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Recent Advances in Quantitative X-Ray Spectrometric Analysis by Solution Techniques

Published online by Cambridge University Press:  06 March 2019

Eugene P. Bertin
Eugene P. Bertin*
Affiliation:
Radio Corporation of America Electronic Components and Devices Harrison, New Jersey
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Abstract

Usually X-ray spectrometric analyse? of samples in their original forms—solid, powder, small fabricated parts, liquid, etc.—are more rapid and convenient than analyses by any other method. Thus, the analyst is well advised to strive to analyze samples in their original form whenever practical. However, it is often necessary to reduce nonliquid samples to some other form, for example, when standards are unavailable in the original form, when the same substance is received for analysis in a variety of forms, when homogeneity or matrix effects are severe, or when an internal standard must be added. In such cases, samples and standards are often reduced to a powder, a fusion product, or a solution. If the decision is made to put the sample into solution, the many well-known advantages of solution techniques are realised, including: (1) homogeneity; (2) easy preparation of standards and blanks; (3) easy concentration, dilution, separation, and other treatment; (4) reduced matrix effects and wide choice of ways to deal with matrix effects; (5) wide choice of ways to present the specimen to the spectrometer; and (6) applicability of internal-standard, standard-addition or -dilution, indirect, absorption, and scatter methods. This paper reviews work reported since 1960 in which the specimen is presented to the spectrometer in liquid form. The review is not particularly critical and stresses experimental techniques and treatment of data rather than specific materials and results. The work is discussed in the following categories: (1) sensitivity ; (2) liquid-specimen cells; (3) interaction of primary beam and liquid specimens; (4) matrix effects; (5) indirect (association) analysis; (6) X-ray scatter methods; and (7) X-ray absorption-edge spectrometry.

Type
Research Article
Information
Advances in X-Ray Analysis , Volume 11: Sixteenth Annual Conference on Applications of X-ray Analysis, August 9-11, 1967 , 1967 , pp. 1 - 22
Copyright
Copyright © International Centre for Diffraction Data 1967

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References

1. Bertin, E. P., “Solution Techniques in X-Ray Spectrometric Analysis,” Nurelco Reptr. 12: 15–26, 1965.Google Scholar
2. Campbell, W. J., “Fluorescent X-Ray Spectrographic Analysis of Trace Elements, Including Thin Films,” Am. Soc. Testing and Mater., Spec. Tech. Publ. 349: 48–69, 1964.Google Scholar
3. Campbell, W. J., Leon, M., and Thatcher, J. W., “Solution Techniques in Fluorescent X-Ray Spectrography,” U.S. Bur. Mines Rept. Invest. 5497 (24 pp.), 1959.Google Scholar
4. Bertin, E. P. and Longobucco, R. J., “Sample-Preparation Methods for X-Ray Fluorescence Emission Spectrometry,” Narelco Reptr. 9: 31–43, 1962.Google Scholar
5. Gunri, E. L., “X-Ray Spectrographic Analysis of Liquids and Solutions,” Am. Soc. Testing and Mater., Spec. Tech. Publ. 349: 70–85, 1964.Google Scholar
6. Louis, R., “X-Ray Analysis of Mineral Oil Products,” Erdoel Kohle 17: 360–367, 1964.Google Scholar
