Advertisement

Chromatographia

, Volume 56, Issue 11–12, pp 733–738 | Cite as

Speciation of mercury compounds by gas chromatography with atomic emission detection. Simultaneous optimization of a headspace solid-phase microextraction and derivatization procedure by use of chemometric techniques

  • A. M. Carro
  • I. Neira
  • R. Rodil
  • R. A. Lorenzo
Originals Gas Chromatography

Summary

A method is proposed for the extraction and determination of organomercury compounds and Hg(II) in seawater samples by headspace solid-phase microextraction (HS-SPME) combined with capillary gas chromatography-microwave-induced plasma atomic emission spectrometry. The mercury species were derivatized with sodium tetraphenylborate, sorbed on a polydimethylsiloxane-coated fused-silica fibre, and desorbed in the injection port of the GC, in splitless mode.

Experimental design methodology was used to evaluate the effect of six HS-SPME-derivatization vairables: sample, volume, NaBPh4 volume, pH, sorption time, extraction-derivatization temperature, and rate of stirring. Use of a multicriterion decision-making approach, with the desirability function, enabled determination of the optimum working conditions of the procedure for simultaneous analysis of three mercury species.

Key Words

Gas chromatography Headspace Solid phase microextraction Speciation Seawater Mercury 

Preview

Unable to display preview. Download preview PDF.

Unable to display preview. Download preview PDF.

