Hostname: page-component-586b7cd67f-rdxmf Total loading time: 0 Render date: 2024-11-27T05:36:07.724Z Has data issue: false hasContentIssue false

Evaluation and Application of an Improved Slit Probe for the X-Ray Secondary Emission Spectrometer

Published online by Cambridge University Press:  06 March 2019

Eugene P. Bertin*
Affiliation:
Radio Corporation of America Harrison, New Jersey
Get access

Abstract

X-ray probe accessories for commercial flat-crystal X-ray secondary emission (fluorescence) spectrometers have consisted of pinhole apertures in the primary or secondary X-ray beam. The smaller the aperture the lower the intensity, and apertures having diameters less than approx. 0.1 mm are of real value only for relatively high concentrations of elements having intense spectral lines.

There are two practical methods for increasing the intensity obtained with small apertures. One method is use of curved crystals ; it is applicable to any type of sample. The other method m use of a slit instead of a pinhole. It is limited to samples such as long linear inclusions ; sections of coated surfaces, diffusion couples, and metal-to-metal and metal-to-ceramic interfaces; and other layered structures where composition varies in a direction normal to the layers, but not along any one layer. The slit also has several other disadvantages that do not apply to the pinhole. However, when used with samples of the proper type, the slit has two outstanding advantages : Increased sensitivity and statistical precision are realized by replacing a pinhole of a given diameter with a slit of the same width ; alternatively, improved resolution is realized without loss of intensity by replacing the pinhole with a slit of smaller width. Moreover, the slit can be installed on a commercial X-ray spectrometer quickly and conveniently, and often allows useful X-ray probe work to be done on samples for which pinhole apertures would be inadequate.

A slit probe of the type already described by the writer has been improved and evaluated on a General Electric X-ray spectrometer equipped with a curved crystal. The improved accessory has been applied to studies of several metal-tometal and metal-to-ceramic systems. Some of these studies are discussed in detail.

Type
Research Article
Copyright
Copyright © International Centre for Diffraction Data 1964

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.)

