Statistical optimization of the silylation reaction of a mercaptosilane with silanol groups on the surface of silica gel

Journal of Chromatography. a
Romain DabreWolfgang Lindner


Thiol-modified silica is often used as an intermediate product for further synthesis of modified stationary phases for chromatography or purification processes. Different conditions were used to synthesize such thiol-modified particles, but systematic optimizations remained scarce. In this study the reaction conditions for the synthesis of mercaptopropyl-modified silica were optimized. The general synthetic method consists in slurrying the silica gel in toluene before adding 3-mercaptopropyldimethoxymethylsilane together with a tertiary amine as catalyst (here dimethylaminopyridine). Reaction time and temperature were optimized using a full factorial design of experiment (DoE) from 3 to 25h with temperature varying between 45 and 105 degrees C. The surface coverage of the silica with mercaptopropyl-groups was analyzed by two different ways (elemental analysis and chemical surface reaction with 2,2'-dipyridyl disulfide followed by HPLC-UV analysis of stoichiometrically liberated pyridyl-2-thione). We obtained a three-dimensional (3D) plot of the surface coverage as a function of reaction time and temperature. The arch-shaped hyperplane allowed us to determine an optimum with regard to time and temperature, which yields to the hi...Continue Reading



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