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Mass spectrometry MS is a technique widely implemented for the measurement of environmental pollutants. The aim of this thesis was to investigate the use of alternative MS-based techniques to assist specific analytical challenges including separation of stereoisomers using supercritical fluid chromatography SFCreduced ionization competition with appropriate mobile phase additives, and applied rotationally averaged collision-cross section CCS of ions via ion mobility measurements of emerging POPs. Chromatographic efficiency improvements for the brominated flame retardant, hexabromocyclododecane HBCDDwere implemented through the development of two supercritical fluid chromatography SFC methods. Based on the inherent qualities of supercritical fluids, separation of both predominant diastereomers and respective enantiomers was performed in a shorter time with wider chromatographic resolution using SFC than existing LC methods. Following a survey of analytical methodologies for HFPO-DA, the challenge of extreme dimer formation, in-source fragmentation and very low [M-H]- production was described.

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