References

1. Bertin, E. P., “X-Ray Probe with Slit Aperture in the Secondary Beam,” Anal. Chem. 36:441443, 1964.Google Scholar
2. Anal. Chem. 32:(9) 30A, 32A-36A, 38A, 1960.Google Scholar
3. Cosslett, V. E., Duncumb, P., Long, J. V. P., and Nixon, W. C., “Microanalysis by X-Ray Absorption, Fluorescence, Emission., and Diffraction Using Ultra-Fine X-Ray Sources,’ Advances in X-Ray Analysis, Vol. 1, University of Denver, Plenum Press, New York, 1958, pp. 329337.Google Scholar
4. Despujols, J., Roulet, H., and Senernaud, G., “X-Ray Fluorescence Analysis with a Focused Primary Beam,” X-Ray Optics and X-Ray Microanalysis, Proc. Third Intern. Symp., Stanford Univ., Calif., 1962, H. H. Pattee, V. E. Cosslett, and A. Engstrom (eds.), Academic Press, New York, 1963, pp. 445449.Google Scholar
5. Long, J. V. P. and Cosslett, V. E., “Some Methods of X-Ray Microchemical Analysis,” X-Ray Microscopy and Microradiography, Proc. First Intern. Symp., Cambridge, England, 1956, V. E. Cosslett, A. Engstrom, and H. H. Pattee (eds.), Academic Press, Inc., New York, 1957, pp. 435442.Google Scholar
6. Bertin, E. P. and Longobucco, R. J., “Some Special Sample Mounting Devices for the X-Ray Fluorescence Spectrometer,” Advances in X-Ray Analysis, Vol. 5, University of Denver, Plenum Press, New York, 1962, pp. 447456.Google Scholar
7. Bertin, E. P. and Longobucco, R. J., “X-Ray Spcctrometric Determination of Composition and Distribution of Sublimates in Receiving-Type Electron Tubes,” Advances in X-Ray Analysis, Vol. 7, University of Denver, Plenum Press, New York, 1964, pp. 566583.Google Scholar
8. Heinrich, K. F. J., “X-Ray Probe with CoIIimation of the Secondary Beam,” Advances in X-Ray Analysis, Vol 5, University of Denver, Plenum Press, New York, 1962, pp. 516526.Google Scholar
9. Raag, V., Bertin, E. P., and Longobucco, R. J., “Distribution of Cathode Sublimation Deposits in a Receiving Tube as Determined by X-Ray Spectrometric Scanning,” Advan. Electron Tube Techniques 2:249259, 1963.Google Scholar
10. Zimmerman, R. H., “Industrial Applications of X-Ray Methods for Measuring Plating Thickness,” Advances in X-Ray Analysis, Vol. 4, University of Denver, Plenum Press, New York, 1961, pp. 335350.Google Scholar
11. Zimmerman, R. H., “X-Rays Check Plating Thickness,” Iron Age- 186:(15), 8487, 1960.Google Scholar
12. Zimmerman, R. H., “Measuring Plating Thickness, Industrial Applications of X-Ray Methods,” Metal Finishing 59:(5), 6773, 1961.Google Scholar
13. Miller, D. C., “Norelco Pinhole Attachment,’ Advances in X-Ray Analysis, Vol. 4, University of Denver, Plenum Press, New York, 1961, pp, 513520.Google Scholar
14. Sloan, R. D., “X-Ray Spectrographic Analysis of Thin Films by the Milliprobe Technique,” Advances in X-Ray Analysis, Vol. 5, University of Denver, Plenum Press, New York, 1962, pp. 512515.Google Scholar
15. Wittig, W. J., “Development and Use of a Sernimicro X-Ray Fluorescence Attachment,” Develop. Appl. Spectry. 3:3644, 1964.Google Scholar
16. Wittig, W. J., “The Use of an X-Ray Fluorescence Semi-Microprobe Attachment in Metallurgy,” Advances in X-Ray Analysis, Vol. 8, University of Denver, Plenum Press, New York, 1965, pp. 248258.Google Scholar
17. Dunne, J. A., “A New Focusing Vacuum X-Ray Macroprobe Analyzer,” Advances in X-Ray Analysis, Vol. 8, University of Denver, Plenum Press, New York, 1965, pp. 223230.Google Scholar
18. Johnson, M., Beeley, P. R., and Nutting, J., “The Application of X-Ray Fluorescence in Probe Analysis to the Study of Segregation in Steels,” Advances in X-Ray Analysis, Vol. 8, University of Denver, Plenum Press, New York, 1965, pp. 259268.Google Scholar
19. Togel, K., “X-Ray Fluorescence Analysis of Small Quantities and Areas,” Siemens-Z. 36:497501, 1962.Google Scholar
20. Weyl, R., “Nondestructive Measurement of Composition and Thickness of Thin Layers by X-Ray Fluorescence,” Z. Angew. Phys. 13:283288, 1961.Google Scholar
21. General Electric Co., X-Ray Dept., 4855 Electric Av., Milwaukee, Wis., 53201, Butt. 8A-3862, 1962.Google Scholar
22. Philips Electronic Instruments, 750 South Fulton Av., Mount Vernon, N.Y., 10550, commercial literature.Google Scholar
23. Picker X-Ray Corp., 1275 Mamaroneck Av., White Plains, N.Y., commercial literature.Google Scholar
24. Siemens-America, Inc., 350 5th Av., New York, N.Y., 10001, General Equipment Catalog, 1962.Google Scholar
25. Lewis, R., Moll, S., Ogilvie, R., and Schur, S., “A Method for Identification, of Stratospheric Particles,” Advanced Research Metals Corp., Somerville, Mass., Research Rept. AMR-100S, 65 pp., 1960.Google Scholar
26. Stever, K. R., Johnson, J. L., and Heady, H. H., “X-Ray Fluorescence Analysis of Tungsten-Molybdenum Metals and Electrolytes,” Advances in X-Ray Analysis, Vol. 4, University of Denver, Plenum Press, New York, 1961, PP-475-487.Google Scholar
27. Bertin, E. P., “An Intensity-Ratio Technique for X-Ray Spectrometric Analysis of Binary Samples,” Anal, Chem. 36:826832, 1964.Google Scholar
28. Birks, L. S., Brooks, E. J., and Friedman, H., “Fluorescent X-Ray Spectre s copy,” Anal. Chem. 25:692697, 1953; Norelco Reptr. 3:44-49, 1956.Google Scholar
29. Storks, K. H. and Loomis, T. C., Bell Telephone Labs., Murray Hill, N.J., private communication.Google Scholar