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Proquest Dissertations Characterization of Simple Saccharides and Other Organic Compounds in Atmospheric Particulate Matter and Source Apportionment Using Positive Matrix Factorization Thesis by Yuling Jia In Partial Fulfillment of the Requirements for the Degree of Doctor of Philosophy APPROVED, THESIS COMMITTEE: Matthew P. Fraser, Associate Professor, Director, Co-Chair Civil and Environmental Engineering Robert Griffin, Associate Professor, Chair Civil and Environmental Engineering Daniel Cohan, Assistant Professor Civil and Environmental Engineering -4/ Carrie A. Masiello, Assistant Professor Earth Science Pierre Herckes, Assistant Professor Chemistry & Biochemistry, Arizona State University Rice University, Houston, TX May, 2010 UMI Number: 3421320 All rights reserved INFORMATION TO ALL USERS The quality of this reproduction is dependent upon the quality of the copy submitted. Jn the unlikely event that the author did not send a complete manuscript and there are missing pages, these will be noted. Also, if material had to be removed, a note will indicate the deletion. UMT Dissertation Publishing UMI 3421320 Copyright 2010 by ProQuest LLC. All rights reserved. This edition of the work is protected against unauthorized copying under Title 17, United States Code. uest ProQuest LLC 789 East Eisenhower Parkway P.O. Box 1346 Ann Arbor, Ml 48106-1346 ABSTRACT Characterization of Simple Saccharides and Other Organic Compounds in Atmospheric Particulate Matter and Source Apportionment Using Positive Matrix Factorization by Yuling Jia Ambient particulate matter samples were collected at various sites in Texas, Arizona, and Austria from 2005 to 2009 to characterize the organic compositions and local PM sources. The primary biologically derived carbon sources, specifically the atmospheric entrainment of soil and associated biota and primary biological aerosol particles (PBAPs), are major sources contributing to ambient PM. This dissertation work proposes simple saccharides as well-suited tracers to characterize the contribution to ambient PM from these primary biologically derived carbon sources. Saccharide concentrations in ambient PM were determined from various locations and various seasons. Aerosol saccharide compounds displayed seasonal variations, inter-correlations, and size fractionations (fine vs. coarse) that were consistent between samples and that can be used to determine sources. The difference in aerosol saccharide concentrations and relative species abundances was reflective of different climate patterns and ecosystems. Selected saccharide compounds including an established marker (levoglucosan) and novel markers (glucose, sucrose, trehalose, mannitol, and arabitol) were used along with other markers to model the major source contributions to ambient PM using a positive matrix factorization (PMF) model. Major local PM sources were resolved at three Texas sites (San Augustine, Dallas, and Big Bend National Park) and one Arizona site (Higley), with two source factors enriched in the proposed novel saccharide markers that can be related to the primary biologically derived carbon sources. The contribution to PM from the saccharide-rich primary biological sources was estimated to range from 16% (remote area) to 36% (rural and suburban area) at the four sampling sites studied. Other PM sources identified by PMF included motor vehicles, secondary aerosol formation, meat cooking, biogenic wax, sea salt, crustal material, and road dust. To further characterize the primary biologically derived carbon sources, different soil and source samples representing PBAPs (plants and spores) were collected at Higley (AZ) to study their saccharide compositions in particle sizes equivalent to PM2.5 and PM10. It was found that the total measured non-levoglucosan saccharide content relative to PM mass in ambient aerosols (0.2% on average in PM2.5 and 0.11% in PM10) was much higher than the soil samples (<0.02% in both PM2.5 and PM10) but much lower than in the PBAP source samples (2% on average in plant PBAP samples and 16% in spore PBAP samples). The measured PBAP samples contained a concentration of sucrose and glucose that is consistent with the saccharide-rich source profiles resolved from ambient aerosol data analyzed by PMF while the measured soil samples did not. This can be interpreted as confirmation that PBAPs are an important PM source in additional to soil and associate biota at Higley, AZ. However, the saccharide levels in the measured PBAP samples were several orders of magnitude higher than the PMF results, suggesting that the ambient aerosol samples are a combination of high saccharide concentration PBAPs and lower saccharide concentration soils at Higley, AZ. Acknowledgements I would like to express my deepest gratitude to