Summary
When headspace gas chromatography utilizing capillary columns is used for trace analysis, sample enrichment is often needed. This involves splitless sample injection of fairly large gas volumes and relatively long sampling times. As a result of this, the band of the sample vapor may be too large causing peak distortion and poor resolution. This problem can be easily overcome by the use of cryogenic trapping. While this can be accomplished by cooling the whole column to subambient temperature during sample introduction, a more convenient way is to utilize part of the first coil of the capillary column as a cryogenic trap.
The paper discusses the theoretical background and instrumentation of cryogenic trapping and demonstrates the possibilities through a number of examples.
Similar content being viewed by others
References
M. Kuck, 2nd Internat. Colloquium on Gas Chromatography Headspace Analysis, Ueberlingen, October 18–20, 1978; see “Applied Headspace Gas Chromatography” (B. Kolb, ed.), Heyden, London, 1980 pp. 12–22.
B. Kolb, P. Pospisil, T. Borath, M. Auer, J. High Resolut. Chromatogr./Chromatogr. Commun.2, 283 (1979).
L. S. Ettre, J. E. Purcell, J. R. Widomski, B. Kolb, P. Pospisil, J. Chromatogr. Sci.18, 116 (1980).
J. M. Raccio, J. R. Widomski. Chromatogr. Newslett.9, 42 (1981).
C. Sadowski, J. E. Purcell, Chromatogr. Newslett.9, 52 (1981).
B. Kolb, P. Pospisil, “Sample Introduction in Capillary Gas Chromatography” (P. Sandra, ed.), Huethig Verlag, Heidelberg, 1985, Vol. I, pp. 191–216.
G. Machata, Microchim. Acta (Wien)214, 262 (1964).
G. Macharata, Blutakohol4 (5), 3 (1967).
D. Jentzsch, H. Krueger, G. Lebrecht, G. Dencks, J. Gut, Z. Anal. Chem.236, 96 (1968).
G. L. McClure (Perkin-Elmer Corp., Norwalk, CT), unpublished result (1984).
W. Closta H. Klemm, P. Pospisil, R. Riegger, G. Siess, B. Kolb, Chromatogr. Newslett.11, 13 (1983).
L. S. Ettre, B. Kolb, S. G. Hurt, Amer. Lab.15 (10), 76 (1983).
W. F. Cowen, W. J. Cooper, J. W. Highfill. Anal. Chem.47, 2483 (1975).
P. C. Wylie, 190th National American Chemical Society Meeting Chicago, III. September 8–13, 1985.
J. C. Giddings. “Dynamics of Chromatography”, M. Dekker, Inc., New York, 1966, 323 pp.
L. S. Ettre, Chromatographia18, 477 (1984).
L. S. Ettre. “The Science of Chromatograph” (F. Bruner, ed.). Elsevier, Amsterdam, 1985; pp. 87–109.
L. S. Ettre, J. High Resolut. Chromatogr./Chromatogr. Commun.8, 497 (1985).
B. Kolb, Chromatographia15, 587 (1982).
B. Kolb, P. Pospisil, M. Auer. Chromatographia19, 13 (1984).
L. S. Ettre, E. Jones, B. S. Todd, Chromatogr. Newslett.12, 1 (1984).
R. C. M. de Nijs, J. de Zeeuw. Chrompack News10, (2), 1 (1983); J. Chromatogr.279, 41 (1983).
Author information
Authors and Affiliations
Additional information
Enlarged text of a paper presented at the 37th Pittsburgh Conference on Analytical Chemistry and Applied Spectroscopy, Atlantic City, NJ, March 10–14, 1986.
Rights and permissions
About this article
Cite this article
Kolb, B., Liebhardt, B. & Ettre, L.S. Cryofocusing in the combination of gas chromatography with equilibrium headspace sampling. Chromatographia 21, 305–311 (1986). https://doi.org/10.1007/BF02311600
Received:
Accepted:
Issue Date:
DOI: https://doi.org/10.1007/BF02311600