Summary
A two-step, in situ synthesis and bonding reaction of monomeric alkyl chemically bonded stationary phases is described. Silane ligands are first synthesized from the corresponding terminal olefin and dimethylhydrochlorosilane using a hexachloroplatinic acid catalyst. The platinum may then be removed if desired by adsorption to activated carbon. Bonding to silica gel is then carried out in the normal manner directly, without further purification. The resulting bonded phase is equivelant both chemically and chromatographically to phases produced in the normal manner using vacuum-distilled or otherwise purified silanes. This approach provides a simple protocol for the synthesis of novel silanes not commericially available, or of silanes not sufficiently volatile for purification by vacuum distillation.
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References
D. W. Syndorf, G. E. Marcel, J. Phys. Chem.86, 5203 (1982).
W. E. Rudzinski, T. Montgomery, paper, No. IP-40, Eighth International Symposium on Column Liquid Chromatography, May 20–25, 1984, New York, NY.
H. Engelhardt, G. Ahr, Chromatographia14, 227 (1981).
J. H. Knox, A. Pryde, J. Chromatogr.112, 171 (1975).
J. J. Kirkland, Chromatographia8, 661 (1975).
D. G. J. Kingston, B. B. Gerhart, J. Chromatogr.116, 182 (1976).
E. J. Kikta, E. Grushka, Anal. Chem.48, 1098 (1976).
C. J. Little, A. D. Dale, M. B. Evans, J. Chromatogr.153, 381 (1978).
M. C. Henion, C. Picard, M. Caude, J. Chromatogr.166, 21 (1978).
C. J. Little, D. A. Dale, M. B. Evans, Whatley, J. Chromatogr.166, 21 (1978).
H. Hemestberger, P. Behrensmeyer, J. Henning, H. Ricken, Chromatographia12, 71 (1979).
G. E. Berendsen, L. deGalan, J. Liquid Chromatogr.1, 403 (1978).
G. E. Berendsen, L. DeGalan, J. Liquid Chromatogr.1, 561 (1978).
K. K. Unger, M. Becker, P. Roumeliotis, J. Chromatogr.125, 115 (1976).
P. Roumeliotis, K. K. Unger, J. Chromatogr.149, 211 (1978).
M. Tanaka, H. Goodel, B. L. Karger, J. Chromatogr.158, 233 (1978).
G. E. Berendsen, K. A. Pikaart, L. deGalan, J. Liquid Chromatogr.3, 1437 (1980).
R. F. Meyer, R. A. Harwick, Anal. Chem.56, 2211 (1984).
S. D. Fazio, J. B. Crowther, T. V. Raglione, R. A. Hartwick, Anal. Chem., in press (1985).
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Shih-Hsien, H., Fazio, S.D., Tomellini, S.A. et al. In situ silane synthesis and bonding of monomeric stationary phases for high-performance liquid chromtography. Chromatographia 20, 161–163 (1985). https://doi.org/10.1007/BF02262705
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DOI: https://doi.org/10.1007/BF02262705