The objective of this project is research on and development of new mass spectral techniques in order to provide new and/or more rapid solutions to problems involving (1) chemical structure determination, (2) complex mixture analysis and (3) measurement of trace components in biological systems. The scope and utility of these mass spectral methods are evaluated, and a comparison to other types of analyses, both new and established, is carried out. Fast atom bombardment mass spectrometry and combined liquid chromatography-mass spectrometry are the techniques of current interest. Fast atom bombardment mass spectrometry in both the positive and negative ion mode continues to be applied for the rapid structure determination of nucleosides, nucleotides, natural products and synthetic intermediates and products. Reductive dehalogenation of nucleosides during fast atom bombardment ionization has been studied and correlated with analyte and matrix electron affinity. 3-Nitrobenzyl alcohol has been evaluated as a liquid matrix for the fast atom bombardment analysis of natural products, nucleosides and acylated lactones. Micro-column liquid chromatography is under investigation for direct combination with a continuous-flow fast atom bombardment ionization interface.