Methacrylic acid and its derivatives are used in the manufacture of important industrial polymeric products. They have a variety of industrial applications including plastics, thickening agents, surfactants, and chelating agents, etc. In the present work, equilibrium extraction of methacrylic acid is carried out to recover it from aqueous solution. A quaternary ammonium salt, trioctylmethylammonium chloride (TOMAC), is used along with different diluents which belong to different categories. These include isoamyl alcohol, n-butyl acetate, methyl isobutyl ketone (MIBK), toluene, carbon tetrachloride, rice bran oil, and kerosene. Parameters such as distribution coefficients, extraction efficiency, loading ratio, stoichiometric loading ratios, and the equilibrium complexation constants are reported. In both physical and chemical extraction processes, MIBK, being proton−accepting, provides maximum extraction efficiency. The values of equilibrium complexation constant of the TOMAC−diluent systems studied decrease in the following order: rice bran oil > carbon tetrachloride > butyl acetate > toluene > kerosene > MIBK > isoamyl alcohol.