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Films of a series of monodisperse, moderately syndiotactic poly(methy1 methacrylate) (PMMA) standards, with M,,, ranging from 2,900-428,000, were solution-cast and spun-cast from chloroform onto clean aluminium substrates. The polymers were thoroughly characterized by conventional spectroscopic and chromatographic techniques. The films were studied using x-ray photoelectron spectroscopy (XPS) and time-of-flight secondary-ion mass spectrometry (ToF SIMS). The effects of molecular weight and film thickness on SIMS spectra were investigated thoroughly by unit-mass and high-resolution ToF SIMS. Film thickness had a pronounced effect on the negative SIMS spectra, particularly in films a few monolayers thick. This was seen in both the total negative ion counts ( d z and the key negative ion intensity ratios. A parallel effect was observed with respect to the effect of molecular weight. These differences are attributed to (i) the original end-group concentration in the surface which decreases with increasing molecular weight and (ii) the original end-group concentration in the surface which increases as film thickness decreases.