In situ propylation using sodium tetrapropylborate as a fast and simplified sample preparation for the speciation analysis of organolead compounds using GC-MIP-AES

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Monika Heisterkamp and Freddy C. Adams


Abstract

A fast and simple sample preparation procedure for the speciation of organolead compounds is described. Separation and detection of the different species was carried out using gas chromatography hyphenated to microwave-induced plasma atomic emission spectrometry. Derivatization was performed using in situ propylation with sodium tetrapropylborate in an acetic acid-sodium acetate buffer medium of pH 4.5 with simultaneous extraction of the propylated species into hexane. Detection limits (as Pb) ranging from 77 fg (0.15 ng kg–1) to 102 fg (0.21 ng kg–1) and relative standard deviations between 4 and 6% were achieved. Accuracy of the procedure was confirmed by analysis of a certified reference material (CRM 605, Road Dust), where the desorption of the different species from the matrix by acid leaching was also integrated in the derivatization and extraction step. The optimized sample preparation procedure was applied to the analysis of alpine snow sampled at the Mont-Blanc in France.


References

  1. C. N. Hewitt and R. M. Harrison, in Organometallic Compounds in the Environment, ed. P. J. Craig, Longman, Harlow, 1986, pp. 160–179 Search PubMed.
  2. R. Łobiński, Analyst, 1995, 120, 615 RSC.
  3. F. C. Adams, M. Heisterkamp, J. P. Candelone, F. Laturnus, K. van de Velde and C. F. Boutron, Analyst, 1998, 123, 767 RSC.
  4. W. M. R. Dirckx, M. B. de la Calle, M. Ceulemans and F. C. Adams, J. Chromatogr. A, 1994, 683, 51 CrossRef CAS.
  5. A. M. Naghmush, K. Pyrzynska and M. Trojanowicz, Talanta, 1995, 42, 851 CrossRef CAS.
  6. K. Bergmann and B. Neidhard, Fresenius' J. Anal. Chem., 1996, 356, 57 CrossRef CAS.
  7. L. Ebdon, S. Hill and R. W. Ward, Analyst, 1987, 112, 1 RSC.
  8. P. Uden, J. Chromatogr. A, 1995, 703, 393 CrossRef CAS.
  9. G. Lespes, M. Pontin-Goutier and A. Astruc, Environ. Sci. Technol., 1992, 13, 207 CAS.
  10. M. Paneli, E. Rosenberg, M. Grasserbauer, M. Ceulemans and F. C. Adams, Fresenius' J. Anal. Chem., 1997, 357, 756 CrossRef.
  11. R. Łobiński and F. C. Adams, J. Anal. At. Spectrom., 1992, 7, 987 RSC.
  12. I. A. Pereiro and R. Lobiński, J. Anal. At. Spectrom., 1997, 12, 1381 RSC.
  13. T. De Smaele, L. Moens, R. Dams and P. Sandra, Fresenius' J. Anal. Chem., 1996, 354, 778.
  14. M. Heisterkamp, T. De Smaele, J. P. Candelone, L. Moens, R. Dams and F. C. Adams, J. Anal. At. Spectrom., 1997, 12, 1077 RSC.
  15. L. Ebdon, S. J. Hill and C. Rivas, Spectrochim. Acta, Part B, 1998, 53, 289 CrossRef.
  16. A. Prange and E. Jantzen, J. Anal. At. Spectrom., 1995, 10, 105 RSC.
  17. R. Łobiński and F. C. Adams, Anal. Chim. Acta, 1992, 262, 285 CrossRef CAS.
  18. Y. Wang, A. B. Turnbull and R. M. Harrison, Appl. Organomet. Chem., 1997, 11, 889 CrossRef CAS.
  19. B. Pons, A. Carrera and C. Nerín, J. Chromatogr. B, 1998, 716, 139 CrossRef CAS.
  20. M. A. R. Abdel-Moati, Environ. Pollut., 1996, 91, 97 CrossRef CAS.
  21. V. Minganti, R. Capelli and R. De Pelligrini, Fresenius' J. Anal. Chem., 1995, 351, 471 CrossRef CAS.
  22. D. S. Forsyth and W. D. Marshall, Anal. Chem., 1983, 55, 2132 CrossRef CAS.
  23. C. Witte, J. zpunar-Lobinska, R. Łobiński and F. C. Adams, Appl. Organomet. Chem., 1994, 8, 621 CAS.
  24. A. Wasik, I. R. Pereiro and R. Łobiński, Spectrochim. Acta, Part B, 1998, 53, 867 CrossRef.
  25. M. Ceulemans and F. C. Adams, J. Anal. At. Spectrom., 1996, 11, 201 RSC.
  26. M. Heisterkamp and F. C. Adams, Fresenius' J. Anal. Chem., 1998, 362, 489 CrossRef CAS.
  27. K. Bergmann and B. Neidhart, Fresenius' J. Anal. Chem., 1996, 356, 57 CrossRef CAS.
  28. T. De Smaele, L. Moens, R. Dams, P. Sandra, J. Van der Eycken and J. Vandyck, J. Chromatogr. A, 1998, 793, 99 CrossRef.
  29. S. Hancock and A. Slater, Analyst, 1975, 100, 422 RSC.
  30. J. J. Sullivan and B. D. Quimby, Anal. Chem., 1990, 62, 1034 CrossRef CAS.
  31. C. Vincent, M. Vallon, F. Pinglot, M. Funk and L. Reynaud, J. Glaciol., 1997, 43, 513 Search PubMed.