On-line mass spectrometry system for measurements at single-crystal electrodes in hanging meniscus configuration


We present the construction and some first applications of an On-line electrochemical mass spectrometry system for detecting volatile products formed during electrochemical reactions at a single-crystal electrode in hanging meniscus configuration. The system is based on a small inlet tip made of porous Teflon and a Peek holder, which is brought in close proximity (ca. 10–20 μm) to the electrode surface. The tip is connected to the mass spectrometer by glass and metal tubing. Because of the small amount of gas entering the mass spectrometer, no differential pumping is needed during the measurement. The tip construction and preparation introduced here leads to reproducible voltammetry with very good cleanliness characteristics. The presence of the tip has no significant influence on the blank voltammetry of a Pt(111) in sulfuric acid, and on voltammetric responses for CO adlayer oxidation, methanol oxidation, and hydroxylamine electrochemistry on Pt(111). The formation of gaseous products in these reactions can be followed accurately and is in good agreement with earlier results obtained by other mass spectrometric or spectroscopic techniques. The time response and tailing of the setup is on the order of seconds and mainly determined by the distance between the tip and the electrode.

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  1. 1.

    Bruckenstein R.R., Gadde J., (1971) J. Am. Chem. Soc. 93: 793

    CAS  Article  Google Scholar 

  2. 2.

    Wolter O., Heitbaum J., (1984) Ber. Bunsenges. Phys. Chem. 88: 2

    CAS  Google Scholar 

  3. 3.

    Wolter O., Heitbaum J., (1984) Ber. Bunsenges. Phys. Chem. 88: 6

    CAS  Google Scholar 

  4. 4.

    Willsau J., Heitbaum J., (1986) Electrochim. Acta 31: 1443

    Article  Google Scholar 

  5. 5.

    Bittins-Cattaneo B., Cattaneo E., Königshoven P., Vielstich W., (1991) In: Bard A.J. (eds) Electronanalytical Chemistry Vol 17. Marcel Dekker, New York, pp. 181

    Google Scholar 

  6. 6.

    Baltruschat H., (1999) In: Wieckowski A. (eds) Interfacial Electrochemistry, Theory, Principles, and Applications. Marcel Dekker, New York, pp. 577

    Google Scholar 

  7. 7.

    Baltruschat H., (2004) J. Am. Soc. Mass Spectrom. 15:1693

    CAS  Article  Google Scholar 

  8. 8.

    Baltruschat H., Schmiemann U., (1993) Ber. Bunsenges. Phys. Chem. 97:452

    CAS  Google Scholar 

  9. 9.

    Hartung T., Baltruschat H., (1990) Langmuir 6: 953

    CAS  Article  Google Scholar 

  10. 10.

    Jusys Z., Massong H., Baltruschat H., (1999) J. Electrochem. Soc. 146:1093

    CAS  Article  Google Scholar 

  11. 11.

    Smith S.P.E., Casado-Rivera E., Abruña H., (2003) J. Solid State Electrochem. 7: 582

    CAS  Article  Google Scholar 

  12. 12.

    Gao Y., Tsuji H., Hattori H., Kita H., (1994) J. Electroanal. Chem. 372: 372

    Article  Google Scholar 

  13. 13.

    Jambunathan K., Hillier A., (2003) J. Electrochem. Soc. 150: E312

    CAS  Article  Google Scholar 

  14. 14.

    Jambunathan K., Jayaraman S., Hillier A., (2004) Langmuir 20: 1856

    CAS  Article  Google Scholar 

  15. 15.

    de Groot M.T., Merkx M., Wonders A.H., Koper M.T.M., (2005) J. Am. Chem. Soc. 127: 7579

    Article  Google Scholar 

  16. 16.

    Lebedeva N.P., Koper M.T.M., Herrero E., Feliu J.M., van Santen R.A., (2000) J. Electroanal. Chem. 487:37

    CAS  Article  Google Scholar 

  17. 17.

    Clavilier J., El Achi K., Petit M., Rodes A., Zamakhchari M.A., (1990) J. Electroanal. Chem. 295:333

    CAS  Article  Google Scholar 

  18. 18.

    Parsons R., VanderNoot T., (1988) J. Electroanal. Chem. 257: 9

    CAS  Article  Google Scholar 

  19. 19.

    T.H.M. Housmans, A.H. Wonders and M.T.M. Koper (2006) J. Phys. Chem. B (in press)

  20. 20.

    Wang H., Loffler T., Baltruschat H., (2001) J. Appl. Electrochem. 31:759

    CAS  Article  Google Scholar 

  21. 21.

    Rosca V., Beltramo G.L., Koper M.T.M., (2004) J. Electroanal. Chem. 566: 53

    CAS  Article  Google Scholar 

  22. 22.

    Rosca V., Beltramo G.L., Koper M.T.M., (2004) J. Phys. Chem. B 108:8294

    CAS  Article  Google Scholar 

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This work was partially supported by the Netherlands Organization for Scientific Research (NWO).

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Correspondence to M.T.M. Koper.

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Wonders, A., Housmans, T., Rosca, V. et al. On-line mass spectrometry system for measurements at single-crystal electrodes in hanging meniscus configuration. J Appl Electrochem 36, 1215–1221 (2006). https://doi.org/10.1007/s10800-006-9173-4

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  • on-line mass spectrometry
  • electrocatalysis
  • single-crystal electrodes
  • hanging meniscus