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Fundamental Studies and Applications of Ambient Plasma Ionization Sources for Mass Spectrometry Wade C

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Fundamental Studies and Applications of Ambient Plasma Ionization Sources for Mass Spectrometry Wade C Brigham Young University BYU ScholarsArchive All Theses and Dissertations 2017-07-01 Fundamental Studies and Applications of Ambient Plasma Ionization Sources for Mass Spectrometry Wade C. Ellis Brigham Young University Follow this and additional works at: https://scholarsarchive.byu.edu/etd Part of the Chemistry Commons BYU ScholarsArchive Citation Ellis, Wade C., "Fundamental Studies and Applications of Ambient Plasma Ionization Sources for Mass Spectrometry" (2017). All Theses and Dissertations. 6484. https://scholarsarchive.byu.edu/etd/6484 This Dissertation is brought to you for free and open access by BYU ScholarsArchive. It has been accepted for inclusion in All Theses and Dissertations by an authorized administrator of BYU ScholarsArchive. For more information, please contact [email protected], [email protected]. Fundamental Studies and Applications of Ambient Plasma Ionization Sources for Mass Spectrometry Wade C. Ellis A dissertation submitted to the faculty of Brigham Young University in partial fulfillment of the requirements for the degree of Doctor of Philosophy Paul Burton Farnsworth, Chair Daniel E. Austin David V. Dearden Jaron C. Hansen Eric T. Sevy Department of Chemistry and Biochemistry Brigham Young University Copyright © 2017 Wade C. Ellis All Rights Reserved ABSTRACT Fundamental Studies and Applications of Ambient Plasma Ionization Sources for Mass Spectrometry Wade C. Ellis Department of Chemistry and Biochemistry, BYU Doctor of Philosophy The field of ambient desorption/ionization mass spectrometry (ADI-MS) has existed for over a decade. ADI-MS is a technique that offers benefits including fast analysis time, simple ionization sources that are easily constructed, and little to no required sample preparation. The research presented here describes efforts to better understand plasma-based ADI-MS sources and to explore the use of hydrogen-doped plasma gases with these sources. The use of hydrogen- doped argon (H2/Ar) and hydrogen-doped helium (H2/He) as plasma gases for a dielectric barrier discharge (DBD) and an AC glow discharge is presented first. When using the DBD, the intensity of the signal obtained when analyzing organic molecules in positive ion mode was increased by factors up to 37 times. In negative ion mode, only H2/Ar was shown to enhance the signal of an organic analyte. The limits of detection for caffeine when using hydrogen-doped plasma gases were found to decrease by factors of 78 and 1.9 for H2/Ar and H2/He respectively. The same phenomenon was observed when using H2/Ar with the AC discharge, but no signal enhancement was observed when using hydrogen-doped helium with the AC discharge. Similarly, if the DBD was allowed to ground through a wire rather than through the air, no signal enhancement was observed for H2/He. Using H2/Ar with metal samples is presented second. By using the metal sample as the grounded electrode for the AC glow discharge, many different metals could be detected directly with a time-of-flight mass spectrometer (TOF-MS) in the form of atomic ions both on their own and in combination with water and ammonia from the discharge. Any refractory metals tested did not yield signal. In addition to direct analysis with a TOF-MS, the AC discharge was used as a sampling method for an inductively coupled plasma mass spectrometer (ICP-MS). When coupled with an ICP-MS, the AC glow discharge was found capable of sampling even refractory elements, though the power of the ICP was required for ionization and detection. Scanning electron microscope (SEM) images of a copper surface exposed to the plasma discharge showed signs of melting when using the H2/Ar. Finally, a computer simulation of the chemistry and flow dynamics of a DC glow discharge generated in helium is presented. The simulation explores many of the fundamental processes at work and how they depend on the composition of the plasma gas. The generation of important species in the plasma was found to depend more on the amount of N2 and H2O impurities in the plasma gas rather than on the humidity or air pressure. Keywords: ambient desorption/ionization, mass spectrometry, inductively coupled plasma, glow discharge, dielectric barrier discharge, hydrogen doping, computer simulation, metal sampling ACKNOWLEDGEMENTS I gratefully acknowledge the mentorship of my advisor, Paul Farnsworth, as well as the support of my coworkers in the Farnsworth Lab. I thank the members of my graduate committee for their time and attention. I thank Ross Spencer for the many hours he spent helping in the development of the computer simulation that I describe in this work. I especially thank my wife, Terra, for her support and encouragement throughout my education. Funding for the research described in this dissertation was provided principally by the Department of Chemistry and Biochemistry at Brigham Young University. My personal financial support was provided through two fellowships. For the first three years of my graduate work, I was a recipient of the High Impact Doctoral Research Assistantship administered by Graduate Studies at BYU. For my last year of study, I was awarded the Charles E. and Margaret P. Maw Fellowship by the Department of Chemistry and Biochemistry at BYU. These invaluable sources of support have made getting my education possible in an expedited time frame. TABLE OF CONTENTS ABSTRACT .................................................................................................................................... ii ACKNOWLEDGEMENTS ........................................................................................................... iii TABLE OF CONTENTS ............................................................................................................... iv LIST OF TABLES ........................................................................................................................ vii LIST OF FIGURES ..................................................................................................................... viii 1 Introduction ............................................................................................................................. 1 Chemical Analysis Using Ambient Plasma Discharges ................................................... 1 1.1.1 Ambient Desorption/Ionization ................................................................................ 1 1.1.1.1 Solvent Based Ambient Desorption/Ionization ..................................................... 1 1.1.1.2 Plasma Based Ambient Desorption/Ionization Sources ........................................ 3 1.1.1.2.1 Direct Analysis in Real Time ................................................................................ 3 1.1.1.2.2 Flowing Atmospheric Pressure Afterglow ............................................................ 4 1.1.1.2.3 Dielectric Barrier Discharges ................................................................................ 5 1.1.1.2.4 Other Plasma Based ADI Sources ......................................................................... 5 1.1.2 Characterization of Plasma Based ADI Sources ....................................................... 6 1.1.2.1 Optical Spectroscopic Characterization ................................................................ 7 1.1.2.2 Mass Spectrometric Characterization .................................................................. 13 1.1.2.3 Computational Characterization .......................................................................... 16 Elemental Analysis Using Plasma Discharges ............................................................... 18 1.2.1 Inductively Coupled Plasma ................................................................................... 19 1.2.2 Glow Discharges ..................................................................................................... 20 1.2.3 Laser Induced Breakdown Spectroscopy ................................................................ 20 1.2.4 Solution Cathode Glow Discharges ........................................................................ 21 My Research Focus ........................................................................................................ 22 References ...................................................................................................................... 22 2 The Effects of Added Hydrogen on Ambient Helium and Argon Discharges Used for Mass Spectrometry ................................................................................................................................. 27 Using Hydrogen Doped Plasma Gases in ADI-MS ....................................................... 27 Experimental Setup ........................................................................................................ 29 2.2.1 Chemicals Tested .................................................................................................... 29 2.2.2 Discharge Sources ................................................................................................... 29 iv 2.2.3 Mass Spectrometer Setup ........................................................................................ 31 Signal Enhancement with Added Hydrogen .................................................................. 33 2.3.1 Optimal Amount of Hydrogen in Argon ................................................................. 33 2.3.2 Coated Slides .........................................................................................................
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