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th  - 1987 - 51st ENC Conference

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MF27<br />

MULTINUCLEAR SOLID-STATE NMR STUDIES OF DERIVATIZED SILICA GELS<br />

Robert Zeigler, Greg Quinting, Charle~ E. Bronnimann<br />

and Gary E. Maciel<br />

Department of Chemistry<br />

Colorado State University<br />

Ft. Collins, CO 80523<br />

Solid-state NMR has been demonstrated to be an extremely powerful<br />

technique for probing <strong>th</strong>e structure and dynamics of molecules bound to a<br />

solid surface (1,2). IH, 15N, 29Si and 13C CP/MAS spectra will be pre-<br />

sented for silica gels derivatized wi<strong>th</strong> APTS (aminopropyltrie<strong>th</strong>oxysi-<br />

lane). 13C, 15N, IH (CRAMPS) spectra provide evidence regarding <strong>th</strong>e<br />

nature of <strong>th</strong>e interaction between <strong>th</strong>e amine group of APTS-derivatized<br />

silica gels and <strong>th</strong>e silica gel surface.<br />

13C and 29Si NMR techniques have been used to explore <strong>th</strong>e conforma-<br />

tions and dynamics of dime<strong>th</strong>yloctadecylchlorosilane(C18)-modified silica<br />

gel. The effects of bo<strong>th</strong> C18 surface concentration and <strong>th</strong>e presence of<br />

solvents on <strong>th</strong>e C18 chain dynamics have been explored using TCH and<br />

dipolar dephasing experiments.<br />

IH CRAMPS, 29Si and 13C NMR are being used to study <strong>th</strong>e nature<br />

of <strong>th</strong>e silica surface and silica silylation. Several different species<br />

of protons have been observed on <strong>th</strong>e silica surface and a variety of<br />

instrumental and chemical techniques are being used to characterize <strong>th</strong>e<br />

silica surface.<br />

References<br />

1. Solid State NMR Studies of Aminopropyltrie<strong>th</strong>oxysilane Modified Silica;<br />

G.S. Caravajal, D.E. Leyden, G.E. Maciel, p. 283 in Silanes, Surfaces,<br />

and Interfaces Symposium, D.E. Leyden (ed.) Gordon and Breach Science<br />

Publ. (1986).<br />

2. NMR Studies of cl~-Derivatized Silica Systems; G.E. Maciel, R.C.<br />

Zeigler, R.K. TaTt, p. 413 in Silanes, Surfaces, and Interfaces<br />

Symposium, D.E. Leyden (ed.) Gordon and Breach Science Publ. (1986).

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