One-pot synthesis of a new high vinyl content hybrid silica monolith dedicated to nanoliquid chromatography

Racha El Debs 1 Pauline Gay 1 Vincent Dugas 1 Claire Demesmay 1, *
* Corresponding author
1 Separative Methods - Techniques séparatives
ISA - Institut des Sciences Analytiques
Abstract : A new vinyltrimethoxysilane-based hybrid silica monolith was developed and used as a reversed-phase capillary column. The synthesis of this rich vinyl hybridmacroporous monolith, by cocondensation of vinyltrimethoxysilane with tetramethoxysilane, was investigated using an unconventional (formamide, nitric acid) porogen/catalyst system. A macroporous hybrid silica monolith with 80% in mass of vinyltrimethoxysilane in the feeding silane solution was obtained and compared to a more conventional low vinyl content hybrid monolith with only of 20% vinyltrimethoxysilane. Monoliths were characterized by scanning electron microscopy, Si-29 nuclear magnetic resonance spectroscopy and N-2 adsorption-desorption. About 80% of the vinyl precursor was incorporated in the final materials, leading to 15.9 and 61.5% of Si atoms bonded to vinyl groups for 20% vinyltrimethoxysilane and 80% vinyltrimethoxysilane, respectively. The 80% vinyltrimethoxysilane monolith presents a lower surface area than 20% vinyltrimethoxysilane (159 versus 551 m(2)/g), which is nevertheless compensated by a higher vinyl surface density. Chromatographic properties were evaluated in reversed-phasemode. Plots of ln(k) versus percentage of organic modifier were used to assess the reversed-phase mechanism. Its high content of organic groups leads to high retention properties. Column efficiencies of 170 000 plates/m were measured for this 80% vinyltrimethoxysilane hybrid silica monolith. Long capillary monolithic columns (90 cm) were successfully synthesized (N = 120 000).
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Submitted on : Friday, August 26, 2016 - 4:57:43 PM
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Racha El Debs, Pauline Gay, Vincent Dugas, Claire Demesmay. One-pot synthesis of a new high vinyl content hybrid silica monolith dedicated to nanoliquid chromatography. Journal of Separation Science, Wiley-VCH Verlag, 2016, 39 (5), pp.842-850. ⟨10.1002/jssc.201501076⟩. ⟨hal-01356863⟩



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