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This paper described a simple method to separate and identify the nitrogen compounds in RFCC diesel oil. A 2％ H2SO4 - CH3CH2OH solution was used to extract nitrogen compounds from RFCC diesel oil. Then the nitrogen- rich solution was further separated to four fractions by a silica gel column liquid - solid chromatography. Two discrete fractions containing neutral and basic nitrogen compounds were identified by APCI and GC - MS. The results indicated that the nitrogen compounds in RFCC diesel oil were anilines, quinoline, indole, carbazole and their derivatives.