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A conversion electron and low energy gamma-ray spectrometer has been developed using a silicon lithium-drifted semiconductor detector. The spectrometer has a resolution of 2 Kev for 100 Kev electrons and photons under optimum conditions. The energies of these electrons and gamma-rays can be estimated to ±.1 Kev, and their intensities to within ±6% with the standard sources available. The electron capture decay of ¹⁵³Gd → ¹⁵³Eu was investigated using this spectrometer. The branching capture ratios to the 172.9 Kev, 103.2 Kev, 97.4 Kev, and 0 Kev levels of ¹⁵³Eu were found to be 11%, 39%, 39% and 11%, respectively. Possible Jπ values of ⁵ ̸₂ + or ³ ̸₂ + for the 172.9 Kev level, ⁵ ̸₂ + or ³ ̸₂ + for the 103.2 Kev level, and ³ ̸₂ -, ⁵ ̸₂ -, or ⁷ ̸₂ - for the 97.4 Kev level have been assigned. These values are in agreement with those found by other investigators. / Science, Faculty of / Physics and Astronomy, Department of / Graduate

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Digitized by Kansas Correctional Industries

Wong, Pui Shuen. / Thesis (M.Phil.)--Chinese University of Hong Kong, 2011. / Includes bibliographical references (leaves 92-96). / Abstracts in English and Chinese. / Title Page --- p.i / Abstract (English) --- p.ii / Abstract (Chinese) --- p.iii / Acknowledgements --- p.iv / Table of Contents --- p.V / List of Tables --- p.viii / List of Figures --- p.ix / List of Schemes --- p.xi / Symbols and Abbreviations --- p.xii / Dedication --- p.xiv / Chapter Chapter 1 --- Introduction / Chapter 1.1 --- Mass Spectrometry of peptides/ proteins --- p.1 / Chapter 1.1.1 --- Electrospray ionization of peptides/ proteins --- p.3 / Chapter 1.2 --- Tandem mass spectrometry of peptides/ proteins --- p.4 / Chapter 1.2.1 --- Nomenclature of peptide fragment ions --- p.5 / Chapter 1.2.2 --- Slow heating methods for MSn --- p.6 / Chapter 1.2.2.1 --- Collision induced dissociation --- p.7 / Chapter 1.2.3 --- "Electron based ion activation for MS""" --- p.8 / Chapter 1.3 --- Electron Capture Dissociation --- p.9 / Chapter 1.3.1 --- ECD mechanism for protonated peptide ions --- p.10 / Chapter 1.3.2 --- ECD efficiency --- p.12 / Chapter 1.3.3 --- ECD of metal ions-adducted peptide --- p.13 / Chapter 1.4 --- Overview of present work --- p.14 / Chapter Chapter 2 --- "Instrumentation, Experimental and Calculations" / Chapter 2.1 --- Fourier-transform Ion Cyclotron Resonance Mass Spectrometer --- p.15 / Chapter 2.1.1 --- Basic principle of FTICR-MS --- p.15 / Chapter 2.1.2 --- The instrument --- p.19 / Chapter 2.1.2.1 --- Vacuum system --- p.19 / Chapter 2.1.2.2 --- Nanospray source --- p.24 / Chapter 2.1.2.3 --- Electrostatic ion focusing system --- p.26 / Chapter 2.1.2.4 --- Infinity´ёØ Cell --- p.28 / Chapter 2.1.2.5 --- Electron emission source --- p.29 / Chapter 2.1.2.6 --- Data acquisition system --- p.31 / Chapter 2.2 --- Experimental --- p.31 / Chapter 2.2.1 --- Acquisition pulse program --- p.31 / Chapter 2.2.1.1 --- Simple ESI acquisition pulse program (MS experiment) --- p.31 / Chapter 2.2.1.2 --- ESI-ECD acquisition pulse program (MS experiment) --- p.34 / Chapter 2.2.2 --- Molecular mechanics calculation --- p.36 / Chapter Chapter 3 --- Structural Parameters Affecting Suppression