Influence of the process parameters for the industrially relevant reaction of free fatty acid (FFA) with glycerol is investigated. Furthermore, several drying techniques are investigated and a novel method is suggested that can provide more realistic experimental conditions. Silica as an absorbent is found to be a more suitable method for water removal than distillation or carrier gas. Using response surface methodology, important parameters are identified and optimal conditions found. Empirical correlation is developed to account for the most important parameters. Both oil:glycerol ratio and temperature have optimal values for which the highest conversion can be achieved. Interestingly, the highest conversion can be obtained at 220°C; above this temperature the conversion decreases. It is found that the influence of oil:glycerol ratio also exhibits anomalous behavior, where conversion is constant and decreases above a certain value. At optimal conditions, the FFA is reduced to 1.6% from the initial 8.6%.