SynopsisThe mutual miscibility of random poly( styrene-co-methylmethacry1ate)s with different compositions hut a constant molecular weight of M , 150,000 was studied at room temperature and at 180°C. Compatibility was analyzed with films cast from solutions with different solvents. The reliability of the analytical technique is discussed. The miscibility windows { x , y , } , which define the limits of miscibility of the blends of a given copolymer P(S,MMAI-,) with other copolymers P (S,MMA,,), were determined for all x. The widths I xy z I of these windows are, contrary to the predictions of the Flory-Huggins model, different for yx > x and yx < z, and depend strongly on x . Miscibility is better for blends with a high MMA content. The windows are markedly wider at room temperature. Many blends are, therefore, "semicompatible," i.e., have a critical point of the LCST type between room temperature and 180°C.