Skip to main content
Log in

Design of spectroelectrochemical cell for in situ X-ray absorption fine structure measurements of bulk solution species

  • Published:
Journal of Applied Electrochemistry Aims and scope Submit manuscript

Abstract

A purpose-built spectroelectrochemical cell for in situ fluorescence XAFS (X-ray absorption fine structure) measurements of bulk solution species is described. The cell performance was demonstrated by the collection of europium L3-edge XANES (X-ray absorption near edge structure) during constant-potential electrolysis of 14.2mmEuCl3.6H2Oin1mH2SO4 aqueous electrolyte. Additionally discussed in this report are the probabilities of 2p3/2→5d electronic transitions pertaining to Euiii and Euii ions. Implications for the use of XANES in studying intermediate-valence materials, and some potential applications of the presently reported spectroelectrochemical cell are described.

This is a preview of subscription content, log in via an institution to check access.

Access this article

Price excludes VAT (USA)
Tax calculation will be finalised during checkout.

Instant access to the full article PDF.

Similar content being viewed by others

References

  1. H. D. Abruna, G. M. Bommarito and H. S. Yee, Acc. Chem. Res. 28 (1995) 273.

    Google Scholar 

  2. H. D. Abruna (Ed.), `Electrochemical Interfaces. Modern Techniques for In Situ Interface Characterization', VCH, New York (1991).

    Google Scholar 

  3. H. D. Dewald, Electroanalysis 3 (1991) 145.

    Google Scholar 

  4. M. Froment (Ed.), `Passivity of Metals and Semiconductors', Elsevier, Amsterdam (1983).

    Google Scholar 

  5. L. R. Sharpe, W. R. Heineman and R. C. Elder, Chem. Rev. 90 (1990) 705.

    Google Scholar 

  6. Proceedings of the Symposium on X-ray Methods in Corrosion and Interfacial Electrochemistry, vol. 92-1 (edited by A. J. Davenport and J. G. Gordon, II), The Electrochemical Society, Pennington, NJ (1992).

    Google Scholar 

  7. [7] `Structure of Surfaces and Interfaces as Studied Using Synchrotron Radiation', Faraday Discussions of The Chemical Society, vol. 89, The Royal Society Of Chemistry, London (1990).

    Google Scholar 

  8. H. D. Dewald, J. W. Watkins, II, R. C. Elder and W. R. Heineman, Anal. Chem. 58 (1986) 2968.

    Google Scholar 

  9. D. A. Smith, M. J. Heeg, W. R. Heineman and R. C. Elder, J. Am. Chem. Soc. 106 (1984) 3053.

    Google Scholar 

  10. D. A. Smith, R. C. Elder and W. R. Heineman, Anal. Chem. 57 (1985) 2361.

    Google Scholar 

  11. D. H. Igo, R. C. Elder, W. R. Heineman and H. D. Dewald, Anal. Chem. 63 (1991) 2535.

    Google Scholar 

  12. D. H. Igo, R. C. Elder and W. R. Heineman, J. Electroanal. Chem. 314 (1991) 45.

    Google Scholar 

  13. R. C. Elder, C. E. Lunte, A. F. M. M. Rahman, J. R. Kirchho., H. D. Dewald and W. R. Heineman, ibid. 240 (1988) 361.

    Google Scholar 

  14. F. Villain, V. Briois, I. Castro, C. Helary and M. Verdaguer, Anal. Chem. 65 (1993) 2545.

    Google Scholar 

  15. H. Yoshitake, O. Yamazaki and K. Ota, J. Electroanal. Chem. 371 (1994) 287.

    Google Scholar 

  16. Z. Nagy, H. You, R. M. Yonco, C. A. Melendres, W. Yun and V. A. Maroni, Electrochim. Acta 36 (1991) 209.

    Google Scholar 

  17. M. E. Herron, S. E. Doyle, K. J. Roberts, J. Robinson and F. C. Walsh, Rev. Sci. Instrum. 63 (1992) 950.

    Google Scholar 

  18. M. E. Kordesch and R. W. Hoffman, Nucl. Instrum. Meth. Phys. Res. 222 (1984) 347.

    Google Scholar 

  19. T. W. Capehart, D. A. Corrigan, R. S. Conell, K. I. Pandya and R. W. Hoffman, Appl. Phys. Lett. 58 (1991) 865.

    Google Scholar 

  20. J. McBreen, W. E. O'Grady, K. I. Pandya, R. W. Hoffman and D. E. Sayers, Langmuir 3 (1987) 428.

    Google Scholar 

  21. F. A. Schultz, B. J. Feldman, S. F. Gheller, W. E. Newton, B. Hedman, P. Frank and K. O. Hodgson, in `Redox Mechanisms and Interfacial Properties of Molecules of Biological Importance', vol. 93-11 (edited by F. A. Schultz and I. Taniguchi), The Electrochemical Society, Pennington, NJ (1993) pp. 108–17.

