Cf‐252 particle desorption mass spectrometry (PDMS) has been applied to a series of industrial polymers. PDMS is a surface technique suited for analysis of polymers since 105 fission fragments impinging on the target are sufficient to obtain a mass spectrum, thus minimizing surface damage and charge‐up. Positive and negative ion spectra with masses up to m/z 400 amu were obtained for the following samples: polystyrene, poly(alpha methylstyrene), poly(ethylene terephthalate), poly(methyl methacrylate), and poly(butyl methacrylate). Polymers were studied in the form of solvent recuperated films or as self‐standing films. The mass spectra of positive and negative ions showed masses corresponding to different sized monomer fragments. For each polymer, its spectrum can be used as a fingerprint. The mass spectra were compared to those obtained by other mass spectrometric techniques.

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