Silicon-29 and carbon-13 NMR characterization of mixed horizontally polymerized monolayers on silica gel

作者: Hafeez O. Fatunmbi , Martha D. Bruch , Mary J. Wirth

DOI: 10.1021/AC00063A020

关键词:

摘要: A horizontally polymerized monolayer of mixed C[sub 18] and 3] trifunctional silanes on silica, conventional chromatographic phases, are studied by NMR spectroscopy. For horizontal polymerization, quantitative [sup 13]C 29]Si measurements reveal that a dense highly bonded groups is formed the surface. The polymeric surface, contrast, oligomeric in nature: ratio to reacted substrate silanols only slightly more than 1:1, average oligomer size 5 units. data insignificant vertical polymerization. show chain dynamics for similar those monomeric monolayer, whereas phase significantly slower. These results indicate chains randomly interspersed with short phase. 31 refs., figs., 4 tabs.

参考文章(15)
I Ssuer Chuang, David R. Kinney, Charles E. Bronnimann, Robert C. Zeigler, Gary E. Maciel, Effects of proton-proton spin exchange in the silicon-29 CP-MAS NMR spectra of the silica surface The Journal of Physical Chemistry. ,vol. 96, pp. 4027- 4034 ,(1992) , 10.1021/J100189A022
H.A. Claessens, J.W. De Haan, L.J.M. Van De Ven, P.C. De Bruyn, C.A. Cramers, Chromatographic and solid state nuclear magnetic resonance study of the changes in reversed-phase packings for high-performance liquid chromatography at different eluent compositions Journal of Chromatography A. ,vol. 436, pp. 345- 365 ,(1988) , 10.1016/S0021-9673(00)94595-3
Mary J. Wirth, Hafeez O. Fatunmbi, Horizontal polymerization of mixed trifunctional silanes on silica. 2. Application to chromatographic silica gel Analytical Chemistry. ,vol. 65, pp. 822- 826 ,(1993) , 10.1021/AC00054A029
Frank J. Feher, David A. Newman, Enhanced silylation reactivity of a model for silica surfaces Journal of the American Chemical Society. ,vol. 112, pp. 1931- 1936 ,(1990) , 10.1021/JA00161A044
C. P. Tripp, M. L. Hair, An infrared study of the reaction of octadecyltrichlorosilane with silica Langmuir. ,vol. 8, pp. 1120- 1126 ,(1992) , 10.1021/LA00040A018
Lane C. Sander, Stephen A. Wise, Synthesis and characterization of polymeric C18 stationary phases for liquid chromatography Analytical Chemistry. ,vol. 56, pp. 504- 510 ,(1984) , 10.1021/AC00267A047
Mary J. Wirth, Hafeez O. Fatunmbi, Horizontal polymerization of mixed trifunctional silanes on silica: a potential chromatographic stationary phase Analytical Chemistry. ,vol. 64, pp. 2783- 2786 ,(1992) , 10.1021/AC00046A022
L. T. Zhuravlev, Concentration of hydroxyl groups on the surface of amorphous silicas Langmuir. ,vol. 3, pp. 316- 318 ,(1987) , 10.1021/LA00075A004