m-Xylene is separated from a mixture of C 8 aromatic hydrocarbons (e.g., a raffinate from a p-xylene plant) by chromatography and distillation. Toluene (desorbent) and a mixture of C 8 aromatic hydrocarbons containing m-xylene are applied to a chromatographic separation apparatus packed with a zeolite strongly adsorbing m-xylene for separating the mixture into them -xylene fraction and the non-m-xylene fraction, followed by a first distillation for distilling the m-xylene fraction and separatingm -xylene and toluene, a second distillation for distilling the non-m-xylene fraction and separating the high boiling material and toluene, and recycling the toluene desorbent recovered in the first and the second distillation steps. This process efficiently recovers m-xylene of high purity ( 99.5%) which is suitable as a raw material for isophthalic acid manufacture.