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Development and Characterization of Plasma-Based Sources for Ambient Desorption/Ionization Mass Spectrometry

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Development and Characterization of Plasma-Based Sources for Ambient Desorption/Ionization Mass Spectrometry DEVELOPMENT AND CHARACTERIZATION OF PLASMA-BASED SOURCES FOR AMBIENT DESORPTION/IONIZATION MASS SPECTROMETRY Jacob T. Shelley Submitted to the faculty of the University Graduate School in partial fulfillment of the requirements for the degree Doctor of Philosophy in the Department of Chemistry Indiana University June, 2011 Accepted by the Graduate Faculty, Indiana University, in partial fulfillment of the requirements for the degree of Doctor of Philosophy. Doctoral Committee Gary M. Hieftje, Ph.D. Dennis G. Peters, Ph.D. Stephen C. Jacobson, Ph.D. Bogdan Dragnea, Ph.D. Date of Oral Examination May 31, 2011 ii © 2011 Jacob T. Shelley ALL RIGHTS RESERVED iii Acknowledgements The work presented hereafter would not have been possible without the motivation, guidance, and support of numerous people, both personally and professionally. I am forever indebted to these people for helping me grow as a scientist and as a person. I would first like to thank my parents, Fred and Mindy, and my brother, Keith, for all the love and support they have provided throughout my life. It is comforting to know that no matter how difficult or trying life is, I can always turn to these three people. I would certainly not have made it this far without them. The ever optimistic and encouraging attitude provided by my grandparents, Fred and Lilly Shelley as well as Jane and the late Chuck Baldridge, has always given me motivation and put a smile on my face. I am extremely thankful to my aunt and uncle, Allie and Jerry Hoskins, for providing a home away from home in Phoenix during my undergraduate and graduate studies. I have also been lucky enough to have some truly amazing friends in my life that have provided sanity as well as open ears and hearts during the many difficult times over the past six years. On the top of the list are my classmates Dr. Matt Foley, Soca “Danger” Wibowo, and Nichole Stewart as well as lifelong comrade Brian Spall. Professionally, I owe everything I am and will become as a scientist to my research advisor, Prof. Gary M. Hieftje. He certainly deserves thanks for providing the support and the means to perform this research and earn this degree. But more iv importantly, he has provided me, and the rest of his research group, with a wealth of freedom, opportunities, and experiences that would have not have been had in any other setting. His love of science and education has created a research group that more closely resembles a family. Through this family atmosphere I have made some lifelong friends and colleagues; in particular Dr. Greg Schilling, Josh Wiley, Dr. Carsten Engelhard and the whole Bioiononics Bowling team. In addition to them, I have had the privilege and honor to have great post-doctoral mentors throughout the years in Dr. George Chan, Dr. Steve Ray, and Dr. Francisco Andrade. Their passion for science and knowledge is on par with Prof. Hieftje and I am excited to see the superb work to come from them in the future. I also have to thank the rest of the past and present Hieftje “family” that has made graduate school so much fun: Prof. José Broekaert, Yan Cheung, Elise Dennis, Dr. Eyal Elish, Jeremy Felton, Dr. Gerardo Gamez, Ana Gonzalvez, Alex Graham, Meghan McCormick, Kevin Pfeuffer, Dr. Radislav Potyrailo, Dr. Duane Rogers, Arnon Rubinshtein, Andy Schwartz, Dan Shelby, Andrew Storey, Dr. Mike Webb, Dr. Bill Wetzel, Cori Weinel, Prof. Zhenli Zhu, and, surrogate group member from Prosolia Inc., Dr. Justin Wiseman. Last but not least, many things would not have been accomplished without the administrative assistance of LeeAnn Mobley, Selina Williams, Misty Boteler, and Susan Hieftje. There are several other support groups at Indiana University that deserve special thanks. These include Gary Fleener, Brian Ferguson, Doug Garvin, Rick Moore, and Bruce Frye in the Edward J. Bair Mechanical Instrument Services; John Poehlman and Andy Alexander in the Electrical Instrument Services group; Susie DuMond, Jackie Drake, and Rick Hackler in the Requisitioning office and Chemical Storeroom. v During my time in graduate school I was also fortunate enough to spend half a year doing work in the research group of Prof. R. Graham Cooks at Purdue University through the Center for Analytical Instrumentation Development Fellowship. It certainly is an experience I will never forget. It also led to one of the most productive and fun collaborations I have ever been a part of with Dr. Carsten Engelhard, Dr. George Chan, and myself from Indiana and Dr. Ayanna Jackson and Josh Wiley from Purdue; some of that work is presented below. In addition to the insightful conversations with Prof. Cooks, I