of N-Ca Cleavages of Peptides Ions after Electron Capture / Chapter 3.1 --- Introduction --- p.37 / Chapter 3.2 --- Experimental section --- p.39 / Chapter 3.3 --- Results and Discussion --- p.40 / Chapter 3.3.1 --- Peptides with three arginine residues --- p.40 / Chapter 3.3.1.1 --- General ECD mass spectra features --- p.40 / Chapter 3.3.1.2 --- Comparison of the extent of suppression of triariginated and diarginated model peptides ions --- p.46 / Chapter 3.3.2 --- Peptides with histidine and lysine as proton carriers --- p.47 / Chapter 3.3.2.1 --- General features of ECD mass spectra --- p.47 / Chapter 3.3.2.2 --- Comparison of ECD behavior of peptide ions with different proton carrier --- p.50 / Chapter 3.3.3 --- Peptides with various chain length --- p.53 / Chapter 3.3.3.1 --- General ECD mass spectra features --- p.53 / Chapter 3.3.3.2 --- Reactivation of [M+2H]+* by collision activation --- p.57 / Chapter 3.3.3.3 --- Significance of glutamic acid residues --- p.57 / Chapter 3.3.3.4 --- Results of conformational searches --- p.60 / Chapter 3.4 --- Conclusions --- p.64 / Chapter Chapter 4 --- Investigation of the Role of Conformation of Peptide Ions in Suppression of Backbone fragmentation / Chapter 4.1 --- Introduction --- p.67 / Chapter 4.2 --- Experimental section --- p.69 / Chapter 4.3 --- Results and Discussion --- p.70 / Chapter 4.3.1 --- Peptide with N-methylated amino acid residues --- p.70 / Chapter 4.3.1.1 --- General features of ECD mass spectra --- p.70 / Chapter 4.3.1.2 --- Comparison between normal and N-methylated peptide ions under ECD --- p.72 / Chapter 4.3.2 --- Peptides with proline residues vi --- p.73 / Chapter 4.3.2.1 --- General ECD mass spectra features --- p.73 / Chapter 4.3.2.2 --- Comparison of ECD of peptide ions with and without proline residues --- p.76 / Chapter 4.3.3 --- Transition metal ions as charge carriers --- p.80 / Chapter 4.3.3.1 --- General ECD mass spectra features --- p.80 / Chapter 4.3.3.2 --- Comparison of ECD behavior using proton and metal ions as charge carrier --- p.85 / Chapter 4.4 --- Conclusions --- p.87 / Chapter Chapter 5 --- Conclusions --- p.90 / References --- p.92 / Chapter Appendix I --- Twenty common amino acids --- p.97 / Chapter Appendix II --- Pulse programs for MS and MSn experiments --- p.98

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Ip Wai-Ho Herman. / Thesis (M.Phil.)--Chinese University of Hong Kong, 2003. / Includes bibliographical references (leaves 87-90). / Abstracts in English and Chinese. / Abstract (English) --- p.ii / Abstract (Chinese) --- p.iii / Acknowledgement --- p.iv / Declaration --- p.v / Table of Content --- p.vi / List of Tables --- p.ix / List of Figures --- p.x / Chapter 1 --- INTRODUCTION --- p.1 / Chapter 1.1 --- Fourier transform ion cyclotron resonance mass spectrometry (FRICR) --- p.2 / Chapter 1.1.1 --- History of FTICR --- p.2 / Chapter 1.1.2 --- Theory of FTICR --- p.4 / Chapter 1.1.3 --- FTICR with electrospray ionization source --- p.10 / Chapter 1.2 --- Tandem mass spectrometry --- p.11 / Chapter 1.2.1 --- Introduction --- p.11 / Chapter 1.2.2 --- Collision-induced dissociation --- p.12 / Chapter 1.2.3 --- Surface-induced dissociation --- p.12 / Chapter 1.2.4 --- Photodissociation --- p.13 / Chapter 1.2.5 --- Blackbody