Synthesis Of C-60, C-70 and higher fullerenes was carried out at Pakistan Institute of Nuclear Science and Technology (PINSTECH) using dc arc discharge technique. High-performance liquid chromatography (HPLC) and UV-vis spectroscopy are employed to characterize the fullerenes. The toluene extracted fullerene solutions of the raw soot collected from four different regions (A-D) of dc arc discharge fullerene generator were compared with pure C-60 toluene solution. Due to poor solubility Of C-60 in HPLC grade methanol, different fractions of methanol as a mobile phase with toluene were tried. The mobile phase composition of 80:20 methanol: toluene was found an optimal ratio to achieve the best separation factor of 1.246 between C-60 and C-70 fullerenes. Quantitative concentration is calculated from the HPLC and UV-vis spectra. The molarity Of C-60 carbon molecules for all the regions is calculated from the HPLC spectra by comparing the spectra of known molar solution Of C-60. The maximum concentration Of C-70 is found to be 21% in the region B that is nearer the arc zone and at a higher temperature than other regions. Both the techniques confirm the presence Of C-60, C-70 and higher fullerenes in all the four regions with variation in concentration Of C-60 and C-70. UV-vis spectra of the region C show the additional absorption bands at 285 and 305 nm. (c) 2005 Elsevier B.V All rights reserved.