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Structural Characterization of Polysilicate Intermediates Formed During Sol-Gel Polymerization

  • W. G. Klemperer (a1), V. V. Mainz (a1), S. D. Ramamurthi (a1) and F. S. Rosenberg (a1)

Abstract

Identification of polysilicate intermediates formed during sol-gel processing of silica gels and glasses is an important step toward understanding the nature of this process on a molecular level. Although capillary gas chromatography using mass spectrometric detection gives the molecular formulas for low molecular weight intermediates [1], this approach is only semi-quantitative and provides no structural information. An improved protocol has been developed that allows structural assignment and quantitative determination of the principal mono- through hexasilicate structural isamers formed by hydrolysis of methanolic tetramethylorthosilicate in the presence of HC1. This protocol combines quenching by diazomethane, fractionation using spinning band column distillation, identification by capillary gas chromatography, and structural characterization using 29Si{1H} NMR techniques (l-pulse, ID-INADEQUATE, and 2D-INADEQUATE) to provide structural assignments and response factors for the components separated by gas chromatography.

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References

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Klemperer, W. G. and Ramamurthi, S. D., Polym. Prepr., Am. Chem. Soc. Div. Polym. Chem. 28, 432 (1987).
2. For recent studies of sol-gel polymerization, see: a) Ultrastructure Processing of Ceramics, Glasses, and Composites, edited by Hench, L. L. and Ulrich, D. R. (John Wiley and Sons, New York, 1984);
b) Better Ceramics Through Chemistry, edited Brinker, C. J., Clark, D. E., and Ulrich, D. R. (Mater. Res. Proc. 32, Elsevier, New York, 1986);
c) Science of Ceramic Processing, edited by Hench, L. L. and Ulrich, D. R. (John Wiley and Sons, New York, 1986);
d) Better Ceramics Through Chemistry II, edited by Brinker, C. J., Clark, D. E., and Ulrich, D. R. (Mater. Res. Soc. Proc. 73, Pittsburgh, 1986).
3. Klemperer, W. G. and Ramamurthi, S. D., these Proceedings.
4. Engelhart, G. and Michel, D., High-Resolution Solid-State NMR of Silicates and Zeolites (John Wiley and Sons, Chichester, 1988) Chapter III.
5. Derome, A. E., Modern MR Techniques for Chemistry Research (Pergamon Press, New York, 1987) pp. 234239.

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