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This paper reports experimental conversion of spent vegetable oil with bio-ethanol to long chain biodiesel fuel in presence of a new developed solid K3PO4 heterogeneous catalyst. Examined catalyst was synthesized following dipping impregnation of γ-Al2O3 solid support in an aqueous solution of potassium phosphate tri-basic K3PO4. K3PO4/γ-Al2O3 catalyst samples were distinguished based on their percentage loadings of K3PO4 (CK3PO4) and averaged particle size (dp). Produced catalyst samples were characterized in terms of their textural and surface properties using nitrogen adsorption-desorption isotherms and carbon dioxide & ammonia temperature programmed desorption techniques respectively. While the liquid phase of the product was analyzed using a GC-Mass spectroscopy technique. Ethanolysis runs were carried out following surface response methodology, central composite design (CCD).