Chemical characterization of environmental and industrial particulate samples†

Abstract

The characterization of particles, especially aerosol particles, is of great importance to many scientific fields. A relevant brief overview is given. A rigorous scheme of sampling and in-depth characterization of particulate samples has been developed in the authors’ laboratories and by collaborative groups, including investigations by the following techniques: total reflection X-ray fluorescence spectrometry for quantitative bulk characterization; solid-state speciation by valence band X-ray spectrometry using electron microprobe or Mössbauer spectrometry (only bulk particle characterization possible); scanning electron microscopy and electron probe microanalysis for automatic semiquantitative single particle characterization of particles ≥0.5 µm; transmission electron microscopy for semiquantitative single particle characterization of particles with diameters down to 10 nm; high resolution-scanning electron microscopy, which is also capable of characterizing particles morphologically and qualitatively down to 10 nm in diameter; secondary ion mass spectrometry for the study of trace elemental distributions and isotopic ratios in particles with diameters above 1 µm. It is the aim of this paper to show the advantages and characteristics of this scheme of analysis to match today′s requirements for topochemical methods of analysis. For this purpose a short overview of these methods for particle characterization is also presented.

References

1. H. R. Pruppacher and J. D. Klett, Microphysics of Clouds and Precipitation, Reidel, Dordrecht, 1978.
2. M. O. Andreae, in World Survey of Climatology, Vol. 16: Future Climates of the World: a Modelling Perspective, ed. Henderson-Sellers, A., Elsevier, Amsterdam, 1995, p. 347.
3. Aerosol Measurement, ed. Willeke, K., and Baron, P. A., Van Nostrand Reinhold, New York, 1993.
4. The Physical and Chemical Characterization of Individual Particles, ed, Spurney, K. R., Wiley, New York, 1986.
5. Particles in Our Air: Concentrations and Health Effects, ed. Wilson, R., and Spengler, J. D., Harvard School of Public Health, 1996.
6. M. Ebert, J. Dahmen, P. Hoffmann and H. M. Ortner, Spectrochim. Acta, Part B, 1997, 52, 967.
7. M. Ebert, P. Hoffmann, H. M. Ortner and J. Dahmen, GIT Fachz. Lab., 1996, 10/96, 982.
8. Analysis of Microelectronic Materials and Devices, ed. Grasserbauer, M., and Werner, H. W., Wiley, Chichester, 1991.
9. H. M. Ortner, P. Wilhartitz and B. Lux, in Proceedings of the 12th Plansee Seminar, 1990, Tyrolia, Innsbruck, ed. Bildstein, H., and Ortner, H. M., 1990, vol. 4, p. 279.
10. H. M. Ortner and P. Wilhartitz, Fresenius' J. Anal. Chem., 1990, 337, 686.
11. H. M. Ortner, The Influence of Trace Elements on the Properties of Hard Metals, COST 503 ‘Powder Based Materials’, vol. IV, EU, Brussels, 1997.
12. U. Metz, PhD Thesis, Technical University of Darmstadt, 1995.
13. H. M. Ortner, H. Petter and W. Birzer, in Proceedings of First Plasma-Technique Symposium, ed. Eschnauer, H., Huber, P., Nicoll, A. R., and Sandmeier, S., Plasma Technik, Switzerland, 1988, vol. 2, p. 237.
14. J. W. Niemantsverdriet, Spectroscopy in Catalysis, VCH, Weinheim, 1993.
15. M. Otto, Analytische Chemie, VCH, Weinheim, 1995, pp. 413–513.
16. Cosmic Dust, ed. McDonnel, A. M., Wiley, Chichester, 1978.
17. S. A. Sandford, Fundam. Cosmic Phys., 1987, 12, 1.
18. T. J. Bernatowicz and R. M. Walker, Phys. Today, 1997, 50/12, 26.
19. L. E. Murr and W. H. Kinard, Am. Sci., 1993, 81, 152.
20. F. J. Stadermann and E. K. Jessberger, in Proceedings of European Conference on Space Debris, ESA SD-01, 1993, p. 185.