7. Louis, R., “X-Ray Analysis in the Petroleum Industry,” Erdoel Kohle 18: 187–190, 1965.Google Scholar
8. Cullen, T. J., “X-Ray Spectrometric Analysis of Solutions, a Comparison of Techniques,” Pittsburgh Conf. Anal. Chem. Appl. Spectry., 1963.Google Scholar
9. Jones, R. A., “Determination of Sulfur in Gasoline by X-Ray Emission Spectrography,” Anal. Chem. 33: 71–74, 1961.Google Scholar
10. Louis, R., “X-Ray Emission Analysis of Lubricating Oils,” Z. Anal. Chem. 201: 336–348, 1964.Google Scholar
11. Louis, R., “Detection Limits in X-Ray Emission Spectral Analysis of Mineral Oils,” Z. Anal. Chem. 208: 34–43, 1965.Google Scholar
12. Kang, C. C., Keel, E. W., and Solomon, E., “Determination of Traces of Vanadium, Iron, and Nickel in Petroleum Oils by X-Ray Emission Spectrography,” Anal. Chem. 32: 221–225, 1960.Google Scholar
13. Hale, C. C. and King, W. H. Jr., “Direct Nickel Determinations in Petroleum Oils by X-Ray at the 0.1-P.P.M. Level,” Anal. Chem. 33: 74–77, 1961.Google Scholar
14. Gunn, E. L., “Problems of Direct Determination of Trace Nickel in Oil by X-Ray Emission Spectrography,” Anal. Chem. 36: 2086–2090, 1964.Google Scholar
15. Gunn, E. L., “Practical Methods of Solving Absorption and Enhancement Ploblems in X-Ray Emission Spectrography,” Develop. Appl. Spectry. 3: 69–96, 1964.Google Scholar
16. Croke, J. F., Pfoscr, W. J., and Solazzi, M. J., “New Automatic X-Ray Spectrometer in Industrial Control,” Norelco Reptr. 11: 129–131, 1964.Google Scholar
17. Siemes, H., “X-Ray Fluorescence Spectrometric Determination of Light Elements in Low Concentrations in Water Solutions,” Z. Anal. Chem. 199: 321–334, 1964.Google Scholar
18. Champion, K. P. and Whittem, R. N., “Utilization of Increased Sensitivity of X-Ray Fluorescence Spectrometry Due to Polarization of the Background Radiation, “Nature 199: 1082, 1963.Google Scholar
19. Bertin, E. P. and Longobucco, R. J., “Some Special Sample Mounting Devices for the X-Ray Fluorescence Spectrometer,” in: W. M. Mueller (ed.), Advances in X-Ray Analysis. Vol. 5, Plenum Press, New York, 1962, pp. 447–456.Google Scholar
20. Bertin, E. P. and Longobucco, R. J., “X-Ray Spectrometric Analysis—Nickel, Coppet, Silver, and Gold in Plating Baths,” Metal Finishing 60(3): 54–58, 1962.Google Scholar
21. Beard, D. W. and Proctor, E. M., “A Method of Liquid Analyses Providing Increased Sensitivity for Light Elements,” in: J. B. Newkirk and G. R. Mallett (eds.), Advances in X-Ray Analysis, Vol. 10, Plenum Press, New York, 1967, pp. 506–519.Google Scholar
22. Campbell, W. J., “Apparatus for Continuous Fluorescent X-Ray Spectrograph ic Analysis of Solutions,” Appl. Spectry. 14: 26–27, 1960.Google Scholar
23. Chan, F. L., “Apparatus for Analysis of Liquid Samples by the X-Ray Fluorescence Method with a Vacuum Spectrograph,” Develop. Appl. Spectry. 5: 59–75, 1966.Google Scholar
24. Hudgens, C. R. and Pish, G., “X-Ray Fluorescence Emission Analysis of Slurries,” Develop. Appl. Spectry. 5: 25–29, 1966.Google Scholar
25. Campbell, W. J. and Leon, M., “Fluorescent X-Ray Spectrograph for Dynamic Selective Oxidation- Rate Studies—Designand Applications,” U.S. Bur. Mines Repl. Invest. 5739 (21 pp.), 1961.Google Scholar
26. Karttunen, J. O., “Separation and Fluorescent X-Ray Spectrometric Determination of Zirconium, Molybdenum, Ruthenium, Rhodium, and Palladium in Solution in Uranium-Base Fissium Ailoys,” Anal. Chem. 35: 1044–1049, 1963.Google Scholar
