Patching in reversed-phase high-performance liquid chromatographic materials studied by solid-state NMR spectrometry

The distribution of silane chains over the silica gel surface in reversed-phase high-performance liq. chromatog. (RP-HPLC) phases was studied with special attention being paid to surface homogeneity: there might be areas with high coverage and areas with low coverage of silane chains, hence clustering or patching of the silane chains can occur. Two RP phases were studied before and after well conditioned aging, together with 4 silylated silica gels (serving as models). Two solid-state NMR techniques (e.g.,1H-29Si dipolar dephasing 29Si cross-polarization magic angle spinning NMR and 13C spin-lattice relaxation in the rotating frame) were used. For the 4 model compds. with varying degrees of coverage, only differences in the NMR time consts. were obsd. between the maximally covered phase and the 3 less densely covered silica gels. This proves that silane chains on an RP phase with max. coverage are restricted in their mobilities with respect to the less densely packed materials. For the 2 non-aged RP phases, the silane chains are probably homogeneously distributed over the silica gel surface. Further, the non-aged RP phases were compared with their counterparts, aged under well defined exptl. conditions. After aging, no differences were found between the original and the aged phases, now indicating however, that patching had developed upon agein