21. M. Reichling and F. J. Stadermann, European Space Agency/ESTEC, 1995, PO 142355-2.
22. C. H. Heiss and F. J. Stadermann, European Space Agency/ESTEC, 1995, PO 150474.
23. F. J. Stadermann, PhD Thesis, University of Heidelberg, 1990.
24. H. J. Walls, Forensic Science, Sweet and Maxwell, London, 2nd edn., 1968.
25. R. J. Watling, B. F. Lynch and D. Herring, J. Anal. At. Spectrom., 1997, 12, 195.
26. H. W. Wenz, W. J. Lichtenberg and H. Katterwe, Fresenius' J. Anal. Chem., 1991, 341, 155.
27. M. R. Rampino, in World Survey of Climatology, Vol. 16: Future Climates of the World: a Modelling Perspective, ed. Henderson-Sellers, A., Elsevier, Amsterdam, 1995, p. 95.
28. P. Arndt, J. Bohsung, M. Maetz and E. K. Jessberger, Meteorit. Planet Sci., 1996, 31, 817.
29. L. J. Allamandola, S. A. Sandford and B. Wopenka, Science, 1987, 237, 56.
30. B. Wopenka, Earth Planet. Sci. Lett., 1988, 88, 221.
31. F. J. Stadermann, Phys. Unserer Zeit, 1992, 23, 197.
32. F. J. Stadermann and C. T. Olinger, Meteoritics, 1992, 27, 291.
33. R. Jaenicke, in Atmosphärische Spurenstoffe, ed. Jaenicke, R., VCH, Weinheim, 1987, p. 321.
34. M. Wentzel, H. J. Annegarn, G. Helas, S. Weinbruch, A. Balogh and J. S. Sithole, S. Afr. J. Sci., in the press.
35. H. Gleiter, Prog. Mater. Sci., 1989, 33, 223.
36. R. W. Siegel, in Material Science and Technology, Vol. 15: Processing of Metals and Alloys, ed. Cahn, R. W., VCHWeinheim, 1991, p. 583.
37. H. Gleiter, Nanostruct. Mater., 1992, 1, 1.
38. S. Weber, PhD Thesis, Technical University of Darmstadt, 1997.
39. M. Hein, P. Hoffmann, K. H. Lieser and H. M. Ortner, Fresenius' J. Anal. Chem., 1992, 342, 191.
40. P. Hoffmann, A. N. Dedik, J. Ensling, S. Weinbruch, S. Weber, T. Sinner, P. Gütlich and H. M. Ortner, J. Aerosol Sci., 1996, 27, 325.
41. S. Weinbruch, M. Wentzel, M. Kluckner, P. Hoffmann and H. M. Ortner, Mikrochim. Acta, 1997, 125, 137.
42. Handbook of Environmental Analysis, ed. Smith, R.-U., AOAC, McLean, VA, 2nd edn., 1995.
43. R. Klockenkämper, in Total Reflection X-Ray Fluorescence Analysis, ed. Winefordner, J. D., Chemical Analysis Series, Vol. 140, Wiley, New York, 1997, p. 151.
44. I. Injuk and R. van Grieken, Spectrochim. Acta, Part B, 1995, 50, 1787.
45. A. Shara, A. von Bohlen, R. Klockenkämper and D. Klockow, Quim. Anal., 1993, 12, 57.
46. M. Grasserbauer, Mikrochim. Acta, 1975, I, 563.
47. A. Meisel, G. Leonhardt and R. Szargau, X-Ray Spectra and Chemical Binding, Springer Series in Chemical Physics, Vol. 37, Springer, Berlin, 1989.
48. H. E. Höfer, G. P. Brey, B. Schulz-Dobrick and R. Oberhänsli, Eur. J. Mineral., 1994, 6, 407.
49. U. Rohr, PhD Thesis, Technical University of Darmstadt, 1996.
50. D. L. Sedlak and J. Hoigné, Atmos. Environ., Part A, 1993, 27, 2173.
51. J. H. Seinfeld, Atmospheric Chemistry of Air Pollution, Wiley, New York, 1986.
52. P. Gütlich, R. Linck and A. Trautwein, Mössbauer Spectroscopy and Transition Metal Chemistry, Springer, Berlin, 1978.
53. A. V. Krajnikov, A. N. Demidik and H. M. Ortner, Mater. Sci. Eng. A., 1997, 234–236, 357.
54. M. Grasserbauer, H. J. Dudek and M. F. EbelAngewandte Oberflächenanalyse, Springer, Berlin, 1985.
55. H. M. Ortner and P. Wilhartitz, Mikrochim. Acta, 1991, II, 177.
56. C. Xhoffer, L. Wouters, P. Artaxo, A. Van Put and R. Van Grieken, in Environmental Particles, ed. Buffle, J., and van Leeuwen, H. P., Environmental Analytical and Physical Chemistry Series, Lewis, Chelsea, MI, 1992, vol. 1, p. 107.
