Supercritical carbon dioxide versus toluene as reaction media in silica functionalisation: Synthesis and characterisation of bonded aminopropyl silica intermediate

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dc.contributor.author Ashu-Arrah, Benjamin A.
dc.contributor.author Glennon, Jeremy D.
dc.date.accessioned 2017-05-12T11:36:34Z
dc.date.available 2017-05-12T11:36:34Z
dc.date.issued 2017-04-14
dc.identifier.citation Ashu-Arrah, B. A. and Glennon, J. D. (2017) 'Supercritical carbon dioxide versus toluene as reaction media in silica functionalisation: Synthesis and characterisation of bonded aminopropyl silica intermediate', Journal of Chromatography A, 1501, pp. 18-25. doi:10.1016/j.chroma.2017.04.030 en
dc.identifier.volume 1501 en
dc.identifier.startpage 18 en
dc.identifier.endpage 25 en
dc.identifier.issn 0021-9673
dc.identifier.uri http://hdl.handle.net/10468/3955
dc.identifier.doi 10.1016/j.chroma.2017.04.030
dc.description.abstract This research reports supercritical carbon dioxide versus toluene as reaction media in silica functionalisation for use in liquid chromatography. Bonded aminopropyl silica (APS) intermediates were prepared when porous silica particles (Exsil-pure, 3 μm) were reacted with 3-aminopropyltriethoxysilane (3-APTES) or N,N-dimethylaminopropyltrimethoxysilane (DMAPTMS) using supercritical carbon dioxide (sc-CO2) and toluene as reaction media. Covalent bonding to silica was confirmed using elemental microanalysis (CHN), thermogravimetric analysis (TGA), zeta potential (ξ), diffuse reflectance infrared Fourier transform (DRIFT) spectroscopy, scanning electron microscopy (SEM) and solid-state nuclear magnetic resonance (CP/MAS NMR) spectroscopy. The results demonstrate that under sc-CO2 conditions of 100 °C/414 bar in a substantial reduced time of 3 h, the surface coverage of APS (evaluated from%C obtained from elemental analysis) prepared with APTES (%C: 8.03, 5.26 μmol/m−2) or DMAPTES (%C: 5.12, 4.58 μmol/m2) is somewhat higher when compared to organic based reactions under reflux in toluene at a temperature of 110 °C in 24 h with APTES (%C: 7.33, 4.71 μmol/m2) and DMAPTMS (%C: 4.93, 4.38 μmol/m2). Zeta potential measurements revealed a change in electrostatic surface charge from negative values for bare Exsil-pure silica to positive for functionalised APS materials indicating successful immobilization of the aminosilane onto the surface of silica. en
dc.description.sponsorship Science Foundation Ireland (Irish Separation Science Cluster (ISSC) http://www.separationscience.ie under their Strategic Research Cluster (SRC) programme (grant 08/SRC/B1412)) en
dc.format.mimetype application/pdf en
dc.language.iso en en
dc.publisher Elsevier en
dc.rights © 2017 Elsevier. This manuscript version is made available under the CC-BY-NC-ND 4.0 license http://creativecommons.org/licenses/by-nc-nd/4.0/ en
dc.rights.uri http://creativecommons.org/licenses/by-nc-nd/4.0/ en
dc.subject Chemical functionalisation en
dc.subject Supercritical CO2 en
dc.subject Aminopropyl bonded silica (APS) en
dc.subject Bi-functional bonding en
dc.subject Surface coverage/conversion efficiency en
dc.title Supercritical carbon dioxide versus toluene as reaction media in silica functionalisation: Synthesis and characterisation of bonded aminopropyl silica intermediate en
dc.type Article (peer-reviewed) en
dc.internal.authorcontactother Jeremy Glennon, Chemistry, University College Cork, Cork, Ireland. +353-21-490-3000 Email: j.glennon@ucc.ie en
dc.internal.availability Full text available en
dc.check.info Access to this article is restricted until 24 months after publication at the request of the publisher. en
dc.check.date 2019-04-14
dc.date.updated 2017-05-12T11:28:43Z
dc.description.version Accepted Version en
dc.internal.rssid 394743291
dc.contributor.funder Science Foundation Ireland en
dc.description.status Peer reviewed en
dc.identifier.journaltitle Journal of Chromatography A en
dc.internal.copyrightchecked No !!CORA!! en
dc.internal.licenseacceptance Yes en
dc.internal.IRISemailaddress j.glennon@ucc.ie en


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© 2017 Elsevier. This manuscript version is made available under the CC-BY-NC-ND 4.0 license http://creativecommons.org/licenses/by-nc-nd/4.0/ Except where otherwise noted, this item's license is described as © 2017 Elsevier. This manuscript version is made available under the CC-BY-NC-ND 4.0 license http://creativecommons.org/licenses/by-nc-nd/4.0/
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