Shenmu-Fugu subbituminous coal liquefaction residue was exhaustively extracted with petroleum ether (PE) to afford PE-extractable fraction (PEEF), which was then eluted with petroleum ether through a silica gel-filled column. The PEEF and eluates were analyzed with a gas chromatographer/mass spectrometer and a Fourier transform infrared spectrometer. As a result, a number of 4- to 7-ring condensed arenes (CAS) were detected in the PEEF series of 4- to 6-ring CAs along with long-chain alkanes were isolated from the PEEF by column chromatography.