Chromatographia

, Volume 10, Issue 8, pp 466–472 | Cite as

Use of hydrolyzed chlorosilanes for the preparation of high resolution glass capillary columns

  • C. Madani
  • E. M. Chambaz
  • M. Rigaud
  • P. Chebroux
  • J. C. Breton
  • F. Berthou
Article

Summary

A new procedure for the preparation of high resolution open tubular glass capillary columns is described. This procedure involves the preparation of polysiloxane polymers obtained by alkaline hydrolysis of alkyl chlorosilane. The mixture of polysiloxane polymers is then coated on the wall of previously HCl treated glass capillary columns using a dynamic method. A base-catalysed reaction using gaseous ammonia, applied to the coated polymers leads to a stable chemically bonded stationary phase, with non-polar characteristics. This type of column is easier to prepare than conventional ones and exhibits excellent chromatographic properties, both with regard to their resolution, stability and reproducibility. The flexibility of this method permits the use of other types of commercially available chlorosilanes (i.e. methylphenyl chlorosilane) to prepare polar polysiloxane polymers suitable for analysis of complex biochemical mixtures, such as steroid metabolites.

Keywords

Hydrolysis Steroid Stationary Phase Dynamic Method Alkaline Hydrolysis 

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References

  1. [1]
    I. Halasz, I. Sebastian, Angew. Chem. Intern. Ed. Engl.8, 453 (1969).CrossRefGoogle Scholar
  2. [2]
    J. J. Kirkland, Gas chromatography 1963.L. Fowler Ed., Instrument Society of America, Pittsburg P.A., p. 77.Google Scholar
  3. [3]
    C. Rossi, S. Munari, C. Cengarle, G. F. Tealdo, Chim. Ind. Milan42, 724 (1966).Google Scholar
  4. [4]
    E. W. Abel, Z. H. Pollard, P. C. Uden, G. Nickless, J. Chromatog.22, 23 (1966).CrossRefGoogle Scholar
  5. [5]
    W. A. Aue, C. R. Hastings, J. Chromatog.42, 319 (1969).CrossRefGoogle Scholar
  6. [6]
    J. J. Kirkland, P. C. Yates, U.S. Patent no 3.722.181 (1973).Google Scholar
  7. [7]
    J. J. De Stefano, J. J. Kirkland, J. Chromatog. Sci.12, 337 (1974).Google Scholar
  8. [8]
    C. J. Bossart U.S. Patent no 3.514.925 (1970).Google Scholar
  9. [9]
    C. Madani, E. M. Chambaz, M. Rigaud, J. Durand, P. Chebroux, J. Chromatog.126, 161 (1976).CrossRefGoogle Scholar
  10. [10]
    M. Rigaud, P. Chebroux J. Durand, J. Maclouf, C. Madani, Tetrahedron Letters44, 3935 (1976).CrossRefGoogle Scholar
  11. [11]
    G. Alexander, G. A. F. M. Rutten, J. Chromatog.99 81 (1974).Google Scholar
  12. [12]
    A. Ros, J. Gas. Chromatog.,3, 252 (1965).Google Scholar
  13. [13]
    E. M. Chambaz, C. Madani, A. J. Hadjian, inS. G. Perry Ed., Chromatography 72 vol. 1, Bartholomew Press, Dorbing 1973, p. 89Google Scholar
  14. [14]
    J. J. Franken, G. A. F. M. Rutten, J. A. Rijks, J. Chromatog.126, 117 (1976).CrossRefGoogle Scholar
  15. [15]
    J. L. Marshall, D. A. Parker, J. Chromatog.122, 425 (1976).CrossRefGoogle Scholar
  16. [16]
    M. H. J. Van Rijswick, K. Tesarik, Chromatographia7, 135 (1974).Google Scholar
  17. [17]
    W. Patenode, D. F. Willock, J. Amer. Chem. Soc.68, 358 (1946).CrossRefGoogle Scholar
  18. [18]
    P. A. Digiorgio, L. H. Sommer, F. C.Whitmore, J. Amer. Chem. Soc.68, 344 (1946).CrossRefGoogle Scholar

Copyright information

© Friedr. Vieweg & Sohn, Verlagsgesellschaft mbH 1977

Authors and Affiliations

  • C. Madani
    • 1
  • E. M. Chambaz
    • 1
  • M. Rigaud
    • 2
  • P. Chebroux
    • 2
  • J. C. Breton
    • 2
  • F. Berthou
    • 3
  1. 1.Laboratoire d'HormonologieCHU de GrenobleLa TroncheFrance
  2. 2.BiochimieCHU DupuytrenLimogesFrance
  3. 3.BiochimieFaculté de MédecineBrestFrance

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