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Recycle solvents were obtained in 50 days of continuous operation of a 1 ton/day coal-liquefaction plant at Kimitsu. Acidic fractions were obtained by base extraction for the starting solvent and final solvent, and their components were analyzed in detail by gas chromatography/mass spectrometry. The application of a selected ion monitoring technique has allowed the assignment of the atomic compositions to practically all compounds despite many of their presence as overlapping peaks on the chromatogram: 327 individual compounds for 142 peaks. These compounds have been classified into nine of compound types: phenols, indanols/tetrahydronaphthols, naphthols, biphenyl-ols/acenaphthenols, hexahydroacenaphthylenols, fluorenols, phenanthrenols/anthracenols, phenyl-naphthols, and pyrenols/fluoranthenols. As compared to the initial solvent, the final solvent contains higher concentrations of indanols/tetrahydronaphthols and hexahydro-acenaphthylenols and contains a lower concentration of pyrenols/fluoranthenols.