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Chlorine Cycling in Electrochemical Water and Wastewater Treatment

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Chlorine Cycling in Electrochemical Water and Wastewater Treatment Chlorine Cycling in Electrochemical Water and Wastewater Treatment Systems by Linxi Chen April 3, 2014 B.S., Environmental Engineering, Wuhan University of Technology (2007) A dissertation submitted to the Graduate School of the University of Cincinnati in partial fulfillment of the requirements for the degree of DOCTOR OF PHILOSOPHY Environmental Engineering Program College of Engineering and Applied Science Committee Chair: Dr. Margaret Kupferle, Ph.D., P.E. Abstract In this study, phenol was used in a sodium chloride or sulfate matrix as a representative pollutant to systematically study which operating conditions have the largest impact on chlorine forms in an electrochemical treatment system. Initially, an HPLC method was developed and validated to simultaneously determine phenol and potential intermediates from hydroxylation and hypochlorination pathways during electrooxidation in the presence of chloride. In a combined-reactor configured with a boron-doped diamond (BDD) anode, samples were analyzed to identify and quantify organic intermediates and inorganic chlorine species generated during the electrooxidation of phenol. Ionic strength was kept constant at 50 mM and the applied current density was 12 mA/cm2. The effects of chloride-to-phenol ratio on contaminant removal efficiency and byproduct formation were studied. Experimental results showed that phenol was removed faster at higher chloride-to-phenol ratios but more chlorinated intermediates and chlorate were produced. The impact of initial chloride concentration on the chlorate formation rate was stronger than its impact on phenol removal rate. Analysis of variance (ANOVA) was used to evaluate the statistical significance of operational factors in a full 24 factorial design. Factors studied were anode type (BDD vs. graphite), initial phenol concentration (0.25 – 0.5 mM), initial chloride concentration (5 – 50 mM) and applied current density (12 – 25 mA/cm2), on responses such as phenol i removal rate and chlorate production rate. Results showed that anode type and chloride concentration had the most significant effects either individually or interactively on the phenol removal rate, and that chloride concentration had a considerable effect on the chlorate production rate. Additionally, applied current density had a significant effect on the free chlorine production rate after breakthrough if and when it occurred with BDD in the presence of excess chloride. A 23 factorial design with a given reactor configuration with either BDD or graphite anode was optimized using response surface methodology (RSM) with respect to phenol removal and control of chlorate production. Linear regression results showed that the phenol removal rate was highest at low phenol concentration and high chloride concentration, whereas low chloride concentration minimized chlorate production. In addition to the ANOVA analyses, kinetics of the electrochemical oxidation of phenol and intermediates formed in the presence of chloride were explored for the different anodes at various chloride-to-phenol ratios. Comparison of rate constant k values of the first-order reactions showed that hypochlorination and hydroxylation pathways were in competition and hypochlorination pathway was more favored and 2- chlorophenol was the most dominant species in most cases. Mass balances around carbon and chlorine for measured species were also considered. Lack of closure for both indicated possible formation of other by-products that were not identified by HPLC. LC-QTOF-MS was used to qualitatively investigate the unknown by-products formed during phenol electrooxidation in the presence of chloride at two levels (5 mM and 50 mM) using the BDD anode. Results showed ii formation of chlorinated dimers and trimers of phenol, including potential formation of polychlorinated dibenzo-p-dioxins (PCDDs). Keywords: electrooxidation; phenol; chloride; HPLC; BDD; ANOVA; factorial design; optimization; kinetic modeling; LC-QTOF-MS. iii Acknowledgements I would like to express my gratitude to: • Dr. Margaret Kupferle, my advisor, for her generous support and endless patience. Without her devotion to me and my work, none of this would have been possible. She was always there to encourage me, support me, and keep me on the right track. In the future I will strive to be as good a leader and mentor as she was to me. • The National Science Foundation, for their generous funding and support of this research. They saw the potential in this project and provided the means necessary to make my dream come true. • Dr. Am Jang, for his support and mentoring during my early stages as a graduate student researcher. • Dr. Woohyoung Lee, Dr. Dionysious Dionysiou and Dr. George Sorial for their willingness to serve on my committee, their invaluable comments and guidance through my work. • Dr. Pablo Campo, for his willingness and patience to assist me in instruments and time commitment on reviewing my manuscript. • Jiefei Yu, Xuexiang He, Mugdha Mathure, Liang Yan, Geshan Zhang, Lijuan Sang, Xiaodi Duan, Qingshi Tu and all of my colleagues and friends for their encouragement and motivation both in and out of the lab. • Greg, my colleague, my best friend, and my life partner for his tireless devotion to keeping me motivated, and his willingness to share with me the best times and help me through the worst times. • At last, my family, for their unconditional love and infinite support. v Table of Contents Chapter 1 Introduction ................................................................................................. 1 1.1 Background Introduction ................................................................................. 1 1.1.1 Electrochemical Treatment Technology ....................................................... 1 1.1.2 Phenol as a Representative Organic Waste ................................................... 2 1.1.3 Anode Materials .......................................................................................... 2 1.1.4 Chlorine Chemistry ...................................................................................... 4 1.1.5 Operational Conditions Parameter Study ...................................................... 7 1.1.6 Reaction Kinetics and Mechanism of Electrochemical Oxidation of Phenol . 8 1.2 Research Objectives ....................................................................................... 12 1.3 Approach and Relevance ................................................................................ 13 1.4 References ....................................................................................................... 15 Chapter 2 Development, Validation and Application of an HPLC Method for Phenol Electrooxidation Products in the Presence of Chloride ................................. 19 2.1 Introduction .................................................................................................... 19 2.2 Method Development...................................................................................... 22 2.2.1 Materials .................................................................................................... 22 2.2.2 Development Details .................................................................................. 22 2.3 Method Validation .......................................................................................... 26 2.3.1 Calibration Curves ..................................................................................... 26 2.3.2 Precision (Repeatability and Reproducibility) ............................................. 28 2.3.3 Accuracy .................................................................................................... 31 2.3.4 Method Detection Limit ............................................................................. 31 2.3.5 Column to Column Comparisons ................................................................ 32 2.4 Method Application to Electrooxidation of Phenol ....................................... 33 2.4.1 Experimental Method ................................................................................. 33 2.4.2 Results and Discussion ............................................................................... 34 2.5 Conclusion....................................................................................................... 37 2.6 References ....................................................................................................... 38 Chapter 3 Effect of Chloride-to-Phenol Ratio on Phenol and Intermediates Conversion during Anodic Oxidation ......................................................................... 40 3.1 Introduction .................................................................................................... 40 3.2 Experimental .................................................................................................. 42 3.2.1 Chemicals and Reagents ............................................................................. 42 3.2.2 Experimental Setup .................................................................................... 43 vi 3.2.3 Analytical Methods .................................................................................... 44 3.2.4 Operating Conditions ................................................................................. 45 3.3 Results and Discussion.................................................................................... 45 3.3.1 Effect on Phenol Removal and Intermediates Conversion ..........................
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