Fluorescent X-ray Spectrography: Determination of Trace Elements

  • William J. Campbell
  • John W. Thatcher
Part of the Developments in Applied Spectroscopy book series (DAIS, volume 1)


Serious consideration should be given to the merits of using the available fluorescent X-ray spectrographic instrumentation and techniques for determining trace elements. Limits of detectability for trace elements in metal, oxide, solution, or mineral samples range from 0.1 to 100 ppm, depending on the element being determined, over-all sample composition, and complexity of the X-ray spectra; limits of detectability range from 0.01 to 1 μg for elements that have been preconcentrated by a chemical or physical process, for example, by ion-exchange membrane.


Spectral Line Atomic Number Line Intensity Scattered Radiation Tungsten Trioxide 
These keywords were added by machine and not by the authors. This process is experimental and the keywords may be updated as the learning algorithm improves.


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  1. 1.
    N.W.H. Addink, “The Determination of Trace Elements,” J. Iron and Steel Inst., 199–211, 1960.Google Scholar
  2. 2.
    I. Adler, “Application of X-ray Spectroscopy to Unsolved Problems in Geochemistry,” ASTM STP 269, 47–54, 1960.Google Scholar
  3. 3.
    G.E.B. Barstad and I.N. Refsdal, “Sensitive Quantitative Recording X-ray Spectrometers,” Rev. Sci. Instr. 29, 343–348, 1958.CrossRefGoogle Scholar
  4. 4.
    L.S. Birks, X-ray Spectrochemical Analysis, Interscience Publishers, Inc., New York, 1959, 137 pp.Google Scholar
  5. 5.
    B. Bolger, “Experiences with an X-ray Fluorescent Vacuum Spectrograph.” 5th Internat. Inst, and Measurements Conf., Stockholm, Sweden, Abs., 126–127, 1960.Google Scholar
  6. 6.
    C.S. Brandt and V.A. Lazar, “Analysis of Dried Plant Material by X-ray Emission Spectrograph,” Agr. and Food Chem. 6, 306–309, 1958.CrossRefGoogle Scholar
  7. 7.
    J.D. Brown, “X-ray Fluorescence Analysis Applied to Wax Processing and Cellulose Chemistry,” 6th Ottawa Symposium on Appl. Spectroscopy, Ottawa, Can., October 1959.Google Scholar
  8. 8.
    J.T. Campbell and H.L. Shalgosky, “X-ray Spectrographic Determination of Strontium,” Nature 183, 1481, 1959.CrossRefGoogle Scholar
  9. 9.
    W.J. Campbell, “Application of X-ray Spectroscopy to Trace Element Analysis,” 1st Eastern Anal. Symposium, New York, November 1959, paper 29.Google Scholar
  10. 10.
    W.J. Campbell, “The Determination of Germanium by Fluorescent X-ray Spectrography,” Univ. of Maryland, College Park, Md., Ph.D. thesis, 1956, 144 pp.Google Scholar
  11. 11.
    W.J. Campbell, Fluorescent X-ray Spectrographic Analysis: Studies of Low-Energy K, L, and M Spectral Lines, Bureau of Mines Rept. of Investigations 5538, 1959, 20 pp.Google Scholar
  12. 12.
    W.J. Campbell and H.F. Carl, “Fluorescent X-ray Spectrographic Analysis of Traces of Germanium,” Pittsburgh Conf. on Analytical Chemistry and Applied Spectroscopy, Pittsburgh, March 1956, paper 92.Google Scholar
  13. 13.
