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From the first issue of 2016, Chromatography has changed its name to Separations.

Open AccessArticle
Chromatography 2015, 2(2), 141-155; doi:10.3390/chromatography2020141

Surface Characterization of Some Novel Bonded Phase Packing Materials for HPLC Columns Using MAS-NMR Spectroscopy

Department of Chemistry, Northeastern State University, Broken Arrow, OK 74014, USA
Academic Editor: Frank L. Dorman
Received: 21 December 2014 / Revised: 20 February 2015 / Accepted: 4 March 2015 / Published: 24 March 2015
View Full-Text   |   Download PDF [1614 KB, uploaded 24 March 2015]   |  

Abstract

Information on the surface properties of three novel chemically bonded phase packing materials for High performance liquid chromatography (HPLC) were obtained using spectra obtained by solid state cross-polarization (CP) magic-angle spinning (MAS) nuclear magnetic resonance (NMR) spectroscopic experiments for the 29Si, and 13C nuclei. These packing materials were: Cogent bidentate C18 bonded to type-C silica, hybrid packing materials XTerra MS C18, and XBridge Prep. C18. The spectra obtained using cross-polarization magic angle spinning (CP-MAS) on the Cogent bidentate C18 bonded to type-C silica show the surface to be densely populated with hydride groups (Si-H), with a relative surface coverage exceeding 80%. The hybrid packing materials XTerra and XBridge gave spectra that reveal the silicon atoms to be bonded to organic moieties embedded in the molecular structure of these materials with over 90% of the alkyl silicon atoms found within the completely condensed silicon environments. The hydrolytic stability of these materials were investigated in acidic aqueous solutions at pHs of 7.0 and 3.0, and it was found that while the samples of XTerra and XBridge were not affected by hydrolysis at this pH range, the sample of Cogent lost a significant proportion of its Si-H groups after five days of treatment in acidic aqueous solution. View Full-Text
Keywords: surface characterization; MAS-NMR; packing materials; HPLC surface characterization; MAS-NMR; packing materials; HPLC
This is an open access article distributed under the Creative Commons Attribution License which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited. (CC BY 4.0).

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Abia, J. Surface Characterization of Some Novel Bonded Phase Packing Materials for HPLC Columns Using MAS-NMR Spectroscopy. Chromatography 2015, 2, 141-155.

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