Use of hydrolyzed chlorosilanes for the preparation of high resolution glass capillary columns
- 45 Downloads
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.
KeywordsHydrolysis Steroid Stationary Phase Dynamic Method Alkaline Hydrolysis
Unable to display preview. Download preview PDF.
- J. J. Kirkland, Gas chromatography 1963.L. Fowler Ed., Instrument Society of America, Pittsburg P.A., p. 77.Google Scholar
- C. Rossi, S. Munari, C. Cengarle, G. F. Tealdo, Chim. Ind. Milan42, 724 (1966).Google Scholar
- J. J. Kirkland, P. C. Yates, U.S. Patent no 3.722.181 (1973).Google Scholar
- J. J. De Stefano, J. J. Kirkland, J. Chromatog. Sci.12, 337 (1974).Google Scholar
- C. J. Bossart U.S. Patent no 3.514.925 (1970).Google Scholar
- G. Alexander, G. A. F. M. Rutten, J. Chromatog.99 81 (1974).Google Scholar
- A. Ros, J. Gas. Chromatog.,3, 252 (1965).Google Scholar
- E. M. Chambaz, C. Madani, A. J. Hadjian, inS. G. Perry Ed., Chromatography 72 vol. 1, Bartholomew Press, Dorbing 1973, p. 89Google Scholar
- M. H. J. Van Rijswick, K. Tesarik, Chromatographia7, 135 (1974).Google Scholar