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Heterogeneous Production of Perchlorate and Chlorate By HETEROGENEOUS PRODUCTION OF PERCHLORATE AND CHLORATE BY OZONE OXIDATION OF Cl- by SIXUAN WANG B.E. A Thesis In CIVIL ENGINEERING Submitted to the Graduate Faculty of Texas Tech University in Partial Fulfillment of The Requirements for The Degree of MASTER OF SCIENCE IN CIVIL ENGINEERING Approved Dr. Andrew W. Jackson Chairperson of the Committee Dr. Todd A. Anderson Peggy Gordon Dean of Graduate School August, 2011 Copyright © 2011, Sixuan Wang Texas Tech University, Sixuan Wang, August 2011 ACKNOWLEDGEMENTS This research project would not finish without the support of many people. I would like to express my gratitude to all those who gave me help and support to complete this thesis. I want to thank Dr. Andrew Jackson, the chair of my committee for giving me the chance, guidance, and encouragement. I would like to take this opportunity to thank my committee members, Dr. Todd Anderson, for his continuous support and encouragement all the way. I would also take this opportunity to thank my friends and colleagues Dr. Rao, Nubia, Felipe, Tony and Tim for their continuous help, sharing during these two years of research in Environmental lab. I am very thankful to the Strategic Environmental Research and Development Program (SERDP) for providing the necessary funds for this project. ii Texas Tech University, Sixuan Wang, August 2011 TABLE OF CONTENTS ACKNOWLEDGEMENTS .......................................................................................... ii ABSTRACT .................................................................................................................. v LIST OF TABLES ...................................................................................................... vii LIST OF FIGURES ................................................................................................... viii I. INTRODUCTION ..................................................................................................... 1 1.1 Occurrence of Natural Perchlorate ...................................................................... 3 1.2 Natural Perchlorate Production Mechanisms ...................................................... 4 - 1.2.1 ClO4 Production by UV Irradiation of Oxychlorine Aqueous Species ....... 4 - - 1.2.2 ClO4 Production by Ozone Oxidation of Cl in Aqueous and Dry Systems 6 - 1.2.3 ClO4 Production by Ozone Oxidation of Aqueous Chlorine/Oxy-Chlorine Species ................................................................................................................... 6 1.3 Chlorate Background Information ...................................................................... 7 1.4 Objectives ............................................................................................................ 8 II. MATERIALS AND METHODS ............................................................................. 9 2.1 Experiment Set-up ............................................................................................. 12 2.1.1 Reactor Surface Area Experiment .............................................................. 14 2.1.2 Humidity Experiment ................................................................................. 14 2.1.3 HCl Oxidation Experiment ......................................................................... 16 2.2 Control system................................................................................................... 17 2.3 Chemicals and reagents ..................................................................................... 18 2.4 Measurements of ozone concentrations ............................................................ 18 2.5 Analyses of chlorine oxyanions ........................................................................ 18 2.5.1 Perchlorate Analysis ................................................................................... 18 2.5.2 Chlorate Analysis ....................................................................................... 19 2.5.3 Chloride Analysis ....................................................................................... 20 iii Texas Tech University, Sixuan Wang, August 2011 III. RESULTS ............................................................................................................. 21 3.1 Production of Perchlorate and Chlorate from Ozone Oxidation of non-Aqueous Chloride ................................................................................................................... 21 - - 3.2 The Effect of Reaction Time on ClO4 Generation by Ozone Oxidation of Cl 21 - - 3.3 The Impact of Initial Cl mass on ClO4 production .......................................... 30 - 3.4 The Impact of Moisture on ClO4 production.................................................... 