The comparison of three surface analytlcal tools, static secondary Ion mass spectralmetry (SIMS), ion scatterlng spectroscopy (ISS), and X-ray photoelectron spectroscopy (XPS or ESCA), Is presented. Information avallable from ISS and ESCA is Illustrated by comparing plots ol carbon/oxygen Intensity ratio vs. monomer composition for both methods. Both ESCA and ISS yield linear correlations, ESCA having the higher correlation coefficient. The ISS plot had some devlatlons whlch could not be explained by steric effects alone. Statlc SIMS results were interpreted by uslng a "backbone/slde chain" model of polymer structure which explains ions generated from bond breaking along the hydrocarbon backbone and the pendant side chain functlonality which Is varled in the polymer serles of poly( methacrylates). Posltlve Ion spectral patlerns are Interpreted for shorl chain alkyl, Isomeric butyl, and cyclic and long chain alkyl functlonallties.The chemical analysis of polymer surfaces has provided a fruitful realm for the application of X-ray photoelectron spectroscopy (XPS or ESCA) (1,2). ESCA is now well-known for the unique qualitative and quantitative surface information derived from core and valence level spectra. However, when utilized alone, ESCA has some major weaknesses. We have been active in the extenaiion of surface analysis of polymers by ion beam methods: secondary ion mass spectrometry (SIMS) and ion scattering spectroscopy (ISS) (3-5). In the present paper we will coimpare the analytical capabilities of ISS and SIMS in the so-cdled "static" m d e (Le., low primary ion energies and current densities) with ESCA for the analysis of poly(methacrylates) where the pendant ester group is varied in both length and functionality.Static SIMS analysis of organics has been furthered by the use of a cooled probe technique to analyze frozen liquids. These substances have yielded a varieity of SIMS results. Ions assigned to peaks in the low mass range (0-100 amu) were explained by simple fragmentation of' molecules (bond breaking) as the dominant mechanism (6, 7), with rearrangement ("polymerization") (6) occurring after i9 long bombardment time. High mass results (0-1000 amu) indicated cluster ion formation, with significant rearrangement, could explain most spectral features (8). Since relative intensities of high mass cluster ions decreased logarithmically, it is possible that the peaks cannot be seen under typical detection conditions employed in t hLe low mass studies. Thus it appears that spectral results for the low mass range from 0 to 200 m u , employed in this study, will be dominated by ions directly related to the structure of organic molecules from bond breaking (4, 7) with low intensity rearrangement phenomena accounting for high mass molecular ions. The use of "destructive" methods of analysis like ISS and SIMS requires consideration of the effects on the sample integrity of the method itself. The analysis conditions described (4) were chosen because of indications that moderate to high primary ion beam energies...