27. Zimmerman, R. H. and Heller, H. A., “Quantitative Determination of Major and Minor Constituents in Gold Plating Baths by X-Ray Fluorescence Analysis,” Third National Meeting, Soc. Appl. Spectry., Cleveland, 1964.Google Scholar
28. Gunn, E. L., “Determination of Lead in Gasoline by X-Ray Fluorescence Using an Internal Intensity Reference,” Appl. Spectry. 19: 99–102, 1965.Google Scholar
29. Smith, H. F. and Royer, R. A., “Determination of Aluminum in Organo-Aluminum Compounds by X-Ray Fluorescence,” Anal. Chem. 35: 1098–1099, 1963.Google Scholar
30. Bertin, E. P., Longobucco, R. J., and Carver, R. J., “Simplified Routine Method for X-Ray Absorption-Edge Spectrometric Analysis,” Anal. Chem. 36: 641–655, 1964.Google Scholar
31. Hakkila, E. A. and Waterbury, G. R., “Applications of X-Ray Absorption-Edge Analysis,” Develop. Appl. Spectry. 2: 297–307, 1963.Google Scholar
32. Hakkila, E. A. and Waterbury, G. R., “X-Ray Absorption-Edge Determination of Cobalt in Complex Mixtures,” in: W. M. Mueller (ed,), Advances in X-Ray Analysis, Vol. 5, Plenum Press, New York, 1962, pp. 379–388.Google Scholar
33. Dunn, H. W., “X-Ray Absorption-Edge Analysis,” Anal. Chem. 34: 116–121, 1962.Google Scholar
34. Griffin, L. H., “Iron-55 X-Ray Absorption Analysis of Organically Bound Chlorine Using Conventional Proportional Counting Facilities,” Anal. Chem. 34: 606–609, 1962.Google Scholar
35. Pierron, C. D. and Munch, R. H., “Rapid X-Ray Fluorescence Method for Determination of V, Cu, Mo, Ti, Co, and Ni,” Develop. Appl. Spectry. 2: 360–365, 1962.Google Scholar
36. Visapaa, A., “Determination by X-Ray Fluorescence of Microgram Amounts of Strontium in Water and Milk,” Teknillisen Kemim Aikakausilehti 20: 146–151, 1963: C.A. 59: 8121c, 1963.Google Scholar
37. Visapaa, A., “Determination by X-Ray Fluorescence of Microgram Amounts of Barium in Water,” teknillisen Kemian Aikakausilehti 20: 563–568, 1963; C.A. 60:7793b, 1964.Google Scholar
38. Hirokawa, K., Shimanuki, T., and Goto, H., “Determination of Manganese in Ferromingancse and Chromium in Ferrochromium by X-Ray Fluorescent Spectroscopy,” Sci. Rept. Res. Inst. Tohuku Univ., Ser. A 15: 127–132, 1963.Google Scholar
39. Kirchmavr, H. R. and Mach, D., “X-Ray Fluorescence Analysis of Rare-Earth Metal-Manganese Alloys,” Z. Metallk. 55: 247–250, 1964.Google Scholar
40. Kuilbom, S. D., Pollard, W. K., and Smith, H. F., “Combined Infrared and X-Ray Spectrometric Method for Determining Sulfonate and Sulfate Concentration of Detergent Range Alkylbenzene Sulfonate Solutions,” Anal. Chem. 37: 1031–1034, 1965.Google Scholar
41. Caley, J. L., “Use of X-Ray Emission Spectrography for Petroleum Product Quality and Process Control,” in: W. M. Mueller and M, Fay (eds.), Advances in X-Ray Analysis, Vol. 6, Plenum Press, New York, 1963. pp. 396–402.Google Scholar
42. Tomldns, M. L., Borun, G. A., and Fahlbusch, W. A., “Quantitative Determination of Tantalum, Tungsten, Niobium, and Zirconium in High-Temperature Alloys by X-Ray Fluorescent Solution Method,” Anal. Chem. 34: 1260–1263, 1962.Google Scholar
43. Blank, G. R. and Heller, H. A., “X-Ray Spectrometric Determination of Thorium in Refined Uranium Materials,” Norelco Reptr. 8: 112–115, 1961; Develop. Appl. Spectry. 1: 3–15, 1962.Google Scholar
