High performance liquid chromatographic–mass spectrometric detection of giant fullerenes

Fullerene-rich soot generated by resistive heating of graphite has been gently extracted with toluene, in order to remove some C₆₀ and C₇₀ compounds, followed by extraction with boiling 1,2,4-trichlorobenzene at 214°C. After filtration and removal of the solvent, the residue was re-dissolved in dichloromethane and characterized by non-aqueous reversed phase liquid chromatography coupled on-line with atmospheric pressure chemical ionization mass spectrometry. Several novel fullerenes were detected, including C₇₂, C₈₀, C₈₆, and C₈₈ as well as other fullerenes up to C₁₀₈ and higher. The results indicate that chromatographic separation of large fullerene molecules can be achieved with low boiling point solvents and conventional liquid chromatographic techniques.