Preparation of thermally stable phenylpolysiloxane fused silica capillary columns. Optimization and evaluation of the deactivation by capillary GC and solid state29Si NMR
✍ Scribed by Wu, Q. ;Hetem, M. ;Cramers, Carel A. ;Rijks, Jacques A.
- Publisher
- John Wiley and Sons
- Year
- 1990
- Tongue
- English
- Weight
- 534 KB
- Volume
- 13
- Category
- Article
- ISSN
- 0935-6304
No coin nor oath required. For personal study only.
✦ Synopsis
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 ^29^Si 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.