ISSN:
0935-6304
Keywords:
Gas chromatography, GC
;
Fused silica capillary columns
;
CP-MAS NMR
;
Deactivation methods
;
Chemistry
;
Analytical Chemistry and Spectroscopy
Source:
Wiley InterScience Backfile Collection 1832-2000
Topics:
Chemistry and Pharmacology
Notes:
The effect of deactivating a fused silica surface by silylation with 1,1,3,3-tetraphenyl-1,3-dimethylilazane (TPDMDS), triphenylsilylamine (TPSA), and octamethylcyclotetrasiloxane (D4) and by polydimethylsiloxane degradation (PSD) is studied. Rehydrated, dried, and deactivated Cab-O-Sil M5 samples are used as model materials for 29Si CP-MAS NMR analysis.At about 350 °C, TPDMDS yelds mainly diphenylmethylsiloxysilane, dimethyldisiloxysilane, and triphenylsiloxysilane groups. TPSA yields phenyltrisiloxysilane, diphenyldisiloxysilane, and triphenylsiloxysilane groups. At 400°C, the products formed initially are eventually replaced by methyltrisiloxysilane or phenyltrisiloxysilane groups, while a substantial number of silanol groups still remains. The possible consequences for wettability are discussed.D4 reacts with Cab-O-Sil even at 200°C, but a large number of silanol groups remains. This number decreases gradually at higher temperatures and becomes negligible above 400°C. The formation of methyltrisiloxysilane groups, which starts at 425°C, is predominant at 490°C.
Additional Material:
9 Ill.
Type of Medium:
Electronic Resource
URL:
http://dx.doi.org/10.1002/jhrc.1240081005
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