Retention of Fullerenes by Octadecyl Silica. Correlation with NMR Spectra at Low Temperatures

The temperature effect on the retention of fullerenes in the range 80°C to −70°C in liquid chromatography (LC) has been examined using octadecylsilica stationary phases (ODS). It has been found that the maximum retention temperature lies around −10°C with a highly carbon loaded ODS phase. Solid state CPMAS NMR measurements on the stationary phases indicated that the relaxation time at the 30 ppm methylene signal changes with the temperature and has a minimum relaxation time at the temperature which closely matches the maximum retention temperature observed in chromatography. The interpretation of both NMR spectroscopic and LC chromatographic data are discussed.