analysis Using the NBS*Quant82 System” Adv. in X-ray Analysis. Vol 26 pp 149156 (1983)Google Scholar