In this study, a systematic and detailed investigation on liquid-liquid extraction of sulfur olive oil miscella in hexane with aqueous ethanol solutions was performed. Optimal extraction conditions for recovery of free fatty acids (FFA) with a minor loss of neutral oil were determined in bench-scale single-stage extractions. It was concluded that, to ensure deacidification with a low triglycerides loss, it is appropriate to extract the miscella with 30% or more dilute ethanol solutions. It was also noted that under these circumstances the free fatty acid percentage extracted is not affected by increases in contents of FFA and partial glycerides of sulfur olive oil, and the solvent must be saturated with hexane before extraction. Changing the oil:hexane ratio in miscella from 1:2 to 2:1 by weight did not have any significant effect on extraction results.