A process for the high yield production of high purity glacial methacrylic acid ("HPMAA") with minimization of decomposition of hydroxy isobutyric acid (HIBA). The HPMAA is substantially pure, specifically 99% pure or greater with a water content of 0.05% or less. This improved process involves the steps of providing a crude MAA stream which was formed by hydrolyzing acetone cyanohydrin and, therefore, includes HIBA which is an intermediate product of the hydrolysis reaction, and purifying that crude methacrylic acid stream in a series of successive distillation steps.