The synthesis of biofuels through the pyrolysis of vegetable oil is studied as an alternative to the biodiesel process because it produces bio hydrocarbons that have similar properties to fossil fuels. This study uses palm olein as raw material reacted at gradually increasing temperatures ranging from 225, 250, 275, and 300°C, using zeolite as catalyst at atmosferic pressure. The volatiles compounds are condensed and collected according to the fraction and analyzed for density, viscosity, calorific value, moisture content and composition of volatile compounds using GC-MS. Palm olein as raw material had the characteristics of moisture content of 0.095% (w/w), viscosity of 41.25 mm2/s, calorific value of 39.93 MJ/kg and pour point of 20°C. The hydrocarbon fractions of various temperatures had a red to bright yellow color, liquid phase and only the 300°C fraction which had a solid fraction. The density was in the range of 0.8452 - 0.8527 g/cm3(40°C), viscosity of 3.0726 - 3.8137 mm2/s, moisture content of 0.0801 - 0.1878% (w/w) and pour point of 4 - 22 ° C. Density, viscosity and pour point from a temperature fraction of 225 – 275°C met national biodiesel standards. The composition of volatile compounds mainly consisted of n-decanoic acid, undecanoic acid, dodecanoic acid, 8-heptadecene, heptadecane, tetradecanoic acid, 2-heptadecanone, and n-hexadecanoic acid. The main volatile compounds were still in the form of fatty acids where n-hexadecanoic acid was the dominant compound (42.8 - 71.6%). In general, the characteristics and profiles of the volatile compounds of 225, 250 and 275°C fractions were similar and different from the 300°C fraction.