Hostname: page-component-586b7cd67f-t7fkt Total loading time: 0 Render date: 2024-11-23T15:01:34.739Z Has data issue: false hasContentIssue false
  • English
  • Français

X-Ray Spectrographic Analysis of the 3-d Transition Metal Corrosion Products Using Potassium Bromide Disks*

Published online by Cambridge University Press:  06 March 2019

L. A. Schluter
L. A. Schluter*
Affiliation:
White Sands Missile Range New Mexico
Get access

Abstract

A technique has been developed for quantitative analysis of the major constituents in small samples (less than 0.1 g) of corrosion products found On various missile parts. The technique was developed primarily to aid in interpretation of X-ray diffraction patterns of multicomponent corrosion products. The corrosion sample is mixed with KBr and the mixture is pressed into a disk in the same fashion commonly used in infrared work. The Br Kβ1 line serves as an internal standard. Intensities of the element's Kα line and the internal standard are established by scanning through the appropriate Bragg angle and recording peak heights on a strip-chart recorder. A xenon-filled proportional detector and a pulse-height analyzer were used.

The percent of an element is determined by references to calibration curves which relate intensity ratios to weight ratios for the 3-d transition metals. The oxides of the metals were used in the preparation of the calibration curves. The weight ratio vs. intensity ratio relationship is linear over the weight ratio range 0.01 to 0.11. Data were collected using an air path and a helium path; the higher intensity ratios obtained with, the helium path, and the dependence of intensity on atomic number are illustrated. A comparison is made between the intensity ratios in a KBr matrix and in a NaBr matrix. The technique developed requires about 15 min sample preparation time.

Type
Research Article
Information
Advances in X-Ray Analysis , Volume 7: Twelfth Annual Conference on Applications of X-ray Analysis, August 7-9, 1963 , 1963 , pp. 590 - 597
Copyright
Copyright © International Centre for Diffraction Data 1963

Access options

Get access to the full version of this content by using one of the access options below. (Log in options will check for institutional or personal access. Content may require purchase if you do not have access.)

Footnotes

*

Paper read by Irwin B. Smith.

References

1. Klug, H. P. and Alexander, L. E., X-Ray Diffraction Procedures, John Wiley & Sons, Inc., New York, 1954, p. 384.Google Scholar
2. Birks, L. S., X-Ray Spectrochemical Analysis, Interscience Publishers, New York, 1959.Google Scholar
3. Liebhafsky, H. A., Pfeiffer, H. G., Winslow, E. H., and Zemany, P. D., X-Ray Absorption and Emission in Analytical Chemistry, John Wiley & Sons, Inc., New York, 1960.Google Scholar
4. Bertin, E. P. and Longobucco, R. J., “Sample Preparation Methods for X-Ray Fluorescence Emission Spectrometry,” Norelco Reporter 9: 31, 1962.Google Scholar
5. Perkin-Elmer Instruction Manual 990-9020, Perkin-Elmer Corp., Norwalk Conn., 1959.Google Scholar
6. Miller, D. C., “Some Considerations in the Use of Pulse-Height Analysis with X-Rays,” Norelco Reporter 4: 37, 1957.Google Scholar
7. Kiley, W. R., “The Function and Application of Counters and the Pulse Height Analyzer,” Norelco Reporter 7: 143, 1960.Google Scholar
8. “X-Ray Wavelengths for Spectrometer,” General Electric Co., Milwaukee, Wis., 1959.Google Scholar
9. Parrish, W. and Kohler, T. R., “Use of Counter Tubes in X-Ray Analysis,” Rev. Set, Imtr, 27: 795, 1956.Google Scholar
10. Dowling, P. H., Hendee, C. F., Kohler, T. R., and Parrish, W., “Counter for X-Ray Analysis,” Norelco Reporter 4: 23, 1957.Google Scholar
11. Lawson, K. E., Infrared Absorption of Inorganic Substances, Reinhold Publishing Corp., New York, 1961, p. 5.Google Scholar