A low-temperature, ambient-pressure, catalyzed, batch process involving hydrolysis was used to prepare fatty acids from palm oil and palm kernel oil. The acid value and saponification value were determined and used to calculate the concentration of triglycerides in solutions. The effects of water-to-oil ratio, catalyst concentration, temperature, and reaction time on the hydrolysis were studied, and the kinetics of the hydrolysis was developed. The catalyst used was a mixture of linear alkyl benzene sulfonate and sulfuric acid. The overall rate of reaction expression was used to quantify the mass transfer and chemical reaction resistances and, hence, the total resistance. The mechanism of reaction was also developed. The variation of resistances and reaction rate constant with temperature were investigated. It was found that the kinetics was one of shifting order from zero order to higher order as the reaction progressed from zero time. The total resistance represented the lumped effect of the resistances to mass transfer and chemical reaction, and it was found to be a good measure of the extent of reaction, that is, the smallest total resistance corresponded with the highest conversion and vice versa. Temperature effect on the mass transfer resistance was very weak, but temperature effect on chemical reaction resistance was Strong.