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Compositional Analysis of Complex Organic Mixtures by Electrospray Ionization Fourier Transform Ion Cyclotron Resonance Mass Spectrometry Zhigang Wu

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Compositional Analysis of Complex Organic Mixtures by Electrospray Ionization Fourier Transform Ion Cyclotron Resonance Mass Spectrometry Zhigang Wu Florida State University Libraries Electronic Theses, Treatises and Dissertations The Graduate School 2004 Compositional Analysis of Complex Organic Mixtures by Electrospray Ionization Fourier Transform Ion Cyclotron Resonance Mass Spectrometry Zhigang Wu Follow this and additional works at the FSU Digital Library. For more information, please contact [email protected] THE FLORIDA STATE UNIVERSITY COLLEGE OF ARTS AND SCIENCES Compositional Analysis of Complex Organic Mixtures by Electrospray Ionization Fourier Transform Ion Cyclotron Resonance Mass Spectrometry By Zhigang Wu A Dissertation submitted to the Department of Chemistry and Biochemistry in Partial Fulfillment of the Requirements for the Degree of Doctor of Philosophy Degree Awarded: Spring Semester, 2004 Copyright2004 Zhigang Wu All Rights Reserved The members of the Committee approve the Dissertation of Zhigang Wu Defended on April 7, 2004. Alan G. Marshall Professor Directing Dissertation William M. Landing Outside Committee Member William T. Cooper Committee Member Timothy A. Cross Committee Member Ryan P. Rodgers Committee Member The Office of Graduate Studies has verified and approved the above named committee members. ii To my parents, Xiaohua Wu and Shiping Cao; iii ACKNOWLEDGMENTS First, I need to thank Dr. Alan G. Marshall, my academic graduate advisor and supporter. His deep and broad academic knowledge and great personality are invaluable throughout my graduate career. His wise and forecasting advices has helped me directly cut to the “point” and inspired me to discover more underneath. I also wish to acknowledge Dr. Ryan P. Rodgers, my supervisor, for his expertise, direction, and support. His initiation and development in petroleum applications have led me to a broader and better understanding of this area. His immediate and inspiring direction made an easy and fun research for me. Our numerous discussions have strengthened every aspect of my research. I also would like to thank Dr. Christopher L. Hendrickson for his expertise in FT-ICR’s instrumental optimization. He was always at the first place when I needed instrumental help. His helpful direction and discussions have helped me a better understanding and utilization of the FT-ICR instrument. The author would also like to thank John P. Quinn and Daniel McIntosh for their technical and mechanical expertise, respectively. I would like to express my gratitude to the past (from Fall 1999) and current (to end of Spring 2004) members of the ICR Program at Florida State University for their professional, personal, and moral support. In particular: Chrisi Hughey, Kicki Håkansson, Ying Xiong, Melinda McFarland, Michael Chalmers, Jinmei Fu, Greg Blakney, and Mark Emmett. Work supported by NSF (CHE-99-09502), NIH (GM-31683, AI-44626), Florida State University, and the National High Magnetic Field Laboratory in Tallahassee, FL. iv TABLE OF CONTENTS LIST OF TABLES ............................................................................. x LIST OF FIGURES........................................................................... xi ABSTRACT .................................................................................... xx Chapter 1. Introduction to Mass Spectrometry and FT-ICR MS .............. 1 History of Mass Spectrometry....................................................... 1 FT-ICR MS ................................................................................... 5 Summary ................................................................................... 10 Chapter 2. Resolution of 10,000 Compositionally Distinct Components in Polar Coal Extracts by Negative-Ion Electrospray Ionization Fourier Transform Ion Cyclotron Resonance Mass Spectrometry ...................... 13 Introduction ............................................................................... 13 Experimental Methods................................................................ 16 Sample Preparation........................................................... 16 Mass Analysis................................................................... 16 Mass Calibration and Data Reduction ............................... 17 Results and Discussion .............................................................. 19 Kendrick Mass Analysis .................................................... 24 Heteroatomic Classes........................................................ 25 Alkylation Patterns ........................................................... 30 Type Analysis (Rings + Double Bonds)............................... 30 Conclusion................................................................................. 34 v Chapter 3. Detailed Compositional Analysis at Different Stages of Coal Liquefaction by Negative-Ion Electrospray Ionization Fourier Transform Ion Cyclotron Resonance Mass Spectrometry ....................................... 37 Introduction ............................................................................... 37 Experimental Methods................................................................ 39 Sample Preparation........................................................... 40 Results and Discussion .............................................................. 40 Kendrick Plot .................................................................... 40 Heteroatomic Classes........................................................ 46 Alkylation Patterns ........................................................... 46 Type Analysis (Rings + Double Bonds)............................... 47 Elemental Analysis ........................................................... 47 Conclusion................................................................................. 50 Chapter 4. Compositional Determination of Acidic Species in Illinois #6 Coal Extracts by Electrospray Ionization Fourier Transform Ion Cyclotron Resonance Mass Spectrometry............................................................. 54 Introduction ............................................................................... 54 Experimental Methods................................................................ 55 Isolation of Acid Fractions................................................. 55 Sample Preparation........................................................... 56 Mass Analysis................................................................... 56 Results and Discussion .............................................................. 57 Homologous Series and Compound Class.......................... 57 Comparison of Acid Fractions and Pyridine Extract........... 61 Compound Type and Carbon Distribution ......................... 61 Conclusion................................................................................. 68 vi Chapter 5. Two and Three Dimensional van Krevelen Diagrams: A Graphical Analysis Complementary to the Kendrick Mass Plot for Sorting Elemental Compositions of Complex Organic Mixtures Based on Ultrahigh-Resolution Broadband FT-ICR Mass Measurements ............. 69 Introduction ............................................................................... 69 Experimental Methods................................................................ 72 Sample Preparation........................................................... 72 Mass Calibration and Data Reduction ............................... 72 Results and Discussion .............................................................. 72 Elemental Compositions from a Plot of Kendrick Mass Defect vs. Kendrick Nominal Mass ............................................... 72 Sorting of Compound Classes by Use of a van Krevelen Diagram............................................................................ 73 Three Dimensional van Krevelen Diagram ......................... 77 Visual Comparisons between Various Fossil Fuels ............ 82 Conclusion .......................................................................................... 83 Chapter 6. Comparative Compositional Analysis of Untreated and Hydrotreated Oil by Electrospray Ionization Fourier Transform Ion Cyclotron Resonance Mass Spectrometry ............................................. 88 Introduction ............................................................................... 88 Experimental Methods................................................................ 90 Sample Preparation........................................................... 90 Mass Analysis................................................................... 90 Kendrick Mass and Data Reduction .................................. 90 Results and Discussion .............................................................. 90 Untreated Fuel.................................................................. 90 vii Species Removed or Generated by Hydrotreatment............ 91 Effect of Single-Stage Hydrotreatment on Aromaticity and Carbon Distribution.......................................................... 92 Effect of Two-Stage Hydrotreatment on Aromaticity and Carbon Distribution.......................................................... 99 Conclusion............................................................................... 100 Chapter 7. Composition of Explosives by Electrospray Ionization Fourier Transform Ion Cyclotron Resonance Mass Spectrometry .................... 104 Introduction ............................................................................. 104 Experimental Methods.............................................................. 106 Sample Preparation........................................................
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