The aim of this study was to separate phenol from Bio-Oil obtained from the pyrolysis of agricultural wastes (BAW). The BAW was obtained in one step catalytic pyrolysis in which temperature of the reactor was kept at 30°C and then increased up to 900°C. After pyrolysis, the BAW was distillated and analyzed by Gas chromatography and Mass spectrometry (GC-MS) technique and comprehensive two-dimensional gas chromatography with time-of-flight mass spectrometry detection (GC × GC/TOFMS) Where BAW showed the presence of more than 120 other important compounds and phenol. After detection, phenol was separated by solvent extraction method, where Ethyl ether (C 4 H 10 O), Caustic soda (NaOH) and Hydrochloric acid (HCl) were used to separate phenol from BAW and then Nuclear magnetic resonance spectroscopy (NMR) was done to confirm the recovery of phenol.