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Homogeneity Characterization of NBS Spectrometric Standards II: Cartridge Brass and Low-Alloy Steel*

  • H. Yakowitz (a1), D. L. Vieth (a1), K. F. J. Heinrich (a1) and R. E. Michaelis (a1)

Abstract

Most modern instrumental methods of analysis depend on the use of known standards of composition for calibration. Newer analytical techniques, such as the solids mass spectrometer, laser probe and, especially, the electron-probe microanalyzer have reduced the amount of a sample which can be analyzed quantitatively to a range of about 0.1 to as small as 0.00005 μg. As a corollary to these microanalytical advances, homogeneity requirements have become severe to meet analytical standards. This paper describes a continuation of the National Bureau of Standards' effort to characterize more fully existing standards as to suitability for the new microanalytical techniques. An NBS cartridge brass sample in both the wrought (NBS-1102) and chill cast forms (NBS-C1102), as well as a low-alloy steel sample (NBS-463), have been investigated by means of electron-probe micreanalysis and optical metallography. Some 17 elements are contained in the brass, while 25 elements are found in the steel. Results for 10 elements in the steel and 6 elements in the brass are presented. In the steel, iron, nickel, copper, and silicon ate essentially distributed homogeneously at micron levels, while manganese, tantalum, niobium, zirconium, sulfur, and chromium are not. In the brass, copper and zinc are distributed homogeneously at micron levels while lead, sulfur, aluminum, and silicon are not. Electron-probe micreanalyzer results indicate that both NBS-1102 and NBS-C1102 brass are suitable for use as a calibration standard for electronprobe microanalysis as well as other microsnalyticat techniques, such as the solids mass spectrometer. The results for brass have been corroborated by a number of laboratories using the electron-probe analyzer.

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Contribution of the National Bureau of Standards, not subject to copyright.

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1. Michael, R. E. is, Yakowitz, H., and Moore, G. A., “Métallo graphic Characterization of an NBS Spectra metric Low-Alloy Steel Standard,” J. Res. Nat I. Bur. Std, A68:343 (1964). Issued in expanded form as Natl. Bur. Std. (U.S.) Misc. Publ. 260-3 (1964) 17 pp.
2. Michael, R. E. is, Wyman, L. L., and Flitsch, R., “Preparation of NBS Copper-Base Spectrochemical Standards,” Natl. Bur. Std. (U.S.), Misc. Publ, 260-2 (1964), 36 pp.
3. “Standard Methods for Estimating the Average Grain Size of Metals,” 1964 Book of ASTM Standards, Part 31 : 225 (1964) Plate III.
4. Polushkin, E. P., Defects and Failures of Metals, American Elsevier Publishing Co., Inc., New York (1956), p. 47 ff.
5. Duncumb, P. and Shields, P. K., “Effect of Critical Excitation Potential on the Absorption Correction in X-ray Microanalysis.” Tube Investments Research Laboratories Technical Report No. 181 (1964), 9 pp., 7 figures.
6. Castaing, R., “Application of Electron Probes to Local Chemical and Crystallographic Analysis,” thesis, University of Paris (1951), pp. 83 ff.
7. Heinrich, K. F. J., X-ray Absorption Uncertainty, The Electron Microprobe, John Wiley & Sons, Inc., New York (1966), p. 296.

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