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Development and Evaluation of Passive Sampling Devices to Characterize the Sources, Occurrence, and Fate of Polar Organic Contam

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DEVELOPMENT AND EVALUATION OF PASSIVE SAMPLING DEVICES TO CHARACTERIZE THE SOURCES, OCCURRENCE, AND FATE OF POLAR ORGANIC CONTAMINANTS IN AQUATIC SYSTEMS Jonathan Karl Challis A Thesis Submitted to the Faculty of Graduate Studies in Partial Fulfillment of the Requirements for the Degree of DOCTOR OF PHILOSOPHY Department of Chemistry University of Manitoba Winnipeg, MB, Canada Copyright © May 2018 by Jonathan Karl Challis ABSTRACT The primary goal of this dissertation was to develop and evaluate an improved aquatic passive sampling device (PSD) for measurement of polar organic contaminants. Chemical uptake of current polar-PSDs (e.g., POCIS – polar organic chemical integrative sampler) is dependent on the specific environmental conditions in which the sampler is deployed (flow-rate, temperature), leading to large uncertainties when applying laboratory-derived sampling rates in-situ. A novel configuration of the diffusive gradients in thin-films (DGT) passive sampler was developed to overcome these challenges. The organic-DGT (o-DGT) configuration comprised a hydrophilic-lipophilic balance® sorbent binding phase and an outer agarose diffusive gel (thickness = 0.5–1.5 mm), notably excluding a polyethersulfone protective membrane which is used with all other polar-PSDs. Sampler calibration exhibited linear uptake and sufficient capacity for 34 pharmaceuticals and pesticides over typical environmental deployment times, with measured sampling rates ranging from 9–16 mL/d. Measured and modelled diffusion coefficients (D) through the outer agarose gel provided temperature-specific estimates of o-DGT sampling rates within 20% (measured-D) and 30% (modelled-D) compared to rates determined through full-sampler calibration. Boundary layer experiments in lab and field demonstrated that inclusion of the agarose diffusive gel negated boundary layer effects, suggesting that o-DGT uptake is largely insensitive to hydrodynamic conditions. The utility of o-DGT was evaluated under a variety of field conditions and performance was assessed in comparison to POCIS and grab samples. o-DGT was effective at measuring pharmaceuticals and pesticides in raw wastewater effluents, small creeks, large fast-flowing rivers, open-water lakes, and under ice at near-zero water II temperatures. Concentrations measured by o-DGT were more accurate than POCIS when compared to grab samples, likely resulting from the influence in-situ conditions have on POCIS. Modelled sampling rates were successfully used to estimate semi-quantitative water concentrations of suspect wastewater contaminants using high-resolution mass spectrometry, demonstrating the unique utility of this o-DGT technique. This dissertation establishes o-DGT as a more accurate, user-friendly, and widely applicable passive sampler compared to current-use polar-PSDs. The o-DGT tool will help facilitate more accurate and efficient monitoring efforts and ultimately lead to more appropriate exposure data and environmental risk assessment. III ACKNOWLEDGEMENTS As I pen the final words of this dissertation and reflect back on the challenging and rewarding journey that is a PhD I am overcome with feelings of gratitude. I am grateful to the many important people that have helped me along the way and I feel truly privileged to have had this opportunity. First, I want to thank my advisors, Dr. Charles Wong and Dr. Mark Hanson. It has been a true honour and privilege to work alongside both of you throughout my PhD. Your unique perspectives and advice served invaluable to the success of this research, your work ethic and leadership provided excellent examples to strive towards, and your open and collaborative approaches to supervising students and running a research group allowed me to thrive. Thank you both for the opportunity, advice, encouragement, and unwavering support. I was extremely fortunate to have received excellent funding and awards throughout my program, including from the University of Manitoba, CREATE H2O program, SETAC, Natural Sciences and Engineering Research Council, and most notably the Vanier CGS program. Thank you for the monetary support that made my research possible. Thank you to U of M Chemistry for the yearly graduate awards, Dr. Jennifer van Wijngaarden for the prompt responses to any and all graduate program related questions, and The University of Winnipeg Richardson College for the Environment and Science Complex for the excellent laboratory space. To my advisory committee, Dr. Feiyue Wang, Dr. Hélène Perreault, and Dr. Gregg Tomy, thank you for the support and insight throughout my program. Thank you to Dr. Chris Metcalfe for serving as the external committee member. Feiyue, a special thank you for the letter of