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In the supercritical CO2 method of extraction of palm oil, many processes in conventional method, such as degumming, deodorization, refining and bleaching processes, are eliminated. The supercritical method allows palm oil to be extracted and fractionated simultaneously, which not only reduces the cost of processing, but also provides a more environmental-friendly processing alternative. In this research, the high-pressure phase behaviour of the binary system between supercritical carbon dioxide (SC–CO2) and palm oil fatty acid components were investigated. The phase transition is observed from a camera which is connected to a high-pressure variable-volume view cell. Carbon dioxide has high solvating power, nontoxic, inflammable and low critical points. The determination of phase behaviour could offer an insight to the right operating condition of palm oil supercritical fluid carbon dioxide extraction process in order to acquire the desired extraction selectivity and an optimum yield. The phase boundaries of some fatty acids components, lauric acid (C12), stearic acid (C18), and oleic acid (C18) in compressed supercritical carbon dioxide were determined at temperatures of 313.15 K, 323.15 K, 333.15 K, 343.15 K and 353.15 K under pressures between 10 MPa and 60 MPa.