    W.J. Campbell, H.F. Carl, and C.E. White, “Quantitative Analyses by Fluorescent X-ray Spectrograph—Determination of Germanium in Coal and Coal Ash,” Anal. Chem. 29, 1009–1017, 1957.CrossRefGoogle Scholar
  14. 14.
    W.J. Campbell and M. Leon, Fluorescent X-ray Spectrograph for Dynamic Selective Oxidation Rate Studies: Design and Principles, Bureau of Mines Rept. of Investigations 5739, 1961, 21 pp.Google Scholar
  15. 15.
    W.J. Campbell, M. Leon, and J.W. Thatcher, “Flat Crystal X-ray Optics,” Proc. 6th Conf. on Ind. Applications of X-ray Analysis, Denver Research Inst., Denver, Colo., August 1957, 193–206.Google Scholar
  16. 16.
    W.J. Campbell, M. Leon, and J.W. Thatcher, Solution Techniques in Fluorescent X-ray Spectrograph, Bureau of Mines Rept. of Investigations 5497, 1959, 24, pp.Google Scholar
  17. 17.
    W.J. Campbell and J.W. Thatcher, Determination of Calcium Wolframite Concentrates by Fluorescent X-ray Spectrography, Bureau of Mines Rept. of Investigations 5416, 1958, 18 pp.Google Scholar
  18. 18.
    M.B. Cavanagh, The Application of X-ray Fluorescence to Trace Analysis, Naval Res. Lab. Rept. 4528, 1955, 4 pp.Google Scholar
  19. 19.
    E.N. Davis, and B.C. Hoeck, “X-ray Spectrographic Method for the Determination of Vanadium and Nickel in Residual Fuels and Charging Stocks,” Anal. Chem. 27, 1880–1884, 1955.CrossRefGoogle Scholar
  20. 20.
    E.N. Davis, and R.A. Van Nordstrand, “Determination of Barium, Calcium, and Zinc in Lubricating Oils—Use of Fluorescent X-ray Spectroscopy,” Anal. Chem. 26, 973–977, 1954.CrossRefGoogle Scholar
  21. 21.
    G.V. Dyroff and P. Skiba, “Determination of Trace Amounts of Iron, Nickel, and Vanadium on Catalysts by Fluorescent X-ray Spectrography,” Anal. Chem. 26, 1774–1778, 1954.CrossRefGoogle Scholar
  22. 22.
    C.W. Dwiggins, Jr., “Quantitative Determination of Low-Atomic-Number Elements Using Intensity Ratio of Coherent to Incoherent Scattering of X-rays,” Anal. Chem. 33, 67–70, 1961.CrossRefGoogle Scholar
  23. 23.
    C.W. Dwiggins, Jr. and H.N. Dunning, “Quantitative Determination of Nickel in Oils by X-ray Spectrography,” Anal. Chem. 31, 1040–1042, 1959.CrossRefGoogle Scholar
  24. 24.
    C.W. Dwiggins, Jr. and H.N. Dunning, “Quantitative Determination of Traces Vanadium, Iron and Nickel in Oils by X-ray Spectrography,” Anal. Chem. 32, 1137–1141, 1960.CrossRefGoogle Scholar
  25. 25.
    H.R. Erard and G. L. Underhill, General Operating Accuracies in Fluorescent X-ray Spectroscopy, Springfield Armory, Springfield, Mass., SA-TR20-2405, 1959, 53 pp.Google Scholar
  26. 26.
    D.A. Flikkema, R.P. Larsen, and R.V. Schablaske, The X-ray Spectrometric Determination of Uranium in Solution, Argonne Nat. Lab. Rept. 5641, Lemont, Ill., 1956, 9 pp.Google Scholar
  27. 27.
    H. Friedman, L.S. Birks, and E.J. Brooks, “Basic Theory and Fundamentals of Fluorescent X-ray Spectrographic Analysis.” ASTM STP 157, 3–26, 1954.Google Scholar
  28. 28.
    F.W.J. Garton and H.M. Davis, “Summarized Proceedings of a Colloquium on X-ray Fluorescence Analysis,” Brit. J. Appl. Phys. 10, 105–116, 1959.CrossRefGoogle Scholar
