Skip to main content
SpringerLink
Log in

Determination of lead in geological and biological materials by graphite furnace atomic absorption spectrometry

Bestimmung von Blei in geologischen und biologischen Materialien durch AAS mit der Graphitrohrküvette

  • Original Papers
  • Published:
Fresenius' Zeitschrift für analytische Chemie Aims and scope Submit manuscript

Zusammenfassung

Schwerwiegende systematische Fehler bei der Bestimmung von Blei in geologischen und biologischen Materialien mit der Graphitrohrküvette werden aufgezeigt. Die Reaktion von Blei mit Alkali-, Erdalkali- und Eisenchloriden während der Atomisierungsphase führt zur Bildung von Bleimonochlorid, das nur unvollständig dissoziiert und eine Signalunterdrückung zur Folge hat. Ein Zusatz von 20% Wasserstoff zu Stickstoff als Spülgas vermindert die Signalunterdrückung, indem überschüssiges Chlor als Chlorwasserstoff entfernt wird. Die Nachweisgrenze liegt bei ca. 0,6 ppm für Gesteine und bei ca. 0,3 ppm für Pflanzenmaterialien. Je nach der Konzentration beträgt die relative Standardabweichung 1–12%. Die Genauigkeit der Methode wurde an 39 internationalen Standardreferenzproben überprüft.

Summary

Serious systematic errors inherent in the determination of lead in geological and biological samples by flameless atomic-absorption spectrometry are demonstrated. The reduced absorption of lead is due to partial interaction with alkaline, alkaline-earth and iron chlorides during the atomization stage. Incomplete dissociation of the volatile monochloride of lead in the gaseous phase reduces the absorption signal. An addition of 20% hydrogen to nitrogen (purge gas) diminishes signal suppression by removing the chlorine in form of volatile HCl. The detection limit is about 0.6 ppm in rocks and about 0.3 ppm in plant materials. Depending on the content in the samples the relative standard deviation is between 1 and 12%. The accuracy of the method was tested on 39 international standard reference samples.

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

Access this article

Log in via an institution

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

Instant access to the full article PDF.

