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Analysis of the Detection of Organophosphate Pesticides in Aqueous Solutions Using Polymer-Coated Sh-Saw Devices

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Analysis of the Detection of Organophosphate Pesticides in Aqueous Solutions Using Polymer-Coated Sh-Saw Devices Marquette University e-Publications@Marquette Dissertations (2009 -) Dissertations, Theses, and Professional Projects Analysis of the Detection of Organophosphate Pesticides in Aqueous Solutions Using Polymer- Coated SH-SAW Devices Arnold Kweku Mensah-Brown Marquette University Recommended Citation Mensah-Brown, Arnold Kweku, "Analysis of the Detection of Organophosphate Pesticides in Aqueous Solutions Using Polymer- Coated SH-SAW Devices" (2010). Dissertations (2009 -). Paper 79. http://epublications.marquette.edu/dissertations_mu/79 ANALYSIS OF THE DETECTION OF ORGANOPHOSPHATE PESTICIDES IN AQUEOUS SOLUTIONSUSING POLYMER-COATED SH-SAW DEVICES by ARNOLD K. MENSAH-BROWN, B.SC., M.S. A Dissertation submitted to the Faculty of the Graduate School, Marquette University, in Partial Fulfillment of the Requirements for the Degree of Doctor of Philosophy Milwaukee, Wisconsin December 2010 ABSTRACT ANALYSIS OF THE DETECTION OF ORGANOPHOSPHATE PESTICIDES IN AQUEOUS SOLUTIONS USING POLYMER-COATED SH-SAW DEVICES ARNOLD K. MENSAH-BROWN, B.SC., M.S MARQUETTE UNIVERSITY, 2010 Organophosphate pesticides (OPs) have been found as contaminants in surface and ground waters, soil, and agricultural products. Because OPs are toxic compounds, rapid detection/monitoring of OPs in groundwater is necessary to allow for real-time remediation. Detection of OPs in water has already been demonstrated using poly(epichlorohydrin) [PECH] and polyurethane as the sensing layers. However, the response times were relatively long, hindering real-time monitoring. In this work, a hybrid organic/inorganic chemically sensitive layer [bisphenol A-hexamethyltrisiloxane (BPA-HMTS)] that shows a high degree of partial selectivity for OPs is synthesized, characterized (in terms of the glass transition temperature, Tg, water stability, sensitivity, selectivity, detection limit, and absorption/response time) for the rapid detection of organophosphate pesticides. Direct chemical sensing in aqueous solutions is performed using guided shear horizontal surface acoustic wave sensor platforms on 36° rotated Y- cut LiTaO3 and 42.75° rotated Y-cut Quartz, respectively. It is shown that, for the same coating thickness, a 60% reduction in sensor response time is achieved without reduction in sensitivity compared to PECH. Considering the Tg, for the polymers, it is seen that the faster response shown by BPA-HMTS is due to the porous siloxane backbone, HMTS. Kinetic studies for the absorption of OPs (parathion-methyl, parathion, and paraoxon) from aqueous solutions into the BPA-HMTS coating are conducted. The data are analyzed within the context of two absorption models: penetration-limited and diffusion- limited absorptions. It is shown that the absorption process is rate limited by penetration with a concentration independent absorption time constant or mass transfer coefficient. The absorption time constants for parathion-methyl, parathion, and paraoxon are calculated. A limit of detection of 60, 20 and 100 μg/L (ppb) for parathion-methyl, parathion, and paraoxon, respectively, is calculated for the present non-optimized sensor. Concentrations as low as 500 μg/L (ppb) parathion are actually measured. This is much lower than the typical concentrations found on agricultural produce (≥ 10 ppm). Furthermore, sensor signal analysis in the form of the extended Kalman filter (EKF) is employed on-line during the detection process. The sensor response was first represented by a state-space model which includes all relevant contributions to the polymer-coated device response. This allows for the steady-state response and absorption time constant to be extracted on-line well before the steady-state is reached, thus further reducing the time for analyte identification and quantification. It is noted the absorption time constant, often unique to a class of analyte-coating pairs, can be used to improve analyte recognition. i ACKNOWLEDGMENTS ARNOLD K. MENSAH-BROWN, B.SC., M.S This is arguably the most challenging endeavor I have undertaken. It has not been easy and I know that it is by God’s grace that I am what I am, and the grace that He has given me was not without effect. On the contrary, I have worked hard, although it was not really my own doing. This grace includes my faith, the opportunity to use my energy and talents to do this work, and the people He has put in my life to help me on my journey. I would like to express my gratitude to my advisor and mentor, Dr. Fabien Josse; the countless hours of discussions, suggestions, and review of this dissertation helped me complete this work in a timely manner. I am also thankful to him for exposing