  29. 29.
    W.T. Grubb and P.D. Zemany, “X-ray Emission Spectrography Using Ion Exchange Membranes,” Nature 176, 221, 1955.CrossRefGoogle Scholar
  30. 30.
    C.C. Hale and W.H. King, Jr., “Direct Nickel Determinations in Petroleum Oils by X-ray at the 0.1 ppm Level,” Anal. Chem. 33, 74–77, 1961.CrossRefGoogle Scholar
  31. 31.
    K.F.J. Heinrich and T.D. McKinley, “The Determination of Impurities in Elemental Niobium and Its Compounds by X-ray Spectroscopy, Pittsburgh Conf. on Anal. Chem. and Appl. Spectroscopy, Pittsburgh, March 1959, paper 61.Google Scholar
  32. 32.
    L. F. Herzog, “Age Determination by X-ray Fluorescence, Rubidium-Strontium Ratio Measurement in Lepidolite,” Science 132, 293–294, 1960.CrossRefGoogle Scholar
  33. 33.
    T. M. Hess, Determination of Rare-Earth Oxides in Y 2 O 3 by Means of the X-ray Spectrograph, Yttrium Anal. Conf., Argonne National Laboratory, Lemont, Ill., Minutes, November 1956, 76 pp.Google Scholar
  34. 34.
    W.F. Hillebrand, “The Analysis of Silicate and Carbonate Rocks,” Geol. Survey Bull. 700, 32, 1919.Google Scholar
  35. 35.
    R.C. Hirt, W.R. Doughman, and J.B. Gisclard, “Application of X-ray Emission Spectrography to Air-Borne Dusts in Industrial Hygiene Studies,” Anal. Chem. 28, 1649–1651, 1956.CrossRefGoogle Scholar
  36. 36.
    W.S. Horton and W.D. Moak, Determination of Microgram Quantities of Thorium in Zircaloy II by X-ray Fluorescence Spectroscopy with Ion-Exchange Membranes, Knolls Atomic Power Lab. Rept. KAPL-M-WSH-4, 1959, 11 pp.Google Scholar
  37. 37.
    R.W. Jones The Determination of Impurities in Uranium by X-ray Fluorescence Spectrometry, Atomic Energy of Canada Ltd., Chalk River, Ontario, CRDC-842, 1959, 7 pp.Google Scholar
  38. 38.
    R.W. Jones Some Applications of X-ray Fluorescence Spectrography to the Determination of Uranium and Thorium, Atomic Energy of Canada Ltd., Chalk River, Ontario, CRDC-843, 1959, 10 pp.Google Scholar
  39. 39.
    W.L. Kehl and R.G. Russell, “Fluorescent X-ray Spectrographic Determination of Uranium in Water and Rrines,” Anal. Chem. 28, 1350–1351, 1956.CrossRefGoogle Scholar
  40. 40.
    J.W. Kemp, “The Future of X-ray Fluorescence Instrumentation,” ASTM STP 269, 55–62, 1960.Google Scholar
  41. 41.
    M.C. Lambert, Some Practical Aspects of X-ray Spectrography, Hanford Atomic Products Operation, Richland, Wash., HW-58967, 1959, 66 pp.Google Scholar
  42. 42.
    M.C. Lambert, X-ray Spectrographic Determination of Uranium and Plutonium in Aluminum Alloys and Other Reactor Fuel Materials, Reactor Fuel Measurement Techniques Symposium, Michigan State Univ., East Lansing, Mich., TID-7560, June 1958, 208 pp.Google Scholar
  43. 43.
    G.L. Lewis, Jr. and E.D. Goldberg, “X-ray Fluorescence Determination of Rarium, Titanium, and Zinc in Sediments,” Anal. Chem. 28, 1282–1285, 1956.CrossRefGoogle Scholar
  44. 44.
    H.A. Liebhafsky, H.G. Pfeiffer, E.H. Winslow, and P.D. Zemany, X-ray Absorption and Emission in Analytical Chemistry, John Wiley and Sons, Inc. New York, 1960, 357 pp.Google Scholar