44. Blank, G. R. and Heller, H. A., “X-Ray Spectrometric Determination of Zirconium in Refined Uranium Materials,” Norelco Reptr. 9: 23–27, 1962.Google Scholar
45. Boyd, B. R. and Dryer, H. T., “Analysis of Nonmetallics by X-Ray Fluorescence Techniques,” Develop. Appl. Spectry. 2: 335–349, 1963.Google Scholar
46. Blank, G. R. and Heller, H. A., “X-Ray Spectrometric Determination of Copper, Tin, and Uranium in Bronze Heat-Treating Material,” in: W. M. Mueller fed.), Advances in X-Ray Analysis, Vol. 4. Plenum Press, New York, 1961, pp. 457–473.Google Scholar
47. Hakkila, E. A., Hurley, R. G., and Waterbury, G. R., “X-Ray Fluorescence Spectrometric Determination of Zirconium and Molybdenum in the Presence of Uranium, ” Anal. Chem. 36: 2094–2097, 1964.Google Scholar
48. Strasheim, A. and Wybenga, F. T., “Determination of Certain Noble Metals in Solution by Means of X-Ray Fluorescence Spectroscopy. I. Determination of Platinum, Gold, and Iridium,” Appl. Spectry. 18: 16–20, 1964.Google Scholar
49. Wybenga, F. T. and Strasheim, A., “Determination of Certain Noble Metals in Solution by Means of X-Ray Fluorescence Spectroscopy. II. Determination of Palladium, Rhodium, and Ruthenium,” Appl. Spectry. 20: 247–250, 1966.Google Scholar
50. Bartkiewicz, S. A. and Hammatt, E. A., “X-Ray Fluorescence Determination of Cobalt, Zinc, and Iron in Organic Matrices,” Anal. Chem. 36: 833–836, 1964.Google Scholar
51. Haycock, R. F., “Determination of Barium, Calcium, and Zinc in Additives and Lubricating Oils by X-Ray Fluorescence Spectroscopy,” J. Inst. Petrol 50: 123–128, 1964.Google Scholar
52. Mitchell, B. J. and O'Hear, H. J., “General X-Ray Spectrographic Solution Method for Analysis of Iron-, Chromium-, and/or Manganese-Bearing Materials,” Anal. Chem. 34: 1620–1625, 1962.Google Scholar
53. Scott, R. B., “X-Ray Spectrographic Analysis of Antimonials,” Appl. Spectry. 1: 17–23, 1962.Google Scholar
54. Cullen, T. J., “Coherent Scattered Radiation Internal Standardization in X-Ray Spectrometric Analysis of Solutions,” Anal. Chem. 34: 812–814, 1962.Google Scholar
55. Lopp, V. R. and Claypool, C. G., “Direct Determination of Vanadium and Nickel in Crude Oils by X-Ray Fluorescence,” in: W. M. Mueller (ed.), Advances in X-Ray Analysis, Vol. 3, Plenum Press, New York, 1960, pp. 131–137.Google Scholar
56. Stever, K. R., Johnson, J. L., and Heady, H. H., “X-Ray Fluorescence Analysis of Tungsten-Molybdenum Metals and Electrolytes,” in: W. M. Mueller (ed.), Advances in X-Ray Analysis, Vol. 4, Plenum Press, New York, 1961, pp. 474–487.Google Scholar
57. Jones, R. A., “Determination of Manganese in Gasoline by X-Ray Emission Spectrography,” Anal. Chem. 31: 1341–1344, 1959.Google Scholar
58. Gunn, E. L., “Absorption Effects in X-Ray Fluorescence Measurement of Elements in Oil,” in: W. M. Mueller and M. Fay (eds.), Advances in X-Ray Analysis, Vol. 6, Plenum Press, New York, 1963, pp. 403–416.Google Scholar
59. Dwiggins, C. W. Jr., “Automated Determination of Elements in Organic Samples Using X-Ray Emission Spectrometry,” Anal. Chem. 36: 1577–1581, 1964.Google Scholar
60. Carter, H. V., “Simplified Mathematical Matrices for Solution Analysis,” Norelco Reptr, 13: 45–47, 1966.Google Scholar
61. Haldfila, E. A. and Waterbury, G. R., “X-Ray Fluorescence Spectrometric Determination of Chromium, Iron, and Nickel in Ternary Alloys,” Anal. Chem. 37: 1773–1775, 1965.Google Scholar
