Chain order and mobility of high-density c(18) phases by solid-state NMR spectroscopy and liquid chromatography

M Pursch; L C Sander; K Albert

doi:10.1021/ac9606113

Chain order and mobility of high-density c(18) phases by solid-state NMR spectroscopy and liquid chromatography

Anal Chem. 1996 Dec 1;68(23):4107-13. doi: 10.1021/ac9606113.

Authors

M Pursch¹, L C Sander, K Albert

Affiliation

¹ Institut für Organische Chemie, Universität Tübingen, Auf der Morgenstelle 18, D-72076 Tübingen, Germany, and Analytical Chemistry Division, Chemical Science and Technology Laboratory, National Institute of Standards and Technology, Gaithersburg, Maryland 20899.

PMID: 21619319
DOI: 10.1021/ac9606113

Abstract

C(18) phases prepared by different synthetic pathways are examined by solid-state NMR spectroscopy. Silane functionality is clearly indicated by (29)Si CP/MAS NMR spectroscopy. Order and mobility of the alkyl chains are investigated with high-speed (1)H MAS and (13)C CP/MAS NMR spectroscopy. Differences in coverage are monitored by (1)H line widths,( 13)C chemical shifts, (13)C cross-polarization constants, and (1)H relaxation times in the rotating frame. It is shown that C(18) phases prepared by the surface polymerization technique exhibit a more regular surface coverage than sorbents prepared by conventional polymeric synthesis. The findings from solid-state NMR investigations are discussed in the context of liquid chromatography (LC) separations of linear and bulky polycyclic aromatic hydrocarbon (PAH) solutes.