The availability of waste shells and empty palm oil bunches is very potential to be processed into liquid smoke. Liquid smoke is obtained from condensation of smoke resulting from the decomposition of organic compounds contained in shells and empty bunches of oil palm in the pyrolysis process. In this study investigated the effect of massvariations of raw materials and heating temperature on the shell pyrolysis process and empty fruit bunches of oil palm into liquid smoke. Variations in mass of raw materials are (125 grams of empty bunches and 375 grams of oil palm shells;250 grams of empty bunches and 250 grams of oil palm shells;375 grams of empty bunches and 125 palm oil shells) with heating temperatures at 400ºC and 500ºC. The parameters measured are density, color and aroma, yield on each sample, pH, concentration of acetic acid andphenol. From the results of the study, it is known that the sample that produces the most liquid smoke is a mixture of 125 grams of empty bunches and 375 grams of palm oil shells at a temperature of 500oC which is 266 mL. The liquid smoke is then purifiedby the distillation method to a temperature of 150oC. Liquid smoke color changes from black brown to clear to brass, liquid smoke has a sharp aroma of smoke. The mass of liquid smoke is 0.9866 g/mL with pH 2. The concentration of acetic acid is 10.793% and phenol is 56.856%.Keywords: distillation, pyrolysis, acetic acid, phenol.