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Trammell BC, Ma L, Luo H, et al. Highly cross-linked self-assembled monolayer stationary phases: an approach to greatly enhancing the low pH stability of silica-based stationary phases. Anal Chem. 2002;74(18):4634-9doi: 10.1021/ac020206d.
Trammell, B. C., Ma, L., Luo, H., Jin, D., Hillmyer, M. A., & Carr, P. W. (2002). Highly cross-linked self-assembled monolayer stationary phases: an approach to greatly enhancing the low pH stability of silica-based stationary phases. Analytical chemistry, 74(18), 4634-9. https://doi.org/10.1021/ac020206d
Trammell, Brian C, et al. "Highly cross-linked self-assembled monolayer stationary phases: an approach to greatly enhancing the low pH stability of silica-based stationary phases." Analytical chemistry vol. 74,18 (2002): 4634-9. doi: https://doi.org/10.1021/ac020206d
Trammell BC, Ma L, Luo H, Jin D, Hillmyer MA, Carr PW. Highly cross-linked self-assembled monolayer stationary phases: an approach to greatly enhancing the low pH stability of silica-based stationary phases. Anal Chem. 2002 Sep 15;74(18):4634-9. doi: 10.1021/ac020206d. PMID: 12349964.
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Anal Chem. 2002 Sep 15;74(18):4634-9. doi: 10.1021/ac020206d.

Highly cross-linked self-assembled monolayer stationary phases: an approach to greatly enhancing the low pH stability of silica-based stationary phases.

Analytical chemistry

Brian C Trammell, Lianjia Ma, Hao Luo, Dihua Jin, Marc A Hillmyer, Peter W Carr

Affiliations

  1. Department of Chemistry, University of Minnesota, Minneapolis 55455, USA.

PMID: 12349964 DOI: 10.1021/ac020206d

Abstract

A new type of silica-based stationary phase with dramatically improved acid stability compared to any currently available silica-based stationary phase has been developed. Superior low pH stability is achieved by first self-assembling a densely bonded monolayer of (chloromethyl)-phenylethyltrichlorosilane (CMPES). The self-assembly step is followed by a Friedel-Crafts cross-linking of the reactive moieties with their neighbors, by addition of secondary, cross-linkable aromatic reagents, or by both. This phase is not endcapped. Elemental analysis data shows that an aluminum chloride catalyst is very effective at bonding aromatic cross-linking reagents, such as styrene heptamer and triphenylmethane, to the reactive CMPES monolayer. The stability of the retention factor of decylbenzene on the cross-linked self-assembled CMPES phases is compared to a sterically protected C18 phase to illustrate its superior resistance to acid-catalyzed-phase loss. Inverse size exclusion chromatography and flow-curve comparisons of the cross-linked self-assembled CMPES and the sterically protected C18 stationary phases illustrate their similar chromatographic efficiency.

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