This project is in the general area of analytical and surface chemistry and in the subfield of mass spectrometry. The objectives of this research are the development of new instrumentation and methodologies with which the peptide sequences of biopolymers at the picomole level can be determined. By combining fast atom and ion bombardment techniques for sample ionization with tandem quadrupole Fourier transform detection of fragment ions, Professor Hunt has, during the tenure of NSF grant CHE-8319728, developed a prototype mass spectrometer with which the high resolution characterization of polymeric ions with masses ranging up to 13,000 Daltons has been demonstrated. The current project renews those efforts and has as its primary target the optimization of this new instrument which should enable the sequence analysis of biopolymers of up to 50,000 Daltons. New concepts in mass spectrometer instrumentation are expected to ensue from this research project. These advances in instrument and technique development could provide unprecedented analytical capability for the characterization of trace quantities of polymeric materials and impact broadly and positively in biotechnology and materials chemistry.