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Surface layer matrix-assisted laser desorption ionization mass spectrometry imaging (SL-MALDI-MSI) is a powerful new surface sensitive imaging technique to establish surface component localization of multicomponent polymer materials. This study demonstrates the ability of SL-MALDI-MSI to image defects from foreign materials, material absence, mechanical scribing, and solvent perturbation at the surface of low-molecular-weight poly(methyl methacrylate) and polystyrene thin films. The surface specificity of the SL-MALDI-MSI technique is validated by imaging polystyrene on poly(methyl methacrylate) bilayer films; only polystyrene ions are detected from the surface of the unperturbed polystyrene layer. A key process enabling SL-MALDI-MSI is the solvent-free sublimation of matrix and salt uniformly on the sample's surface.