Preparation of thermally stable phenylpolysiloxane fused silica capillary columns : optimization and evaluation of the deactivation by capillary GC and solid state 29Si NMR

Quanji Wu, M.J.J. Hetem, C.A.M.G. Cramers, J.A. Rijks

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Abstract

The deactivation of fused silica capillary columns with a laboratory-made poly-diphenylvinylmethylhydrosiloxane copolymer has been investigated. The deactivation obtained at different temperatures and reaction times is characterized with a dual column capillary GC system [1]. In parallel, the effect of the silylation temperatures and reaction times on the nature, the structure, and the chemical properties of the deactivation layer has also been studied by solid-state 29Si NMR spoctroscopy. A fumed silica, Cab-O-Sil M5, was used as a model substrate for these spectroscopic studies. The deactivated fused silica capillaries show an excellent thermal stability (up to 400°C), a high resistance to solvolysis, and a minimal interaction to various critical test components. A good wettability of the fused silica capillary columns deactivated with this reagent was confirmed by successful subsequent coating with polysiloxanes with different phenyl contents
Original languageEnglish
Pages (from-to)811-816
JournalJournal of High Resolution Chromatography
Volume13
Issue number12
DOIs
Publication statusPublished - 1990

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