    Google Scholar 

  22. S. Kim, I. T. Bae, M. Sandifer, P. N. Ross, R. Carr, J. Woicik, M. R. Antonio and D. A. Scherson, J. Am. Chem. Soc. 113 (1991) 9063.

    Google Scholar 

  23. D. A. Tryk, I. T. Bae, Y. Hu, S. Kim, M. R. Antonio and D. A. Scherson, J. Electrochem. Soc. 142 (1995) 824.

    Google Scholar 

  24. D. A. Tryk, I. T. Bae, D. Scherson, M. R. Antonio, G. W. Jordan and E. L. Huston, ibid. 142 (1995) L76.

    Google Scholar 

  25. D. A. Tryk, S. Kim, Y. Hu, W. Xing, D. A. Scherson, M. R. Antonio, V. Z. Leger and G. E. Blomgren, J. Phys. Chem. 99 (1995) 3732.

    Google Scholar 

  26. M. Pourbaix, `Atlas of Electrochemical Equilibria in Aqueous Solutions', 2nd edn, Cebelcor, Brussels (1974) pp. 183–97.

    Google Scholar 

  27. L. B. Anderson, D. J. Macero, J. Phys. Chem. 67 (1963) 1942.

    Google Scholar 

  28. G. Biedermann and G. S. Terjosin, Acta Chem. Scand. 23 (1969) 1896.

    Google Scholar 

  29. G. Biedermann and H. B. Silber, ibid. 27 (1973) 3761.

    Google Scholar 

  30. A. J. Bard, R. Parsons and J. Jordon, `Standard Potentials in Aqueous Solution', Marcel Dekker, New York (1985) p. 834.

    Google Scholar 

  31. [31] `SPEX Handbook of Sample Preparation and Handling', 4th edn (edited by R. H. Obenauf, R. Bostwick, M. McCann, J. D. McCormack, R. Merriman and S. Selem), SPEX Sample Preparation: Metuchen, NJ (1994) Ch. 4.

  32. M. R. Antonio, M. Dietz, M. Jensen, L. Soderholm and E. P. Horwitz, Inorg. Chim. Acta (1996) in press.

  33. M. R. Antonio, in `XAFS Workshop: SRI'94', Stony Brook, NY (1994).

    Google Scholar 

  34. F. W. Lytle, R. B. Greegor and E. C. Marques, in Proc. 9th Int. Congr. Catal. Calgary, vol. 5 (edited by M. J. Phillips and M. Ternan), The Chemical Institute of Canada: Ottawa (1988) pp. 54–85.

    Google Scholar 

  35. S. Kim, D. A. Tryk, M. R. Antonio, R. Carr and D. Scherson, J. Phys. Chem. 98 (1994) 10269.

    Google Scholar 

  36. A. J. Bard and L. R. Faulkner, `Electrochemical Methods. Fundamentals and Applications', John Wiley & Sons, New York (1980) Ch. 10.

    Google Scholar 

  37. T. Matsushita and H. Hashizume, in Handbook on Synchrotron Radiation', vol. 1A (edited by E. E. Koch), North-Holland, Amsterdam (1983) pp. 261–314.

    Google Scholar 

  38. F. W. Lytle, R. B. Greegor, D. R. Sandstrom, E. C. Marques, J. Wong, C. L. Spiro, G. P. Huffman and F. E. Huggins, Nucl. Instrum. Methods Phys. Res. 226 (1984) 542.

    Google Scholar 

  39. F. W. Lytle, in `Applications of Synchrotron Radiation', vol. 4 (edited by H. Winick, D. Xian, M. H. Ye and T. Huang), Gordon & Breach, New York (1989) pp. 135–223.

  40. M. O. Krause and J. H. Oliver, J. Phys. Chem. Ref. Data 8 (1979) 329.

    Google Scholar 

  41. F. W. Lytle, Ber. Bunsenges. Phys. Chem. 91 (1987) 1251.

    Google Scholar 

  42. M. R. Antonio and L. Soderholm, Inorg. Chem. 33 (1994) 5988.

    Google Scholar 

  43. M. R. Antonio, J. S. Xue and L. Soderholm, J. Alloys Compounds 207/208, (1994) 444.

    Google Scholar 

  44. U. Staub, M. R. Antonio, L. Soderholm, M. Guillaume, W. Henggeler and A. Furrer, Phys. Rev. B: Condensed Matter 50 (1994) 7085.

    Google Scholar 

  45. J. S. Xue, M. R. Antonio, W. T. White, L. Soderholm and S. M. Kauzlarich, J. Alloys Compounds 207/208 (1994) 161.

    Google Scholar 

  46. F. J. Berry, J. F. Marco and A. T. Steel, Hyperfine Interactions 83 (1994) 347.

    Google Scholar 

  47. G. V. Bazuev, L. D. Finkel'shtein, N. D. Samsonov and G. P. Shveikin, Russian J. Inorg. Chem. 32 (1987) 158.

    Google Scholar 

  48. D. Ravot, C. Godart, J. C. Achard and P. Lagarde, in `Valence Fluctuations in Solids' (edited by L. M. Falicov, W. Hanke and M. B. Maple), North-Holland, Amsterdam (1981) pp. 423–26.