must thank Dr. Ewa Sokol, Dr. Fatkhulla Tadjimukhamedov, Dr. Rob Noll, Dr. Demian Ifa, and Paul Hendricks from Aston Labs for sharing their wealth of knowledge on mass spectrometry and giving me a new perspective on scientific research. I would not have pursued chemistry without the teachings and guidance of my high school chemistry teachers, Dr. Meg Cox and the late David Thurston. They showed me how exciting and rewarding science can be. I would not have made it into graduate school or even applied to Indiana University without the urgings of Dr. Chris Hassell, Dr. Cris Lewis, and Dr. James Barnes during my time at Los Alamos National Laboratory. In addition, Dr. Srinivas Iyer and Dr. Andy Koppisch from the Bioscience Division of Los Alamos National Laboratory and Prof. Diane Stearns at Northern Arizona University gave me my first opportunities to pursue scientific research and let me so with almost total freedom. These projects were supported by Award Number 1R41RR025718 from the National Center for Research Resources (NCRR) in collaboration with Prosolia, Inc., Indianapolis, IN. The content is solely the responsibility of the authors and does not necessarily represent the official views of the NCRR or the NIH. vi Additional funding was provided by NSWC Crane through federal grant number N00164-08-C-JQ11, the US Department of Energy through federal grant number DE- FG02-98ER14890, the Lilly Endowment-Indiana MetaCyt Initiative, by the Department of Homeland Security through grant HSHQDC-09-9-00008, and by the Center for Analytical Instrumentation Development at Purdue University. The authors would also like to thank Leco, Horiba Jobin-Yvon, and Prosolia for the loan of equipment used in these studies. vii DEVELOPMENT AND CHARACTERIZATION OF PLASMA-BASED SOURCES FOR AMBIENT DESORPTION/IONIZATION MASS SPECTROMETRY Jacob T. Shelley A number of atmospheric-pressure ionization sources for mass spectrometry has recently appeared in the literature to yield a field that is collectively referred to as Ambient Desorption/Ionization-Mass Spectrometry (ADI-MS). These sources include, among others, Desorption ElectroSpray Ionization (DESI), Direct Analysis in Real Time (DART), the Flowing Atmospheric-Pressure Afterglow (FAPA), and the Low- Temperature Plasma (LTP) probe. Collectively, these ADI-MS sources offer numerous advantages over conventional ionization sources, including direct analysis of solid, liquid, and gaseous samples, high ionization efficiency, and soft ionization. Additionally, their ability to analyze samples directly with no pretreatment dramatically reduces analysis times. The ultimate ambient ionization source would be one that is capable of desorbing and ionizing a broad range of analytes (polar, non-polar, small molecules, biopolymers, etc.) while being minimally influenced by matrix effects. While the plasma-based ADI-MS sources, such as FAPA, DART, and LTP, have been shown to be capable of efficiently ionizing a range of small molecules, few investigations have been aimed at understanding desorption and ionization processes or matrix effects that occur with them. At present, the performance and fundamental characteristics of the FAPA source, developed in our research group, and the LTP probe, developed at Purdue University, are being evaluated through optical and mass-spectrometric methods. The FAPA source consists of a direct-current, atmospheric-pressure glow discharge in a pin-to-plate configuration. A hole in the plate allows ionized and excited plasma species to interact directly with a sample, while physically and electrically isolating the discharge from the sample-introduction region. Conversely, the LTP probe is a high-voltage, alternating- current, dielectric-barrier discharge that interacts directly with a sample. While the viii fundamental processes governing these discharges are quite different, mass spectra produced with both sources are very similar. The major differences are in achievable detection limits and susceptibility to matrix effects, with the FAPA sources routinely performing better. Direct, fundamental comparisons among the FAPA source, the LTP probe, and DART are made. Gary M. Hieftje, Ph.D. Dennis G. Peters, Ph.D. Stephen C. Jacobson, Ph.D. Bogdan Dragnea, Ph.D. ix Table of Contents Acknowledgements iv Abstract viii Table of Contents x List of Tables xvii List of Figures xviii Chapter 1 — Ambient Mass Spectrometry: Approaching the Chemical Analysis of Things as They Are 1.1 The Chemical Analysis of Things as They are 1 1.2 Concept of Ambient Mass Spectrometry 3 1.3 The Hype 5 1.4 Ambient Mass Spectrometry Hype Cycle 7 1.5 Ambient Mass Spectrometry In Practice 11 1.6 The Future: Seeking Enlightenment 15 References 23 Chapter 2 — Laser Ablation Coupled to a Flowing Atmospheric-Pressure Afterglow for Ambient Mass Spectral Imaging 2.1 Introduction 26 2.2 Experimental 29 2.2.1 Chemical Reagents and Materials
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