57. W. Jambers, L. de Bock and R. van Grieken, Fresenius' J. Anal. Chem., 1996, 355, 521.
58. B. Höflich, Diploma Thesis, Technical University of Darmstadt, 1997.
59. J. T. Armstrong, in Electron Probe Quantitation, ed. Heinrich, K. F. J., and Newbury, D. E., Plenum Press, New York, 1991, p. 261.
60. J. T. Armstrong and P. R. Buseck, X-ray Spectrom., 1985, 14, 172.
61. M. Kluckner, O. Brandl, S. Weinbruch, F. J. Stadermann and H. M. Ortner, Mikrochim. Acta, 1997, 125, 129.
62. G. Miehe, in Referate, 3. Jahrestagung der Deutschen Gesellschaft für Kristallographie, Oldenbourg, Munich, 1995, p. 51.
63. E. Bischoff, G. H. Campbell and M. Rühle, Fresenius' J. Anal. Chem., 1990, 337, 469.
64. G. Cressey, C. M. B. Henderson and G. van der Laan, Phys. Chem. Miner., 1993, 20, 111.
65. L. A. J. Garvie and A. J. Craven, Phys. Chem. Miner., 1994, 21, 191.
66. L. A. J. Garvie, A. J. Craven and R. Brydson, Am. Mineral., 1994, 79, 411.
67. M. T. Otten, B. A. Miner, J. H. Rask and P. R. Buseck, Ultramicroscopy, 1985, 18, 285.
68. T. Hofer and P. Warbichler, Ultramicroscopy, 1996, 63, 21.
69. T. Hofer, P. Warbichler and W. Grogger, Ultramicroscopy, 1995, 59, 31.
70. O. L. Kriwanek, A. J. Gubbens, N. Dellby and C. E. Meyer, Microsc. Microanal. Microstruct., 1992, 3, 187.
71. W. Grogger, F. Hofer and G. Kothleitner, Mikrochim. Acta, 1997, 125, 13.
72. W. Jambers, L. De Bock and R. Van Grieken, Analyst, 1995, 120, 681.
73. M. V. Johnston and A. S. Wexler, Anal. Chem., 1995, 67, 721A.
74. J. Injuk, H. Van Malderen, R. Van Grieken, E. Swietlicki, J. M. Knox and R. Schofield, X-Ray Spectrom., 1993, 22, 220.
75. J. Injuk, L. Breitenbach, R. Van Grieken and U. Wätjen, Mikrochim. Acta, 1994, 114/115, 313.
76. I. Borbely-Kiss, E. Koltay, Gy. Szabo, L. Bozo, E. Meszaros and A. Molnar, Nucl. Instrum. Methods Phys. Res., Sect. B, 1990, 49, 388.
77. M. Kasahara, K. Shinoda and K. Takahashi, J. Aerosol Sci., 1993, 24, Suppl. 1, 57.
78. F. G. Rüdenauer and W. Steiger, in Secondary Ion Mass Spectrometry: SIMS VI, ed. Benninghoven, A., Huber, A. M., and Werner, H. W., Wiley, Chichester, 1987, p. 361.
79. S. Gara, G. Stingeder, C. Tian, H. Hutter, H. Führer and M. Grasserbauer, in Secondary Ion Mass Spectrometry: SIMS VIII, ed. Benninghoven, A., Janssen, K. T. F., Thümpner, J., and Werner, H. W., Wiley, Chichester, 1992, p. 537.
80. F. J. Stadermann and H. M. Ortner, in Secondary Ion Mass Spectrometry: SIMS X, ed. Benninghoven, A., Hagenhoff, B., and Werner, H. W., Wiley, Chichester, 1997, p. 325.
81. Kontakte (Merck, Darmstadt), 1992, 2(the whole volume is dedicated to interference pigments).
82. S. Gunst, Diploma Thesis, Technical University of Darmstadt, 1997.
83. S. Gunst, S. Hetland, H. M. Ortner, A. Skogstad and Y. Thomassen, in Book of Abstracts, 3rd Symposium on ‘Speciation of Elements in Biological, Environmental and Toxicological Sciences’, Port Douglas, Australia, 1997, pp. 4–8.