Cyano bonded silica monolith—Development of an in situ modification method for analytical scale columns |
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| Authors: | Arianne Soliven Gary R. Dennis Georges Guiochon Emily F. Hilder Paul R. Haddad R. Andrew Shalliker |
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| Affiliation: | 1. Australian Centre for Research on Separation Science (ACROSS), School of Natural Sciences, University of Western Sydney, Parramatta, NSW, Australia;2. Nanoscale Organisation and Dynamics Group, University of Western Sydney, Parramatta, NSW, Australia;3. Department of Chemistry, University of Tennessee, Knoxville, TN, USA;4. Australian Centre for Research on Separation Science (ACROSS), University of Tasmania, Hobart, Tas., Australia |
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| Abstract: | This study investigates the synthesis and chromatographic behaviour of an analytical size cyanopropyl “cyano” bonded silica monolith. Surface modification was undertaken by treating a neat silica monolith with chloro(3-cyanopropyl)dimethyl silane in dry heptane over a two day period. The resulting monolith showed stability over the duration of the testing program that involved flushing the column with more than 2000 column volumes of mobile phase. Efficiency measurements before and after sylation verified that the integrity of the silica monolith itself was not affected by the modification process, the highest number of theoretical plates (N/m) using anisole was 81,650. A brief selectivity test was then undertaken to assess methylene selectivity and phenyl selectivity. Elemental analysis was used to determine the homogeneity of the carbon load throughout the monolithic bed, and was compared to two commercial C18 and one ‘self’ modified C18 silica monoliths. The development of the in situ modification is also discussed. |
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| Keywords: | Silica monolithic columns Cyano reversed phase Carbon load axial homogeneity |
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