support for my Vanier. IV Thank you to my fellow graduate and undergraduate students, lab managers, technicians, and post-docs I encountered during my research. Thank you to Mimi, Al, Luis, Kevin, Shira, Angelique, Marie-Claire, Trisha, Chelsea, Dana, Adam, and many others! Be it banging our heads on the LC-MS/MS, long days sampling the Red River (rain or shine), mesocosm experiments, extracting samples, venting about our often frustrating research, conferencing, group lunches… the list goes on. Thank you all! To my family and friends, thank you for your support! You are all amazing and I love you! Aaron, my whole life you’ve always been great at forcing me away from my work when I couldn’t seem to do it myself. Thank you for that. To my good friend Paul. Thank you for all the late night chats over a glass (or two…) of Jameson’s. You always helped take my mind off my research. To all my friends, whether you knew it or not, you helped keep me balanced and sane throughout this journey. Thank you! To Mom and Dad, thank you for your incredible encouragement, love, and support in everything I do, it is truly motivating and inspiring. I would not be here without the opportunities and support you have provided me in my life and throughout my PhD. I am so grateful and privileged to have such amazing parents. I love you. Lisha, I dedicate this thesis to you. I owe you the most! Thank you for being my best friend and love of my life throughout this journey. Thank you for inspiring and supporting me every single day, no matter what. Especially in these final months. I’m sorry if I haven’t been my normal self and for my above-normal forgetfulness lately… I blame my thesis brain. Yet, through everything, you always stuck by me and found a way to put a smile on my face. Thank you for your patience, understanding, and love! V TABLE OF CONTENTS ABSTRACT…………………………………………………………………………………... II ACKNOWLEDGEMENTS…………………………………………………………………. IV LIST OF TABLES………………………………………………………………………….... X LIST OF FIGURES…………………………………………………………………………. XI LIST OF EQUATIONS……………………………………………………………………. XIII LIST OF ABBREVIATIONS………………………………………………………………. XV 1. INTRODUCTION TO POLAR ORGANIC CONTAMINANTS AND PASSIVE SAMPLING IN AQUATIC SYSTEMS ........................................................................ 1 1.1 Polar Organic Contaminants in Aquatic Systems .................................. 2 1.1.1 Pharmaceuticals ................................................................................ 6 1.1.2 Pesticides......................................................................................... 17 1.1.3 Analysis of Polar Organic Contaminants .......................................... 24 1.2 Environmental Sampling ..................................................................... 32 1.3 Aquatic Passive Sampling ................................................................... 35 1.3.1 Passive Sampling theory.................................................................. 36 1.3.2 Polar Passive samplers ................................................................... 41 1.3.3 Diffusive Gradients in Thin Films (DGT) .......................................... 43 1.4 Objectives and Hypotheses ................................................................ 45 1.5 Dissertation Outline ............................................................................. 47 2. INPUTS, SOURCE APPORTIONMENT, AND TRANSBOUNDARY TRANSPORT OF PESTICIDES AND OTHER POLAR ORGANIC CONTAMINANTS ALONG THE LOWER RED RIVER, MANITOBA, CANADA ........................................................ 50 2.1 ABSTRACT ......................................................................................... 51 2.2 INTRODUCTION................................................................................. 53 2.3 METHODS AND MATERIALS ............................................................ 57 2.3.1 Sampling sites .................................................................................. 57 2.3.2 Target chemicals .............................................................................. 59 2.3.3 Passive samplers ............................................................................. 60 2.3.4 Antibiotic resistance genes .............................................................. 63 2.3.5 Instrumental Analysis ....................................................................... 64 2.3.6 Data Analysis ................................................................................... 65 VI 2.4 RESULTS AND DISCUSSION ............................................................ 67 2.4.1 Watershed and Land Use Descriptors ............................................. 67 2.4.2 Pesticides......................................................................................... 71 2.4.3 Pharmaceuticals .............................................................................
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