The degree and nature of polymer degradation that occurs in the high temperature microshell formation process developed at the Lebedev Physical Institute has been examined experimentally. We find that significant mass degradation occurs during the final stages of shell formation. This manifests itself both in terms of mass loss and molecular weight degradation as measured by gel permeation chromatography. This decrease in the molecular weight may be in part responsible for the relatively fragile nature of the shells produced by this high temperature process.