    Google Scholar 

  49. G. Michels, S. Junk, W. Schlabitz, E. Holland-Moritz, M. M. Abd-Elmeguid, J. Dünner and A. Mewis, J. Phys.: Condensed Matter 6 (1994) 1769.

    Google Scholar 

  50. G. Wortmann, Hyperfine Interactions 47 (1989) 179.

    Google Scholar 

  51. G. Wortmann, I. Nowik, B. Perscheid, G. Kaindl and I. Felner, Phys. Rev. B: Condensed Matter 43 (1991) 5261.

    Google Scholar 

  52. Z. Tan, J. I. Budnick, W. Q. Chen, D. L. Brewe, S. W. Cheong, A. S. Cooper and L. W. Rupp, Jr., ibid. 42 (1990) 4808.

    Google Scholar 

  53. Z. Tan, J. I. Budnick, S. Luo, W. Q. Chen, S. W. Cheong, A. S. Cooper, P. C. Canfield and Z. Fisk, ibid. 44 (1991) 7008.

    Google Scholar 

  54. M. R. Antonio and L. Soderholm, J. Cluster Sci. (1996) in press.

  55. G. Meitzner, G. H. Via, F. W. Lytle and J. H. Sinfelt, J. Phys. Chem. 96 (1992) 4960.

    Google Scholar 

  56. J. Röhler, in `Handbook on the Physics and Chemistry of Rare Earths', vol. 10 (edited by K. A. Gschneidner, Jr., L. Eyring and S. Hüfner), North-Holland, Amsterdam (1987) pp. 453–545.

    Google Scholar 

  57. J. P. Lelieur, J. Goulon, R. Cortes and P. Friant, J. Phys. Chem. 88 (1984) 3720.

    Google Scholar 

  58. R. K. Singhal and K. B. Garg, J. Magn. Magn. Mater. 116 (1992) 238.

    Google Scholar 

  59. F. Lissner, K. Krämer, T. Schleid, G. Meyer, Z. Hu and G. Z. Kaindl, Anorg. Allg. Chem. 620 (1994) 444.

    Google Scholar 

  60. T. Baba, S. Hikita, R. Koide, Y. Ono, T. Hanada, T. Tanaka and S. Yoshida, J. Chem. Soc., Faraday Trans. 89 (1993) 3177.

    Google Scholar 

  61. E. J. Cho, S. J. Oh, S. Imada, S. Suga, T. Suzuki and T. Kasuya, Phys. Rev. B: Condensed Matter 51 (1995) 10146.

    Google Scholar 

  62. M. Han, S. J. Oh, J. H. Park and H. L. Park, J. Appl. Phys. 73 (1993) 4546.

    Google Scholar 

  63. W. D. Schneider, C. Laubschat, I. Nowik and G. Kaindl, Phys. Rev. B 24 (1981) 5422.

    Google Scholar 

  64. L. F. Mattheiss and R. E. Dietz, ibid. 22 (1980) 1663.

    Google Scholar 

  65. U. Fano and J. W. Cooper, Rev. Modern Phys. 40 (1968) 441.

    Google Scholar 

  66. R. D. Shannon, Acta Cryst. A32 (1976) 751.

    Google Scholar 

  67. G. H. Dieke, `Spectra and Energy Levels of Rare Earth Ions in Crystals', Interscience Publishers, New York (1968) p. 401.

    Google Scholar 

  68. S. Hufner, `Optical Spectra of Transparent Rare Earth Compounds', Academic Press, New York (1978) p. 237.

    Google Scholar 

  69. G. Wortmann, W. Krone, E. V. Sampathkumaran and G. Kaindl, Hyperfine Interactions 28 (1986) 581.

    Google Scholar 

  70. I. Song, M. R. Antonio and J. H. Payer, J. Electrochem. Soc. 142 (1995) 2219.

    Google Scholar 

  71. I. Song, D. Gervasio and J. H. Payer, J. Appl. Electrochem. (1996) in press.

  72. S. L. Amey, G. M. Michal and J. H. Payer, Metall. Mat. Trans A 25A (1994) 723.

    Google Scholar 

  73. I. Song, J. H. Payer, R. Painter and M. Marzano, Plat. Surf. Fin. 82 (1995) 66.

    Google Scholar 

Download references

Author information

Authors and Affiliations

Authors

Rights and permissions

Reprints and permissions

About this article

Cite this article

ANTONIO , M.R., SODERHOLM , L. & SONG , I. Design of spectroelectrochemical cell for in situ X-ray absorption fine structure measurements of bulk solution species. Journal of Applied Electrochemistry 27, 784–792 (1997). https://doi.org/10.1023/A:1018464526864

Download citation

  • Issue Date:

  • DOI: https://doi.org/10.1023/A:1018464526864

Keywords

Navigation