me to the international sensor community and helping me develop my writing and presentation skills. I would also like to thank Dr. Edwin Yaz for sharing his expertise in control systems and estimation theory, which were a great help in developing the state-space models used in this work. My sincere gratitude also goes to my entire research committee: Dr. Yaz, Dr. Schneider, Dr. Cernosek, and Dr. Lee. Thank you for reviewing my work and making suggestions on how to improve this dissertation. I would also like to thank Dr. Henry Mensah-Brown for countless valuable discussions and introducing me to experimental design concepts. I also thank Dr. Michael Wenzel, a former fellow student and friend, for helpful discussions on signal processing and estimation theory. In addition, I would like to thank my former and present fellow students (Michael Wenzel, Greg Novak, Ryan Kabacinski, Meetalee Dalal, Tao Cai, Jinjin Zhang, Russell Cox, Tian Newman, Michael McCarthy, and Ashley Milner) in the Microsensor Research Laboratory at Marquette University. Special thanks also to Dave Gibas, Ray Hamilton, and Tom Silman in the Discovery Learning Center at Marquette University, for their assistance in machining parts for this project and our lab. My sincere appreciation to Darlington Mlambo, a doctoral student in the Chemistry Department at Marquette University, for his help in synthesizing and characterizing the polymer used in this work and for sharing relevant references; your commitment and friendship was a source of moral support. I would also like to thank Dr. Hossenlopp for granting me access to her laboratory, without which the polymer used in this work could not have been synthesized. I would also like to thank Drs. Bender, Schneider, and Lee for helpful discussions. Finally, I sincerely thank my parents, Henry and Christabel, for all their sacrifices, wisdom, patience, prayers, love, care, and encouragement over the years; my sisters, Shirley and Henrietta, as well as members of my extended family, especially Grandma Christina; my uncles, Dr. Sannichie Quaicoe and family, Mr. Papa Yorke and family, Dr. Ernest Hinson and family, and Mr. Ato Coleman and family, for their support and giving me a home away from home; and many of my friends for your prayers, patience, love and support. Special thanks to Melissa Lemke for proofing initial chapters of this dissertation, helpful discussions, prayers, patience, love, listening, encouragement, and sharing in my humanity. ii Prayer for Generosity “Lord, teach me to be generous. Teach me to serve you as you deserve; To give and not to count the cost, To fight and not to heed the wounds, To toil and not to seek for rest, To labor and not to ask for reward, Save that of knowing that I do your will.” -ST. IGNATIUS OF LOYOLA FOUNDER OF THE SOCIETY OF JESUS iii TABLE OF CONTENTS ACKNOWLEDGMENTS ............................................................................. i TABLE OF CONTENTS ............................................................................ iii LIST OF TABLES .........................................................................................v LIST OF FIGURES .................................................................................... vii 1 INTRODUCTION ..................................................................................1 1.1 The Pesticide Problem ........................................................................................ 1 1.1.1 History......................................................................................................... 2 1.1.2 Classification............................................................................................... 3 1.1.3 Environmental and Health Effects of Pesticides ......................................... 4 1.2 Overview of Chemical Sensors ........................................................................... 7 1.3 Acoustic Wave Devices as Chemical Sensors .................................................. 11 1.4 Shear Horizontal Surface Acoustic Wave (SH-SAW) Sensor Platforms ......... 15 1.5 Applications of Acoustic Wave Chemical Sensors .......................................... 17 1.6 Microsensor Arrays ........................................................................................... 18 1.7 Sensor Signal Processing .................................................................................. 20 1.8 Problem Statement and Objective of Research ................................................. 21 1.9 Dissertation Organization ................................................................................. 24 2 GUIDED SH-SAW DEVICE AS A LIQUID-PHASE SENSOR PLATFORM: A REVIEW .........................................................................26 2.1 Introduction ....................................................................................................... 26 2.2 Formulation of
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