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Thesis Occurrence of Cyclo-Siloxanes In THESIS OCCURRENCE OF CYCLO-SILOXANES IN WASTEWATER TREATMENT PLANTS – QUANTIFICATION AND MONITORING Submitted by Harshad Vijay Kulkarni Department of Civil and Environmental Engineering In partial fulfillment of the requirements For the Degree of Master of Science Colorado State University Fort Collins, Colorado Fall 2012 Master’s Committee: Advisor: Pinar Omur-Ozbek Kenneth Carlson Gregory Dooley Copyright by Harshad Vijay Kulkarni 2012 All Rights Reserved ABSTRACT OCCURRENCE OF CYCLO-SILOXANES IN WASTEWATER TREATMENT PLANTS – QUANTIFICATION AND MONITORING Siloxanes are persistent, bio-accumulative and toxic emerging contaminants introduced to wastewater from common healthcare and biomedical products, and various industrial processes. They remain unchanged through wastewater treatment and a considerable portion ends up in surface waters through effluent discharge. 30-60 ng/L Decamethylcyclopentasiloxane (D5) was detected in two UK Rivers, while ~400 ng/L of D5 may be found in wastewater effluents. Hence, siloxanes are under consideration by Canadian Environmental Assessment Agency and UK Environment Agency for drinking water regulations. Siloxanes are hydrophobic and also accumulate in activated sludge and biogas, causing mechanical problems due to scaling. This research aims: to quantify the siloxanes in sludge samples obtained from Loveland, CO wastewater treatment plant (WWTP); and to study their removal. A method was developed to effectively extract siloxanes from activated sludge samples using liquid extraction followed by quantification with gas chromatography/mass spectrometry. Results for Loveland Wastewater Treatment Plant samples indicated that Octamethylcyclotetrasiloxane (D4) and Decamethylcyclopentasiloxane D5 are present up to 17.11 µg/g dried-sludge. The effectiveness of H2O2 in siloxane removal was investigated. Sludge samples were spiked with D4 and D5 at 12 mg/g and were treated with 1ml, 3ml, and 5ml of 30% H2O2 for 1hr, 2hr, and 3hr reaction time each. Results indicated a 72% reduction in D4 and D5 levels after 3 hrs. ii ACKNOWLEDGEMENTS I would like to thank all the individuals whose encouragement and support has made the completion of this thesis possible. First, I would like to express my thanks and gratitude to Prof. Pinar Omur-Ozbek for believing me in my abilities and offering me all the help and encouragement needed. I am indebted by the support and guidance offered by Prof. Pinar Omur- Ozbek, which has helped me become a better researcher. Your advice and guidance will always be cherished throughout my professional and personal life. Thank you, Prof. Pinar Omur-Ozbek, for offering me an opportunity to work with you. Special thank must go to Prof. Gregory Dooley, my graduate committee member for this work, for his sound advice and guidance that helped in completion of this complex work based on detailed analytical experimentations. I express my sincere gratitude for the time and resources provided by Prof. Gregory Dooley without which this work would not have completed. I would like to express my sincere gratitude to Prof. Kenneth Carlson, my other graduate committee member for his valuable advice on overall research aspects and concept development for this research. I would like to thank very specially to John McGee, Manager-Water and Power, City of Loveland for providing financial support for this research and encouragement to develop a research project. Thank you John, for providing me an opportunity to work with you and also helping building up this application based research project. I also would like to thank Dennis Schump, City of Greeley, Link Mueller, City of Fort Collins and Sigmon Cole, City of Boulder for providing us samples for this research. Many thanks go to participants of the online survey who live within United States, India, Spain and South Africa who helped collecting valuable information for this research. I would also like to thank my colleagues Victor Sam, Keerthivasan Venkatapathi, Amol Kitwadkar and Pratigyna Rajkrishna for their unwavering support and invaluable suggestions regarding my work. I would iii also like to thank Adam J Beaupre from Environmental and Radiological Health Sciences department for his valuable inputs in the technical aspects of this research. I express my heartfelt gratitude to my peers and colleagues at CSU Saket Doshi, Sahil Mehta, Swaroop Sahoo and Viney Ugave who directly or indirectly contributed completion of this work, for all their support and encouragement. I would also take this opportunity to express my gratitude to Prof. Sunil Shaha, Prof. Ravi Nikam, Prof. Vidula Swami and Mr. Sunil Karkare who are responsible for my strong passion towards Environmental Engineering and have always encouraged me for research in this field. Last, but never the least, I am indebted by the love, support, and encouragement offered by my parents without which none of this work would have been possible. iv DEDICATION To my parents, Vijay and Juee Without their support, understanding, encouragement, and love this work would not have been possible. v TABLE OF CONTENTS CHAPTER 1. INTRODUCTION ........................................................................................ 1 1.1. MOTIVATION ....................................................................................................... 2 1.2. CONTRIBUTIONS ................................................................................................ 3 1.3. OUTLINE ............................................................................................................... 3 CHAPTER 2. BACKGROUND INFORMATION ............................................................. 4 2.1. Nature of Siloxanes: Physical and Chemical .......................................................... 4 2.2. Engineering Properties of Siloxanes ....................................................................... 8 2.3. Siloxanes in commercial products .......................................................................... 9 2.4. Environmental Significance .................................................................................. 12 2.5. Ecological Significance ........................................................................................ 14 2.6. Regulatory Status .................................................................................................. 16 2.7. Health Issues ......................................................................................................... 19 2.8. Operational Issues ................................................................................................. 20 2.9. Occurrence of Siloxanes in environment .............................................................. 25 2.10. Analysis of Siloxanes: Available Techniques....................................................... 35 2.11. Removal of Siloxanes: Available Techniques ...................................................... 48 CHAPTER 3. PROBLEM STATEMENT ........................................................................ 54 3.1. City of Loveland Wastewater Treatment Plant ..................................................... 55 3.2. Goal of this Study ................................................................................................. 57 CHAPTER 4. EXTRACTION,DETECTION AND MONITORING OF CYCLIC SILOXANES IN WASTE ACTIVATED SLUDGE USING GAS CHROMATOGRAPHY/MASS SPECTROMETRY ........................................................................................................... 58 4.1. Introduction ........................................................................................................... 58 4.2. Materials and Methods .......................................................................................... 60 4.3. RESULTS AND DISCUSSIONS ......................................................................... 66 4.4. Conclusions ........................................................................................................... 71 REFERENCES ........................................................................................................... 73 APPENDIX ........................................................................................................... 79 A. Materials and Instrumentation .............................................................................. 79 B. Methods – Additional Details ............................................................................... 86 C. Survey ........................................................................................................... 96 D. Results ........................................................................................................... 99 E. Utilities Information............................................................................................ 155 vi LIST OF TABLES Table 2-1 Description of Common Siloxanes ................................................................................. 6 Table 2-2 Physical Properties of Common Siloxanes ..................................................................... 7 Table 2-3 Exposure Profile of Siloxanes from Personal Care Products ....................................... 10 Table 2-4 Application – Consumption of Siloxanes ..................................................................... 11 Table 2-5 Chemical and Biochemical Properties of Siloxanes ..................................................... 12 Table 2-6 Half-Life Period for Atmospheric Reactions ..............................................................
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