The objective of this research was to find out the effect of molecular weight of poly(methyl methacrylate) (PMMA) and temperature on the isobaric relaxation behaviors of mixed PMMA/poly(styrene)-block-poly(ethylene oxide) (PS-b-PEO) monolayers. Isobaric relaxation experiments of mixed monolayers of PMMA with different molecular weights and PS-b-PEO at the air/water interface were investigated at three different temperatures (10, 25, and 40 C). The PS-b-PEO monolayer was found to exhibit a fast relaxation curve (i.e., the surface area decreased significantly with increasing time). Addition of PMMA into PS-b-PEO slowed the relaxation behavior especially at the lowest experimental temperature (10 C). It was shown that the area relaxation process of mixed PMMA/PS-b-PEO monolayers could be well represented by a model considering the nucleation and growth mechanisms. The characteristic exponent x values were found to be almost temperature independent. The k x values were detected to decrease mostly as a result of temperature elevation regardless of pure or mixed monolayers. V C 2012 Wiley Periodicals, Inc. J Appl Polym Sci 126: E267-E274, 2012