The pyrolysis process has been used recently to produce wood vinegar from various agro-residues with the intent to investigate their chemical composition and potential uses. In the present study, two agro wastes corncob of Zea mays and stem of Areca catechu (Areca nut) are utilized to produce wood vinegar through the pyrolysis process. Characterization of these corncobs and Areca nut stem-based wood vinegar was investigated via Gas Chromatography-Mass Spectroscopy (GC-MS). Twenty-five compounds were identified from each wood vinegar sample.