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Synthetic polymers have physical and chemical properties that are directly related to their molecular weight distributions, their component monomer species, and the identity of their initiating and terminating groups. These properties are all a function of the molecular mass of the individual oligomers in the polymer distribution. Matrix assisted laser desorption/ionization (MALDI) mass spectrometry facilitates the analysis of these properties by providing singly charged, gas phase species for measurement while Fourier transform ion cyclotron resonance (FTICR) as a mass analyzer can yield the mass resolution necessary for assigning the components of complicated mixtures. This dissertation details recent improvements to the techniques for analyzing polymers by MALDI-FTICR-MS; specifically, methods for increasing mass accuracy, sensitivity with low abundance and weakly ionizing samples, and resolution of isobaric species are presented.

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