Fossil energy is a limited source of primary energy, various efforts have been made to ﬁnd alternative fuels that are renewable. Vegetable oil is one of the plants that can be a source of energy, but must be converted into other forms, namely alkyl esters (biodiesel). Biodiesel is a diesel fuel substitute that can be used as a raw material for making or mixing in transportation fuels. In this study, biodiesel will be produced using an esteriﬁcation-transesteriﬁcation process with NiZn/Al2O3catalyst. Process variables include:temperaturesof90,120,150and180oC.theratiooffeedmethanol:palmoilata ratio of 1: 15. The concentration of NiZn/Al2o3 catalyst was varied at 1, 1.5, 2, and 2.5%. NiZn/Al2O3 catalyst was synthesized using wet impregnation method with loading of nickel and Zink at 5% wt. The catalyst will be analyzed using XRD and SEM analysis. Nickel and Zink metals in the NiZn/Al2O3catalyst catalyst have been dispersed on the surface of Al2O3. Al2O3 calcination before the impregnation process produced NiZn /Al2O3 catalyst with a crystallinity of 62,99%. The results of this study concluded that the biodiesel produced increased with increasing catalyst concentration, temperature, reaction in the esteriﬁcation-transesteriﬁcation process where at a temperature of 90oC and catalyst concentration 0.015 g catalyst / gr feed and reaction time of 1.5 hours obtained biodiesel yield of 35.8%, at temperature of 90oC and at a temperature of 180oC and catalyst concentration of 0.01 g catalyst/gr feed obtained biodiesel yield of 48.3%. Biodiesel was analyzed by GCMS to measure the composition of methyl esters and test the properties of biodiesel according to ASTM standards.