62. Schindler, M. J., Month, A., and Antalec, J., “An X-Ray Fluorescence Technique for Analysis of Iron-Nickel Films over an Extremely Wide Range of Thickness and Composition,” Pittsburgh Conf. Anal. Chem. Appl. Spectry., 1961.Google Scholar
63. Rudolph, J. S. and Nadclin, R. J., “Determination of Microgram Quantities of Chloride in High- Purity Titanium by X-Ray Spectrochemical Analysis,” Anal. Chem. 36: 1815–1817, 1964.Google Scholar
64. Smith, G. S., “A Useful Technique in X-Ray Fluorescence Spectrography,” Chem. Ind. (London) 1963(22): 907-909.Google Scholar
65. Mathies, J. C., Lund, P. K., and Eide, W., “X-Ray Spectroscopy in Biology and Medicine. IV. A Simple, Indirect, Sensitive Procedure for the Determination of Nitrogen (Ammonia) at the Microgram and Submicrogram Level,” Anal. Biochem. 3:408–414, 1962; Norelco Reptr. 9:93-95, 1962.Google Scholar
66. Papariello, G. J., Letterman, H., and Mader, W. J., “X-Ray Fluorescent Determination of Organic Substances Through Inorganic Association,” Anal. Chem. 34: 1251–1253, 1962.Google Scholar
67. McCue, J. C., Bird, L. L., Ziegler, C. A., and O'Connor, J. J., “X-Ray Rayleigh Scattering Method for Determination of Uranium in Solution,” Anal. Chem. 33: 41–43, 1961.Google Scholar
68. Ziegler, C. A., Bird, L. L., and Chleck, D. J., “X-Ray Rayleigb Scattering Method for Analysis of Heavy Atoms in Low-Z Media,” Anal. Chem. 31: 1794–1798, 1959.Google Scholar
69. Dwiggins, C. W. Jr., “Quantitative Determination of Low Atomio Number Elements Using Intensity Ratio of Coherent to Incoherent Scattering of X-Rays; Determination of Hydrogen and Carbon,” Anal. Chem. 33: 67–70, 1961.Google Scholar
70. Toussaint, C. J. and Vos, G., “Quantitative Determination of Carbon in Solid Hydrocarbons Using the Intensity Ratio of Incoherent to Coherent Scattering of X-Rays,” Appl. Spectry. 18: 171–174, 1964.Google Scholar
71. Dodd, C. G., “X-Ray Absorption-Edge Spectrometry,” in: Proceedings of Symposium on Physics and Nondestructive Testing, Southwest Research Institute, San Antonio, Tex., 1962, pp. 199-221.Google Scholar
72. Stewart, J. H. Jr., “Determination of Thorium by Monochromatic X-Ray Absorption,” Anal. Chem. 32: 1090–1092, 1960.Google Scholar
73. Heinrich, K. F. J., “X-Ray Absorption Uncertainty,” in: E. D. McKinley, K. F. J. Heinrich, and D. B. Wittry (eds.), The Electron Microprobe, John Wiley and Sons, New York, 1966, pp. 296–377.Google Scholar
74. Stainer, H. M., “X-Ray Mass Absorption Coefficients, a Literature Survey,” U.S. Bur. Mines Inform. Circ. 8166 (124 pp.), 1963.Google Scholar
75. Dodd, C. G., “Applications of Optical and Electronic Dispersion in X-Ray Absorption-Edge Spectrometry,” in: W. M. Mueller (ed.), Advances in X-Ray Analysis, Vol. 3, Plenum Press, New York, 1960, pp, 11–39.Google Scholar
76. Hakkila, E. A., Hurley, R. G., and Waterbury, G. R., “A Three-Wavelength X-Ray Absorption-Edge Method for Determination of Plutonium in Nitrate Media,” Anal. Chem. 38: 425–428, 1966.Google Scholar
77. Knspp, K. T., Lindahl, R. H., and Mabis, A. J., “An X-Ray Absorption Method for Elemental Analysis,” in: W. M. Mueller, G. R. Mallett, and M. J. Fay (eds.), Advances in X-Ray Analysis, Vol. 7, Plenum Press, New York, 1964, pp. 318–324.Google Scholar
78. Cullen, T. J., “Internal Differential X-Ray Absorption-Edge Spectrometry,” Anal. Chem. 37: 711–713, 1965.Google Scholar