Higher fullerences in ODCB extract of primary soots by arc-heating method were concentrated by selective complexation between t-butyl calixene^[^8^] and C60. Better seperation and UV-Vis spectra of higher fullerenes C70, C76, C78, C84 and C86 were achieved using Waters 2010-HPLC. We found that the ratio of C78 isomers extracted by ODCB is different from that of extracts by other solvents such as toluene and CS2. In the process of HPLC seperation, we found that the logarithm of retention time ln(r~R) has a linear relationship with the number of fullerene carbons (Carbon Number Rule of Fullerenes), we also found that the spectra of fullerenes have a tendency of red-shift associated with the reduction of the symmestry of fullerenes. The existence and seperation of C86 were discussed by analysizing the LD-TOFMS, UV-Vis, HPLC and Carbon Number Rule of Fullerenes.

Key words: ULTRAVIOLET SPECTROPHOTOMETRY, HIGH SPEED LIQUID CHROMATOGRAPHY, MASS SPECTROGRAPHY, CARBON ATOM, FULLERENES