A direct current glow discharge mass spectrometer has been used for a novel application, the sputtering and subsequent analysis of polymers. This was made possible by the application of a secondary cathode, a tantalum diaphragm placed in front of the nonconducting sample. Different types of polymers were measured (polytetrafluoroethylene, polycarbonate, and poly(vinyl chloride)). Important to note is that the mass spectra obtained are predominantly characterized as atomic, a major difference from the radio frequency GDMS spectra of polymers reported earlier. This facilitates quantitative elemental analysis for several reasons.