References

  1. [1]
    Harrington, C.F.Trends Anal. Chem. 2000,19, 167–179CrossRefGoogle Scholar
  2. [2]
    Adams, F.; Slaets, S.Trends Anal. Chem. 2000,19, 80–85.CrossRefGoogle Scholar
  3. [3]
    Gustin, M.S.; Lindberg, S.E.Fresenius J. Anal. Chem. 2000,366, 417–422.CrossRefGoogle Scholar
  4. [4]
    Logar, M.; Horvat, M.; Falnoga I.; Stibilj, V.Fresenius J. Anal. Chem. 2000,366, 453–460.CrossRefGoogle Scholar
  5. [5]
    Hempel, M.; Kuballa, J.; Jantzen, E.Fresenius J. Anal. Chem. 2000,366, 470–475.CrossRefGoogle Scholar
  6. [6]
    Carro, A.M.; Lorenzo, R.A.; Cela, R.LC-GC Int. 1998,16, 926–936.Google Scholar
  7. [7]
    Hight, S.C.; Capar, S.G.J. Assoc. Off. Anal. Chem. 1983,66, 1121–1128.Google Scholar
  8. [8]
    Hight, S.C.; Corcoran, M.T.J. Assoc. Off. Anal. Chem. 1987,70, 24–30.Google Scholar
  9. [9]
    Carro-Díaz, A.M.; Lorenzo-Ferreira, R.A.; Cela-Torrijos, R.J. Chromatogr. 1994,683, 245–252.CrossRefGoogle Scholar
  10. [10]
    Lobinski, R.Appl. Spectrosc. 1997,51, 260A-278A.CrossRefGoogle Scholar
  11. [11]
    Quevauviller, P.J. Chromatogr. A 1996,750, 25–33.CrossRefGoogle Scholar
  12. [12]
    Orellana Velado, N.G.; Pereiro, R.; Sanz-Medel, A.J. Anal. At. Spectrom. 2000,15, 49–53.CrossRefGoogle Scholar
  13. [13]
    Cai, Y.; Monsalud, S.; Furton, K.G.Chromatographia 2000,52, 82–86.CrossRefGoogle Scholar
  14. [14]
    Arthur, C.L.; Pawliszyn, J.Anal. Chem. 1990,62, 2145–2148.CrossRefGoogle Scholar
  15. [15]
    Pawliszyn, J.Solid-Phase Microextraction: Theory and Practice, Wiley-VCH, New York,1997.Google Scholar
  16. [16]
    Bayona, J.M.Organometallic Speciation by Combining Aqueous Phase Derivatization with SPME-GC-FPD-MS, inApplications of Solid Phase Microextraction, Pawliszyn, J. Ed., RSC Chromatography Monographs, Cambridge,1999, p. 284.Google Scholar
  17. [17]
    Cai, Y.; Bayona, J.J. Chromatogr. A 1995,696, 113–122.CrossRefGoogle Scholar
  18. [18]
    Mester, Z.; Lam, J.; Sturgeon, R.; Pawliszyn, J.J. Anal. At. Spectrom. 2000,15, 837–842.CrossRefGoogle Scholar
  19. [19]
    De Smaele, T.; Moens, L.; Sandra, P.; Dams, R.Microchim. Acta 1999,130, 241–251.CrossRefGoogle Scholar
  20. [20]
    Mothes, S.; Wennrich, R.J. High Resol. Chromatogr. 1999,22, 181–182.CrossRefGoogle Scholar
  21. [21]
    Moens, L.; De Smaele, T.; Dams, R.; Van Der Broeck, P.; Sandra, P.Anal. Chem. 1997,69, 1604–1611.CrossRefGoogle Scholar
  22. [22]
    He, B.; Jiang, G.B.; Ni, Z.J. Anal. At. Spectrom. 1998,13, 1141–1144.CrossRefGoogle Scholar
  23. [23]
    He, B.; Jiang, G.B.Fresenius, J. Anal. Chem. 1999,365, 615–618.CrossRefGoogle Scholar
  24. [24]
    Beichert, A.; Padberg, S.; Wenclawiak, B.W.Appl. Organomet. Chem. 2000,14, 493–498.CrossRefGoogle Scholar
  25. [25]
    Dunemann, L.; Hajimiragha, H.; Begerow, J.Fresenius J. Anal. Chem. 1999,363, 466–468.CrossRefGoogle Scholar
  26. [26]
    Cai, Y.; Monsalud, S.; Furton, K.G.; Jaffé, R.; Jones, R.D.Appl. Organomet. Chem. 1998,12, 55–569.Google Scholar
  27. [27]
    O'Reilly, J.E.J. Chromatogr. A 1982,238, 443–444.CrossRefGoogle Scholar
  28. [28]
    Abuín, M.; Carro, A.M.; Lorenzo R.A.J. Chromatogr. A 2000,889, 185–193.CrossRefGoogle Scholar
  29. [29]
    Lewis, G.A.; Mathieu, D.; Phan-Tan-Liu, R.Pharmaceutical Experimental Design, Drugs and the Pharmaceutical Sciences, Vol. 92, Marcel Dekker, New York,1999 pp. 247–293.Google Scholar
  30. [30]
    Pawliszyn, J.Application of Solid-Phase Microextraction, RSC Chromatography Monographs, RSC, Cambridge,1999.Google Scholar
  31. [31]
    Millan, E.; Pawliszyn, J.J Chromatogr. 2000,873, 63–71.CrossRefGoogle Scholar
  32. [32]
    Lespes, G.; Desauziers, V.; Montigny, C.; Potin-Gautier, M.J. Chromatogr. A 1998,826, 67–76.CrossRefGoogle Scholar
  33. [33]
    Weber, J.H.Trends Anal. Chem. 1997,16, 73–78.CrossRefGoogle Scholar
  34. [34]
    Minganti, V.; Capelli, R.; de Pellegrini, R.Fresenius J. Anal. Chem. 1995,351, 471–477.CrossRefGoogle Scholar
  35. [35]
    Hu, G.L.; Wang, X.R.; Wang, Y.R.; Chem, X.; Jia, L.Anal. Lett. 1997,30, 2579–2594.Google Scholar
  36. [36]
    Cai, Y.; Bayona, J.M.J. Chromator. Sci. 1995,33, 89–97.Google Scholar
  37. [37]
    Szpunar, J.; Schmitt V.O.; Lobinski, R.; Monod, J.L.J. Anal. Atom. Spectrom. 1996,11, 193–199.CrossRefGoogle Scholar
  38. [38]
    Carro, A.M.; Neira, I.; Lorenzo, R.A.; Cela, R.7th Int. Conf. Chemometrics in Analytical Chemistry, Antwerp, Belgium, October 16–20,2000.Google Scholar
  39. [39]
    González, A.G.Anal. Chim. Acta 1998,360, 227–241.CrossRefGoogle Scholar
  40. [40]
    Statgraphics Plus Version 6.0, Reference Manual, Manugistics, Rockville, MD,1992.Google Scholar
  41. [41]
    Nemrod for Windows Version 2000, LPRAI, University of Marseille III, Marseille.Google Scholar
  42. [42]
    Harrington, E.C.Ind. Qual. Control 1965,21, 494–498.Google Scholar
  43. [43]
    Derringer G.; Suich, R.J. Qual. Technol. 1980,12, 214–219.Google Scholar
  44. [44]
    Miller, J.N.; Miller, J.C.Statistics and Chemometrics for Analytical Chemistry, 4th edn, Prentice Hall-Pearson Education, Harlow, UK,2000, pp. 107–150.Google Scholar
  45. [45]
    Prosen, H.; Zupancic-Kralj, L.Trends Anal. Chem. 1999,18, 272–282.CrossRefGoogle Scholar

Copyright information

© Friedr. Vieweg & Sohn Verlagsgesellschaft mbH 2002

Authors and Affiliations

  • A. M. Carro
    • 1
  • I. Neira
    • 1
  • R. Rodil
    • 1
  • R. A. Lorenzo
    • 1
  1. 1.Dpto. Química Analítica Nutrición y Bromatología, Fac. QuímicaUniv. Santiago de CompostelaSantiago de CompostelaSpain

Personalised recommendations