my advisor, Dr. Matthew Fraser, for his invaluable support, encouragement, supervision, and useful suggestions throughout the work of this thesis. His far reaching knowledge and expertise has helped improve the quality of this work and his constant help and support to my research has made the past four years a rich learning experience for me. I am sincerely grateful to the following people at Arizona State University for their help and support with this thesis. First of all, Dr. Pierre Herckes and his research group (James Hutchings, Nabin Upadhyay, and Hansina Hill), who provided much support and help to the chemical analysis of various samples in this work. My colleague Andrea Clements who assisted me with sample collection and analysis and Dr. Tony Hartshorn who helped with soil taxonomy. Last but not least, Dr. Scott Bates and Dr. Leslie Landrum who cordially helped me with the identification and collection of plant and spore samples in this study. This thesis work would not have been possible without their help. I would like to thank Dr. Robert Griffin, Dr. Daniel Cohan, and Dr. Carrie Masiello for serving on my committee, spending time on my thesis and providing valuable advice and comments. I would also like to forward my gratitude to my former colleagues at Rice University, Birnur Buzcu-Guven and Shagun Bhat, for their help with my research. A special thanks goes to Dr. Hans Puxbaum and his research group (Nicole Jankowski, Magdalena Rzaca, and Heidi Bauer) at the Vienna University of V Technology. Cooperation with them has been an inspiring experience to both me and my research. Finally, I wish to thank those I love. To my husband Eddie, who has always been so supportive of me and my work. Whose love, help, and encouragement have pulled me through all the hardships throughout the years. My parents, who I am forever indebted to, have always trusted and supported me with their unconditional love. Without them none of my achievements, if there are any, would have been possible. Contents Abstract ii Acknowledgement iv List of Tables xi List of Figures xiii Chapter 1 Introduction 1 1.1 Motivation 1 1.2 Research Objectives 4 1.3 Hypotheses 5 1.4 Approach 5 Chapter 2 Background and literature review 9 2.1 PM 9 2.1.1 Health effect and regulation 9 2.1.2 Carbonaceous composition and sources 12 2.1.2.1 Elemental carbon 12 2.1.2.2. Organic carbon 13 2.2 Saccharides in aerosols 20 2.2.1 Importance 20 2.2.2 Saccharide species and associated sources 22 2.3 Analysis 26 2.3.1 Organic solvent extraction 26 2.3.2 GC-MS and derivatization 28 2.4 Statistical Tool - Correlation Analysis 30 2.5 Source apportionment 32 2.5.1 Sources and molecular markers 34 vii 2.5.2 PMF 37 Chapter 3 Characterization of saccharides in fine particles collected at rural and urban sites in Texas 42 3.1 Sampling 42 3.2 Analytical methods 43 3.2.1 Element carbon (EC) and organic carbon (OC) analysis 43 3.2.2 Gravimetric analysis 44 3.2.3 Organic speciation 44 3.2.3.1 Extraction 44 3.2.3.2 Analysis 45 3.3 Results 47 3.3.1 Detection limit 47 3.3.2 PM2.5, organic carbon (OC), elemental carbon (EC), and total measured saccharides 48 3.3.3 Aerosol saccharides and seasonal variation 50 3.3.4 Correlation Analysis 59 3.3.5 Rural and urban comparison 61 3.3.6 Source apportionment using PMF 62 3.4 Acknowledgement 69 Chapter 4 Characterization of Organic Fine Particulate Matter in Big Bend National Park and Source Apportionment using PMF 72 4.1 Introduction 72 4.2 Experimental Methods 73 4.2.1 Sample Collection 73 4.2.2 Carbon Analysis 74 4.2.3 Sample Extraction 74 viii 4.2.4 Sample Analysis 75 4.3 Results and Discussion 76 4.3.1 Organic speciation 76 4.3.2 Source Apportionment Using PMF 87 4.3.2.1 Data Analysis by PMF 87 4.3.2.2 Source Profiles 88 4.3.2.3 Relative Source Contributions 94 4.4 Conclusions 98 4.5 Acknowledgement 99 Chapter 5 Saccharide Composition in Fine and Coarse Particulate Matter and Soils in Central Arizona 100 5.1 Introduction 100 5.2 Experimental method 102 5.2.1 PM sampling 102 5.2.2 Soil sampling 103 5.2.3 Element carbon (EC) and organic carbon (OC) analysis 106 5.2.4 Gravimetric analysis 106 5.2.5 Organic speciation 106 5.3 Results and discussion 107 5.3.1 Ambient PM speciation 107 5.3.2 Ambient saccharides 113 5.3.2.1 Saccharide concentrations 113 5.3.2.2 PM10 vs. PM2.5 119 5.3.2.3 Correlation analysis 121 5.3.3 Saccharides in resuspended soil samples 126 5.3.3.1 Total measured saccharides and seasonal change 130 5.3.3.2 Agricultural soil vs. currently uncultivated soil vs. road dust 135 5.3.3.3 Fine vs. coarse soils 136 ix 5.3.4 Ambient saccharides vs. soil saccharides 137 5.3.5 Source Apportionment using PMF 143 5.3.5.1 PMF-resolved source factors 143 5.3.5.2 Relative source contribution to ambient PM2.5 and PM10 and comparison of saccharide
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