infrared radiative dissociation (BIRD) --- p.13 / Chapter 1.3 --- Electron capture dissociation --- p.13 / Chapter 1.4 --- Recent advances in ECD experiments --- p.15 / Chapter 1.5 --- Outline the present work --- p.17 / Chapter 2. --- EXPERIMENTAL AND INSTRUMENTATION --- p.18 / Chapter 2.1 --- Instrumentation --- p.19 / Chapter 2.1.1 --- Fourier-transform ion cyclotron resonance mass spectrometer --- p.19 / Chapter 2.1.2 --- Vacuum system --- p.19 / Chapter 2.1.3 --- Electrospray ionization source --- p.23 / Chapter 2.1.4 --- Electrostatic ion focusing system --- p.26 / Chapter 2.1.5 --- Infinity cell --- p.28 / Chapter 2.1.6 --- Electron emission source --- p.29 / Chapter 2.1.7 --- Data acquisition system --- p.32 / Chapter 2.2 --- Experimental --- p.32 / Chapter 2.2.1 --- Simple acquisition pulse program --- p.32 / Chapter 2.2.2 --- ECD pulse program with/without collision cooling --- p.35 / Chapter 3. --- OPTIMIZATION OF EXPERIMENTAL PARAMETERS FOR ELECTRON CAPTURE DISSOCIATION --- p.38 / Chapter 3.1 --- Introduction --- p.39 / Chapter 3.2 --- Experimental --- p.40 / Chapter 3.2.1 --- Materials --- p.40 / Chapter 3.2.2 --- Sample preparation --- p.41 / Chapter 3.2.3 --- Instrumentation --- p.41 / Chapter 3.3 --- Results and discussion --- p.42 / Chapter 3.3.1 --- Benchmark conditions --- p.42 / Chapter 3.3.2 --- Effect of the filament heating currents (If) --- p.45 / Chapter 3.3.3 --- Effect of the average filament bias voltages (Vf) --- p.49 / Chapter 3.3.4 --- Effect of the electron irradiation time (te) --- p.53 / Chapter 3.3.5 --- Reduction of the fragment ions intensity --- p.56 / Chapter 3.3.6 --- Effect of the trapping potentials --- p.60 / Chapter 3.4 --- Conclusions --- p.62 / Chapter 4. --- ENHANCEMENT ON ELECTRON CAPTURE DISSOCIATION EFFICIENCY --- p.63 / Chapter 4.1 --- Introduction --- p.64 / Chapter 4.2 --- Experimental --- p.65 / Chapter 4.2.1 --- Materials --- p.65 / Chapter 4.2.2 --- Sample preparation --- p.65 / Chapter 4.2.3 --- Instrumentation --- p.65 / Chapter 4.3 --- Results and discussion --- p.66 / Chapter 4.3.1 --- Effect of the filament position --- p.66 / Chapter 4.3.2 --- Effect of the collision gas pressure --- p.68 / Chapter 4.3.3 --- Effect of the collision gas --- p.73 / Chapter 4.3.4 --- Effect of the electron irradiation at different pulse gas interval --- p.75 / Chapter 4.3.5 --- Effect of the multiple electron irradiation --- p.76 / Chapter 4.3.6 --- Optimized Conditions --- p.79 / Chapter 4.4 --- Conclusions --- p.84 / Chapter 5. --- CONCLUSIONS --- p.85 / Chapter 5.1 --- Conclusions --- p.86 / REFERENCES --- p.87 / APPENDIX --- p.91 / Appendix A Simple pulse sequence program for ESI FTICR-MS experiments --- p.91 / Appendix B Pulse sequence program for ESI FTICR-MS electron capture dissociation --- p.95 / Appendix C Pulse sequence program for ESI FTICR-MS electron capture dissociation experiments with collision cooling --- p.99 / Appendix D Modified pulse sequence program for ESI FTICR-MS electron capture dissociation experiments with a time lag between collision cooling and electron irradiation. --- p.104 / Appendix E Modified pulse sequence program for ESI FTICR-MS electron capture dissociation experiments with multiple irradiation --- p.109

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