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This work details an application of collinear resonance ionization spectroscopy for the separation of short-lived isomeric states and their subsequent study with decay spectroscopy. It reports the successful construction of a novel decay spectroscopy apparatus that can operate at pressures below 1 x 10^-9 mbar. The method is demonstrated by separating the nuclear ground and isomeric states of 204Fr and performing alpha-decay spectroscopy. An equivalent mass spectrometer would require 4.6 million times as much resolution to achieve the same result. This work unambiguously confirms the existence of a second isomeric state in 204Fr. The author also demonstrates the effectiveness of this method for laser spectroscopy and identification of hyperfine-structure components with energy tagging. This method was successfully used in 202Fr to identify ground and isomeric states. The measurement of 202Fr reported in this thesis demonstrates a factor of 100 improvement in sensitivity compared to state-of-the-art fluorescence techniques. The work reported in this thesis won the author the IOP Nuclear Physics Group Early Career Prize.

Physics. --- Nuclear Physics, Heavy Ions, Hadrons. --- Spectroscopy and Microscopy. --- Nuclear physics. --- Physique --- Physique nucléaire --- Heavy ions. --- Plasma spectroscopy. --- Spectrum analysis. --- Thorium -- Spectra. --- Physics --- Physical Sciences & Mathematics --- Electricity & Magnetism --- Nuclear Physics --- Laser spectroscopy. --- Hadrons. --- Spectroscopy. --- Microscopy. --- Spectrum analysis --- Atomic nuclei --- Atoms, Nuclei of --- Nucleus of the atom --- Analysis, Microscopic --- Light microscopy --- Micrographic analysis --- Microscope and microscopy --- Microscopic analysis --- Optical microscopy --- Optics --- Analysis, Spectrum --- Spectra --- Spectrochemical analysis --- Spectrochemistry --- Spectrometry --- Spectroscopy --- Chemistry, Analytic --- Interferometry --- Radiation --- Wave-motion, Theory of --- Absorption spectra --- Light --- Spectroscope --- Ions --- Qualitative --- Analytical chemistry