The preparation of fullerenes Cjq to C266 in very high yield (up to 44% extractable) by a plasma discharge is reported. Almost one-third of the extractable material is composed of giant fullerenes C84 to C200. An extraction scheme for isolating selected molecular weightfractions of fullerenes is described. The extractions were characterized by time-of-flight mass spectrometry and Fourier transform mass spectrometry. We find that a Soxhlet extraction with benzene extracts 50% more soluble fullerenes than benzene reflux. Soxhlet extractions with 1, 2, 3, 5-tetramethylbenzene preferentially extract higher molecular weight fullerenes. Hexane appears to limit the amount of higher fullerenes extracted, giving solutions containing CM and