  45. 45.
    H.A. Liebhafsky, H.G. Pfeiffer, and P.D. Zemany “Precision in X-ray Emission Spectrography,” Anal. Chem. 27, 1257–1258, 1955.CrossRefGoogle Scholar
  46. 46.
    F.W. Lytle, “Determination of Trace Elements in Plant Material by Fluorescent X-ray Analysis,” Univ. of Nevada, Reno, Nev., M.S. thesis, 1958.Google Scholar
  47. 47.
    F.W. Lytle and H.H. Heady, X-ray Emission Spectrographic Analysis of High-Purity Rare-Earth Oxides, Rureau of Mines Rept. of Investigations 5526, 1959, 9 pp.Google Scholar
  48. 48.
    M. Mack and N. Spielberg, “Statistical Factors in X-ray Intensity Measurements,” Spectrochimica Acta 12, 169–178, 1958.CrossRefGoogle Scholar
  49. 49.
    H.G. Pfeiffer and P.D. Zemany “Trace Analysis by X-ray Emission Spectrography Nature 174, 397, 1954.CrossRefGoogle Scholar
  50. 50.
    T.N. Rhodin “Chemical Analysis of Thin Films by X-ray Emission Spectrography,” Anal. Chem. 27, 1857–1861, 1955.CrossRefGoogle Scholar
  51. 51.
    E.R. Sandell, Colorimetric Determination pf Traces of Metal, Interscience Publishers Inc., New York, 1950, pp. 3–6.Google Scholar
  52. 52.
    R.E. Sladky Determination of Metallic Impurities in Uranyl Nitrate Solution by X-ray Fluorescence, Union Carbide Nuclear Co., Y-12 Plant, Oak Ridge, Tenn., Y-1276, December 1959, 25 pp.Google Scholar
  53. 53.
    N. Spielberg, “Intensities of Radiation from X-ray Tubes and the Excitation of Fluorescence X-rays,” Philips Res. Rept. 14, 215–236, 1959.Google Scholar
  54. 54.
    N. Spielberg, W. Parrish, and K. Lowitzsch, “Geometry of the Non-Focusing X-ray Fluorescence Spectrograph,” Spectrochimica Acta 8, 564–573, 1959.CrossRefGoogle Scholar
  55. 55.
    J.N. Van Niekerk and J.F. DeWet, “Trace Analysis by X-ray Fluoreseence Using Ion-Exchange Resins,” Nature 186, 380–381, 1960.CrossRefGoogle Scholar
  56. 56.
    L. Van Wambeke, “Geochemical Prospecting and Appraisal of Niobium-Rearing Carbonatites by X-ray Methods,” Econ. Geol. 55, 732–758, 1960.CrossRefGoogle Scholar
  57. 57.
    G.R. Webber, “Application of X-ray Spectrometric Analysis to Geochemical Prospecting,” Econ. Geol. 54, 816–828, 1959.CrossRefGoogle Scholar
  58. 58.
    P.D. Zemany, “The Minimum Amount of an Element Detectable by X-ray Spectrography.” 1st Eastern Anal. Symposium, New York, November 1959, paper 30.Google Scholar
  59. 59.
    P.D. Zemany, H.G. Pfeiffer, and H.A. Liebhafsky, “Precision in X-ray Emission Spectrography—Background Present,” Anal. Chem. 31, 1776–1778, 1959.CrossRefGoogle Scholar
  60. 60.
    P.D. Zemany, W.W. Welbon, and G.L. Gaines, “Determination of Microgram Quantities of Potassium by X-ray Emission Spectrography of Ion Exchange Membranes,” Anal. Chem 30, 299–300, 1958.CrossRefGoogle Scholar

Copyright information

© Society for Applied Spectroscopy 1962

Authors and Affiliations

  • William J. Campbell
    • 1
  • John W. Thatcher
    • 1
  1. 1.United States Department of the InteriorBureau of Mines, College Park Metallurgy Research CenterCollege ParkUSA

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