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Microvolume Chemical Analysis of Atmospheric Gases and Aerosols

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Microvolume Chemical Analysis of Atmospheric Gases and Aerosols Microvolume Chemical Analysis of Atmospheric Gases and Aerosols by Hao Tang, M.S. A Dissertation In ANALYTICAL CHEMISTRY Submitted to the Graduate Faculty of Texas Tech University in Partial Fulfillment of the Requirement for the Degree of DOCTOR OF PHILOSOPHY Approved Jonathan E. Thompson, Chair Person Carol L. Korzeniewski Dimitri Pappas Peggy Gordon Miller Dean of the Graduate School August, 2012 Copyright 2012, Hao Tang Texas Tech University, Hao Tang, August 2012 Acknowledgements Time flies, my PhD student life is coming to an end. I had the joy of success and also frustrations of failure during these four years. There are so many people and things worth remembering and thanks. I could not list all but I will remember them in my heart. First of all, I would like to express my heartfelt gratitude to my mentor, Dr. Jonathan Thompson, for his guidance and help in the past four years. He provided me a great atmosphere for doing my research and patiently gave suggestions for experiments and encouragement throughout my PhD study. Without his excellent guidance and caring, I would not be able to finish my PhD program and complete my dissertation. I also want to thank Dr. Pappas and Dr. Korzeniewski for serving as my committee members and giving me valuable suggestions in many aspects. I would like to thank all the professors who have taught and helped me during my time at Texas Tech. Also I owe thanks to all the people from my research group for helping created a comfortable environment to do research. I am thankful for all my friends in Lubbock, PhD life gets easier with your accompany! Finally, I would like to say thank you to my parents. They sacrifice a lot for me and their support is very important for me to finish my PhD program. ii Texas Tech University, Hao Tang, August 2012 Table of Contents Acknowledgements ................................................................................................... ii Table of Contents ...................................................................................................... iii Abstract .................................................................................................................. viii List of Tables ............................................................................................................. x List of Figures ......................................................................................................... xii List of Abbreviations .............................................................................................. xvi Chapter Ι.................................................................................................................... 1 General Introduction .................................................................................................. 1 1.1 Structure of Earth’s Atmosphere ....................................................................... 1 1.2 Atmospheric Composition: Gases and Aerosols ................................................ 1 1.2.1 Introduction to Atmospheric Gases: Sources, Composition & Effects .......... 2 1.2.2. Introduction to Atmospheric Aerosols: Sources, Composition & Effects .... 3 1.3 Analytical Chemistry & the Atmosphere ........................................................... 5 1.3.1 Analysis of Atmospheric Gases ................................................................... 6 1.3.2 Analysis of Atmospheric Aerosol ................................................................ 8 1.4 Introduction to Anlytical Techniques used in this Dissertation Research .......... 12 1.4.1 Microvolume and Miniaturization Techniques for Gas Analysis ................ 12 1.4.2 Capillary Electrophoresis and its Application in Atmospheric Chemistry .. 13 1.5 Summary ........................................................................................................ 17 1.6 References ...................................................................................................... 27 Chapter II ................................................................................................................ 31 iii Texas Tech University, Hao Tang, August 2012 Evaluation of Microvolume Regenerated Cellulose (RC) Microdialysis Fibers for the Sampling and Detection of Ammonia in Air ............................................................. 31 Abstract ................................................................................................................... 31 2.1 Introduction .................................................................................................... 32 2.2 Experimental .................................................................................................. 37 2.2.1 Reagents ................................................................................................... 37 2.2.2 Design of the Permeable Membrane Sampling Probe ................................ 37 2.2.3 Generation of Air Samples Containing Ammonia ...................................... 39 2.2.4 Fluorescent Derivatization and Analysis ................................................... 40 2.2.5 Reaction Kinetics & Specificity Study ...................................................... 42 2.3 Results and Discussion ................................................................................... 43 2.3.1 Efficacy of the Membrane Sampling Probe ............................................... 43 2.3.2 Effect of Relative Humidity (RH) on Probe Performance .......................... 44 2.3.3. Potential Interferences: Amines and Particulate NH4+ ............................. 45 2.3.4 Field Measurements of Ammonia at a Swine Barn .................................... 48 2.3.5 On-Line Analysis Ammonia in the Laboratory .......................................... 49 2.4 Conclusion...................................................................................................... 51 2.5 References ...................................................................................................... 61 Chapter III ............................................................................................................... 63 Characterization of a Novel Particle into Liquid Sampler for Analysis of Single Fluorescent Aerosol Particles through Capillary Electrophoresis .............................. 63 Abstract ................................................................................................................... 63 3.1 Introduction .................................................................................................... 64 iv Texas Tech University, Hao Tang, August 2012 3.2 Experimental .................................................................................................. 67 3.2.1 Reagents ................................................................................................... 67 3.2.2 Preparation of FITC-Amino Acid Conjugates ........................................... 68 3.2.3 Experiment Design ................................................................................... 68 3.2.4 Generation of Test Aerosols ...................................................................... 73 3.3 Results and Discussion ................................................................................... 73 3.3.1 Detection of Particles by Laser Light Scattering ........................................ 73 3.3.2 Particle Collection Efficiency of the Inertial Impactor ............................... 75 3.3.3 Particle Sampling Coupled with CE for Qualitative Analysis .................... 79 3.3.4 Estimation of Injection Efficiency for Single Particles .............................. 82 3.4 Conclusion...................................................................................................... 84 3.5 References ...................................................................................................... 90 Chapter IV ............................................................................................................... 93 The Aqueous Phase Nitration of Phenol and Benzoic Acid Studied through Flow-Gated Capillary Electrophoresis ......................................................................................... 93 Abstract ................................................................................................................... 93 4.1 Introduction .................................................................................................... 94 4.2 Experimental Methods. ................................................................................... 97 4.2.1 Reagents ................................................................................................... 97 4.2.2 Capillary Electrophoresis .......................................................................... 98 4.2.3 UV-VIS Spectroscopy ............................................................................... 99 4.2.4 Solid-Phase Extraction (SPE) and Mass Spectrometry (MS) ................... 100 4.2.5 Safety Concerns ...................................................................................... 101 v Texas Tech University, Hao Tang, August 2012 4.3 Results & Discussion .................................................................................... 102 4.3.1 Analyzing a Known Mixture by the Flow-Gated CE System ................... 102 4.3.2 Analysis of the Benzoic Acid Nitration Reaction: Benzoic Acid + NaNO2 +H2O2 ............................................................................................................
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