The goal of this book was to explore the utility of mass spectrometry in the analysis of polymers. More specifically, it was to directly compare electrospray ionization (ESI) and matrix assisted laser desorption-ionization (MALDI) mass spectrometry with the more established method of 1H NMR in the study of polymer composition (monomer ratios) and structure (end group analysis). Mass spectral analysis of polymers is usually carried out by forming metal ion adducts of the oligomers. I wished to explore the impact this has on the mass spectral analysis. To this end I examined both how the conformation of such ionized polymer oligomers, and how changing the mode of ionization to protonation, affect the way they dissociate.