Tallow fatty acid consists of mixtures of fatty acids differing in chain length and saturation. In separation of tallow fatty acid, the effects of the type and concentration of detergents and electrolytes were studied. And the changes of acid composition of particular fractions were determined by gas-chromatography. Sodium lauryl sulfate (SLS), sodium lauryl ether sulfate (SLES) and sodium lauryl benzene sulfonate (SLBS) were used as detergents and NaCl, Na2SO4 and MgSO4 were used as electrolytes. At low concentration of detergent, the tallow fatty acid was not fully wetted, and at high concentration, the emulsion was so stable that the tallow fatty acid was not well separated. The addition of proper amount of electrolyte increased the separation efficiency by the decrease of interfacial tension and by the increase of the amount of adsorbed detergent on the surface of solid fatty acid crystals. The optimum range of detergent was 0.4-0.6% (wt.) in SLS, 0.2-0.4% in SLES and 2.0-) .0% in SLBS. And the optimum range of electrolyte was 2.0-2.5% in NaCl, 3.0-4.0% In Na2SO4 and 0.5-1.0% in MgSO4 respectively.