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Title: Production and analysis of beams of synthetic polymers by mass spectrometry
Author: Varney, Julie Elizabeth
ISNI:       0000 0001 3542 9059
Awarding Body: University of Warwick
Current Institution: University of Warwick
Date of Award: 1997
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The conditions under which poly(styrene) standards up to m/z = 12 000 can be analysed by matrix-assisted laser desorption/ionisation (MALDI) have been optimised using 9-nitroanthracene as the matrix material in conjunction with silver tri- fluoroacetate addition. The development of such conditions permitted the analysis of a range of polymeric materials including poly(sulfide) samples and novel poly(isobutylene)samples containing aromatic ring functions of molecular masses up to 1000 Da. A series of calculations were carried out in order to assess the accuracy of molecular mass statistics for a range of PMMA and poly( styrene) standards of low poly(dispersity) values up to masses of 12 000 Da obtained by MALDI. It was found that data obtained were in good agreement with those derived from size exclusion chromatography measurements. Electrospray sample preparation was investigated as a method of increasing reproducibilities and signal-to-noise values in MALDI experiments. Electrospraying low mass poly(styrene) samples (up to 3000 Da) increased intensities, however, higher mass samples could not be detected using this method. Moreover, the traditional spotting method worked much better at higher masses. Post-source decay (PSD) experiments have been performed on poly(ethylene glycol), poly( styrene) and the novel poly(isobutylene) samples previously investigated by MALDI using instruments fitted with curved-field and two-stage reflectrons. The type of information obtained using this method compared with tandem mass spectrometry techniques has been investigated. The effect of laser power and pressure has been studied. Ions formed by PSD processes were found to be the same as those formed by low energy CID processes. A range of standard peptide residues were also investigated as part of this work to highlight calibration difficulties associated with PSD analysis using a curved field reflectron. Emitter activation and field desorption mass spectrometry experiments were attempted in order to study polymer materials with little success. Problems and difficulties associated with these experiments have briefly been described.
Supervisor: Not available Sponsor: British Petroleum Company
Qualification Name: Thesis (Ph.D.) Qualification Level: Doctoral
EThOS ID:  DOI: Not available
Keywords: TP Chemical technology