Linoleic acid is a Poly-Unsaturated Fatty Acid (PUFA) that corresponds to Omega 6 Fatty Acid. This is the major component of vegetable oil and very important for health. As an essential fatty acid, linoleic acid has to be obtained from foods. Consumption of omega fatty acid in the form of concentrate has more benefit than the whole oil. Fulfilling this requirement, effective method to separate PUFAs from vegetable oils is needed. One of the favorable methods is urea complexation. Palm oil was used as the fatty acids resource due to its potential feedstock in Indonesia. This aim of this research is to study the effect of urea, ethanol and free fatty acid (FFA) ratios during complexation of palm oil. This research was developed in three steps, 1) free fatty acid preparation from palm oil (saponification process), 2) crystallization of the fatty acids mixture and 3) filtration for separating the unsaturated fatty acid. Concentrated linoleic acid is obtained in the liquid phase, while the saturated fatty acid is obtained in the solid. This research resulted that the concentration of PUFA was increasing as the ratio of urea, FFA and ethanol increases.