Institutional subscriptions

References

  1. Aggett, J., Sprott, A. J.: Anal. Chim. Acta 72, 49 (1974)

    Google Scholar 

  2. Alger, D., Anderson, R. G., Maines, I. S., West, T. S.: Anal. Chim. Acta 57, 271 (1971)

    Google Scholar 

  3. Ando, A., Kurasawa, H., Ohmori, T., Takeda, E.: Geochem. J. 8, 175 (1974)

    Google Scholar 

  4. Barnard, W. M., Fishman, M. J.: At. Absorpt. Newsletters 12, 118 (1973)

    Google Scholar 

  5. Bowen, H. J. M.: Trace elements in biochemistry. London, New York: Acad. Press 1966

    Google Scholar 

  6. Campbell, W. C., Ottaway, J. M.: Talanta 21, 837 (1974)

    Google Scholar 

  7. Campbell, W. C., Ottaway, J. M.: Talanta 22, 729 (1975)

    Google Scholar 

  8. Catalog of N.B.S. standard reference materials, U.S. Department of Commerce (1975)

  9. Cottrell, T. L.: The Strength of Chemical Bonds. London: Butterworths Sci. Publ. 1958

    Google Scholar 

  10. Cruz, R. B., Van Loon, J. C.: Anal. Chim. Acta 72, 231 (1974)

    Google Scholar 

  11. Currie, L. A.: Anal. Chem. 40, 586 (1968)

    Google Scholar 

  12. Dolinšek, F., Stupar, J.: Analyst 98, 841 (1973)

    Google Scholar 

  13. Duval, C.: Inorganic Thermogravimetric Analysis. New York: Elsevier 1963

    Google Scholar 

  14. Ediger, R. D.: At. Absorpt. Newsletters 14, 127 (1975)

    Google Scholar 

  15. Fernandez, F. J., Manning, D. C.: At. Absorpt. Newsletters 10, 65 (1971)

    Google Scholar 

  16. Flanagan, F. J.: Geochim. Cosmochim. Acta 37, 1189 (1973)

    Google Scholar 

  17. Flanagan, F. J.: U.S. Geol. Surv. Prof. Pap. 840, 171 (1976)

    Google Scholar 

  18. Frech, W.: Anal. Chim. Acta 77, 43 (1975)

    Google Scholar 

  19. Frech, W., Cedergen, A.: Anal. Chim. Acta 82, 83 (1976)

    Google Scholar 

  20. Frech, W., Cedergren, A.: Anal. Chim. Acta 82, 93 (1976)

    Google Scholar 

  21. Fuller, C. W.: Anal. Chim. Acta 81, 199 (1976)

    Google Scholar 

  22. Garnys, V. P., Smythe, L. E.: Talanta 22, 881 (1975)

    Google Scholar 

  23. Govindaraju, K., Mevelle, G., Chouard, C.: Anal. Chem. 46, 1672 (1974)

    Google Scholar 

  24. Huber-Schausberger, I., Janda, I., Dolezel, P., Schroll, E.: Tschermaks Miner. Petrogr. Mitt. 14, 195 (1970)

    Google Scholar 

  25. Kaiser, H., Specker, H.: Fresenius Z. Anal. Chem. 149, 46 (1956)

    Google Scholar 

  26. Katz, A.: Chem. Geol. 16, 15 (1975)

    Google Scholar 

  27. Katz, A., Taitel, N.: Talanta 24, 132 (1977)

    Google Scholar 

  28. Koch, O. G., Koch-Dedic, G. A.: Handbuch der Spurenanalyse. Berlin, Heidelberg, New York: Springer 1974

    Google Scholar 

  29. Kondratiev, V. N.: Chemical Bond Energy, Ionization Potentials. Moscow: Nauka 1974

    Google Scholar 

  30. Langmyhr, F. J., Stuberg, J. R., Thomassen, Y., Hanssen, J. E., Doležal, J.: Anal. Chim. Acta 71, 35 (1974)

    Google Scholar 

  31. Littlejohn, D., Ottaway, J. M.: Analyst 103, 595 (1978)

    Google Scholar 

  32. Luecke, W., Eschermann, F., Lennartz, U., Papastamataki, A. J.: N. Jb. Mineral. Abh. 120, 178 (1974)

    Google Scholar 

  33. L'vov, B. V.: Spectrochim. Acta 33B, 153 (1978)

    Google Scholar 

  34. L'vov, B. L., Pelieva, L. A., Sharnopolsky, A. J.: Ž. Prikl. Spectrosk. 27, 395 (1977)

    Google Scholar 

  35. Massmann, H., Gücer, S.: Spectrochim. Acta 29B, 283 (1974)

    Google Scholar 

  36. Oelschläger, W., Lautenschläger, W.: Fresenius Z. Anal. Chem. 287, 28 (1977)

    Google Scholar 

  37. Regan, J. G. T., Warren, J.: Analyst 101, 220 (1976)

    Google Scholar 

  38. Rüdorff, W.: Graphite Intercallation Compounds, Advances in Inorganic Chemistry and Radiochemistry, edited by H. J. Eméleus and A. G. Sharpe. New York: Acad. Press 1959

    Google Scholar 

  39. Rüdorff, W., Stumpp, E., Spriessler, W., Siecke, F. W.: Angew. Chem. 75, 130 (1963)

    Google Scholar 

  40. Steele, T. W., Wilson, A., Goudvis, R., Ellis, P. J., Radford, A. J.: Analyses of the NIMROC reference samples for minor and trace elements, report No. 1945 (1978)

  41. Sturgeon, R. E., Chakrabarti, C. L.: Anal. Chem. 48, 1792 (1976)

    Google Scholar 

  42. Sturgeon, R. E., Chakrabarti, C. L.: Spectrochim. Acta 32B, 231 (1977)

    Google Scholar 

  43. Venghiattis, A. A., Whitlock, L.: At. Absorpt. Newsletters 6, 135 (1967)

    Google Scholar 

  44. Wegschneider, W., Knapp, G., Spitzy, H.: Fresenius Z. Anal. Chem. 283, 183 (1977)

    Google Scholar 

Download references

Author information

Authors and Affiliations

  1. Geochem. Institut der Universität, Goldschmidtstr. 1, D-3400, Göttingen

    H. Heinrichs

Authors
  1. H. Heinrichs
    View author publications

    You can also search for this author in PubMed Google Scholar

Rights and permissions

Reprints and permissions

About this article

Cite this article

Heinrichs, H. Determination of lead in geological and biological materials by graphite furnace atomic absorption spectrometry. Z. Anal. Chem. 295, 355–361 (1979). https://doi.org/10.1007/BF00539703

Download citation

  • Received:

  • Issue Date:

  • DOI: https://doi.org/10.1007/BF00539703

Key words

Search

Navigation