Structural Characterization of Polysilicate Intermediates Formed During Sol-Gel Polymerization

Autor:	Walter G. Klemperer, F. S. Rosenberg, S. D. Ramamurthi, V. V. Mainz
Rok vydání:	1988
Předmět:	Materials science Quenching (fluorescence) Diazomethane Fractionation law.invention chemistry.chemical_compound Hydrolysis chemistry Polymerization law Physical chemistry Gas chromatography Distillation Sol-gel
Zdroj:	MRS Proceedings. 121
ISSN:	1946-4274 0272-9172
DOI:	10.1557/proc-121-15
Popis:	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.
Databáze:	OpenAIRE
Externí odkaz:	https://explore.openaire.eu/search/publication?articleId=doi_________::becc67f61629edf7b9d61c1d0cc0d81e https://doi.org/10.1557/proc-121-15 Zobrazit plný text záznamu Full text from SpringerLink