35 - 3.5 The Impact of Reactor Surface Area on ClO4 Production ............................... 37 - - 3.6 Formation of ClO4 and ClO3 by Ozone Oxidation of HCl Gas ....................... 44 IV. DISCUSSION ....................................................................................................... 47 4.1 Perchlorate Generation by Ozone Oxidation of Cl- .......................................... 47 4.2 Effect of Reaction Time .................................................................................... 47 4.3 Effect of Initial Cl- Mass ................................................................................... 48 4.4 Effect of Reactor Surface Area ......................................................................... 49 4.5 Effect of Humidity ............................................................................................ 50 - - 4.6 ClO4 Formation by O3 Oxidation of Gas Phase Cl .......................................... 51 V. CONCLUSION ...................................................................................................... 52 REFERENCE .............................................................................................................. 55 iv Texas Tech University, Sixuan Wang, August 2011 ABSTRACT - Perchlorate (ClO4 ) an atmospherically produced species, is widely distributed in the environment at low concentrations. Studies have demonstrated the - potential for atmospheric formation of ClO4 and evaluated some mechanisms for - - ClO4 formation by UV irradiation and ozone oxidation of aqueous Cl and oxy- chlorine species as well as the dry oxidation of Cl salts. However, there has been no - systematic evaluation of the controlling factors that impact ClO4 formation by ozone mediated oxidation of dry Cl-. The objective of this study was to determine the - factors that control ClO4 formation by ozone oxidation of chloride in heterogeneous - - systems. Experiments were conducted to evaluate production of ClO4 and ClO3 formation by heterogeneous oxidation by evaluating the ozone oxidation at constant NaCl mass for different oxidation periods, ozone oxidation of varying NaCl masses for a constant oxidation period (1 day), the impact of humidity below the deliquescence point, the impact of reactor and salt surface area, and the physical form - - of Cl (NaCl and HCl). The mass of ClO4 formed in the reactor increased roughly linearly (R2 = 0.98; R2 = 0.83) with respect to reaction time for a constant mass of Cl. - - - ClO4 mass did not consistently vary with an increase in Cl mass while ClO3 increased 3 orders of magnitude (0.043 μg- 37.93 μg) over the 4 order range of Cl- - masses reacted. The manner in which ClO4 formed mass in the humidity system was - similar to how it was produced in the low humidity system; however, ClO3 mass increased by 2 orders of magnitude in the humidity system compared to the dry - - system. ClO4 and ClO3 mass production were linearly related to reactor surface area v Texas Tech University, Sixuan Wang, August 2011 for constant ratio of Cl mass to reactor area but no increase in production was - observed for an increase in Cl surface area at constant Cl mass. ClO4 production form HCl gas was relatively equal to that produced from HCl for similar oxidation time periods and masses. This work suggested that Cl in a variety of forms can be - - heterogeneously oxidized by ozone to produce ClO4 and ClO3 at varying ratios dependent on the oxidation conditions. The ratios appear to be influenced by the total mass of Cl oxidized and associate reaction times. It also appears that the reactor surface area may play a role in the oxidation process perhaps by surface catalyzation. Additional work is required to full evaluate this production mechanisms role in - atmospheric production of ClO4 . vi Texas Tech University, Sixuan Wang, August 2011 LIST OF TABLES 2.1 Experimental Matrix of System Parameters ..................................................... 9 - - - - 3.1 Average ClO4 and ClO3 detected in the reactor, and ClO4 , ClO3 - and Cl in the trapping flask after ozone oxidation of 1.8g of NaCl. .......................... 23 - - - - 3.2 Average ClO4 and ClO3 detected in the reactor, and ClO4 , ClO3 - and Cl in the trapping solution after ozone oxidation of 0.18g of NaCl. ................... 25 - - 3.3 Representation of average ClO4 and ClO3 detected in the reactor, - - - and ClO4 , ClO3 and Cl in the trapping solution of 1day ozone oxidation of different NaCl mass. ............................................................................................... 33 - - 3.4 Average ClO4 and ClO3 Detected in the Reactor and Trapping Solution for 1 Day Oxidation of Cl- Have Different Reactor Surface Area. .............. 39 vii Texas Tech University,
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