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Detailed Geochemical and Mineralogical Analyses of Naturally Occurring Arsenic in the Hawthorn Group Olesya Lazareva University of South Florida

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Detailed Geochemical and Mineralogical Analyses of Naturally Occurring Arsenic in the Hawthorn Group Olesya Lazareva University of South Florida University of South Florida Scholar Commons Graduate Theses and Dissertations Graduate School 11-2-2004 Detailed Geochemical and Mineralogical Analyses of Naturally Occurring Arsenic in the Hawthorn Group Olesya Lazareva University of South Florida Follow this and additional works at: https://scholarcommons.usf.edu/etd Part of the American Studies Commons Scholar Commons Citation Lazareva, Olesya, "Detailed Geochemical and Mineralogical Analyses of Naturally Occurring Arsenic in the Hawthorn Group" (2004). Graduate Theses and Dissertations. https://scholarcommons.usf.edu/etd/1126 This Thesis is brought to you for free and open access by the Graduate School at Scholar Commons. It has been accepted for inclusion in Graduate Theses and Dissertations by an authorized administrator of Scholar Commons. For more information, please contact [email protected]. Detailed Geochemical and Mineralogical Analyses of Naturally Occurring Arsenic in the Hawthorn Group by Olesya Lazareva A thesis submitted in partial fulfillment of the requirements for the degree of Master of Science Department of Geology College of Arts and Sciences University of South Florida Major Professor: Thomas Pichler, Ph.D. Thomas Scott, Ph.D. Jonathan Arthur, Ph.D Peter Harries, Ph.D. Date of Approval: November 2, 2004 Keywords: phosphate, mining, pyrite, aquifer, trace metal, florida © Copyright 2004, Olesya Lazareva ACKNOWLEDGEMENTS First and foremost, I would like to gratefully acknowledge the help, support and encouragement of my advisor Dr. Thomas Pichler, who presented me with this wonderful opportunity, and assisted me with developing the research topic and with completing and revising the paper. His contribution to my development as a geochemist cannot be underestimated. I am extremely thankful for his endless effort to provide invaluable assistance and inspired ideas. It was my luck to work with Dr. Thomas Pichler as my advisor. I would like greatly appreciate Southwest Florida Water Management District (SWFWMD) and Mr. Greg Jones, Director of Resource and Conservation Development for SWFWMD, for financial support of this project I would like to thank my Thesis Committee, Dr. Thomas Scott, Dr. Jonathan Arthur, and Dr. Peter Harries, for supporting me throughout my academic career, reviewing the manuscript and providing very valuable and helpful suggestions. I am also grateful to Dr. Chuck Connor, Department of Geology Chair, for his support in my efforts to study statistics. I want to express my gratitude to a great colleague and a good friend, Roy Price, for his incredible help during field work and throughout the entire academic period. I would like to thank faculty, staff and students in the Department of Geology, University of South Florida for their support and guidance throughout this work. Finally I am grateful to my family, my lovely boyfriend Dmitri Prokhorov, and his wonderful parents for their constant inspiration, advice, support, and wisdom. Without their help, patience, and love this work would never happen. TABLE OF CONTENTS LIST OF TABLES iv LIST OF FIGURES v ABSTRACT viii CHAPTER ONE: INTRODUCTION 1 Problem Statement 2 Purpose of Research 3 Research Plan 4 CHAPTER TWO: GEOLOGY AND HYDROGEOLOGY 9 Arcadia Formation 11 Tampa Member 11 Nocatee Member 13 Peace River Formation 13 Origin of Florida’s Phosphate Deposits 17 Possible Arsenic in the Hawthorn Group 18 Francolite (Carbonate Fluorapatite) 19 Sulfide Minerals 19 Clay and Organic Material 20 Hydrous Ferric Oxides (HFO) 20 CHAPTER THREE: METHODS 22 Sample Collection and Preparation 22 Petrography and Mineralogy 23 Stereo and Petrographic Microscopy 23 Scanning Electron Microscopy 24 Chemistry 24 Inductively Coupled Plasma – Optical Emission Spectrometry and Hydride Generation- Atomic Fluorescence Spectrometry 24 Electron-Probe Microanalyser – Wave Dispersive Spectrometry 26 Statistics 26 CHAPTER FOUR: RESULTS 28 Petrography and Mineralogy 28 Stereo and Petrographic Microscopy 28 Arcadia Formation 28 i Peace River Formation 30 Scanning Electron Microscopy 30 Bulk Chemical Composition 32 Hawthorn Group (All samples) 32 Hawthorn Group (Interval Samples) 35 Undifferentiated Arcadia Formation 36 Tampa Member 38 Nocatee Member 40 Peace River Formation 42 Electron-Probe Microanalyser – Wave Dispersive Spectrometry 45 Hawthorn Group (All samples) 45 Undifferentiated Arcadia Formation 46 Tampa Member 49 Nocatee Member 49 Peace River Formation 50 Probability Analysis 53 CHAPTER FIVE: DISCUSSION 63 Abundance of Arsenic in the Hawthorn Group 63 Sources of Arsenic in the Hawthorn Group 71 Francolite (Carbonate Fluorapatite) 71 Pyrite 72 Clay and Organic Matter 73 Hydrous Ferric Oxides (HFO) 74 Quantified Role of Pyrite 74 Mobilization of Arsenic during Phosphate Mining 77 Mobilization of Arsenic during Aquifer Storage and Recovery (ASR) 79 CHAPTER FIVE: CONCLUSIONS 81 REFERENCES 83 APPENDICES 90 APPENDIX A: Detailed Lithological Descriptions of the Arcadia Formation Core Samples 91 APPENDIX B: Detailed Lithological Composition of the Tampa Member of the Arcadia Formation Core Samples 97 ii APPENDIX C: Detailed Lithological Composition of the Nocatee Member of the Arcadia Formation Core Samples 100 APPENDIX D: Detailed Lithological Descriptions of the Peace River Formation Core Samples 102 APPENDIX E: ICP-OES Results for the Arcadia Formation 105 APPENDIX F: ICP-OES Results for the Tampa Member of the Arcadia Formation 113 APPENDIX G: ICP-OES Results for the Nocatee Member of the Arcadia Formation 117 APPENDIX H: ICP-OES Results for the Peace River Formation 120 APPENDIX I: Electron –Probe Microanalysis of Pyrites 122 iii LIST OF TABLES Table 1a. List of 16 core wells chosen for this research (English units) 7 Table 1b. List of 16 cores chosen for this study (Metric units) 8 Table 2. Maximum, Minimum, Mean and Standard Deviation of arsenic concentrations in ppm for the Hawthorn Group and its Formations/Members 33 Table 3. Correlation matrix for the Hawthorn Group (all samples) 35 Table 4. Correlation matrix for the Hawthorn Group (interval samples) 36 Table 5. Correlation matrix for the undifferentiated Arcadia Formation 38 Table 6. Correlation matrix for the Tampa Member of the Arcadia Formation 39 Table 7. Correlation matrix for the Nocatee Member of the Arcadia Formation 42 Table 8. Correlation matrix for the Peace River Formation 44 Table 9. Electron microprobe results for arsenic in pyrites for the Formation/ Member of the Hawthorn Group (in ppm) 46 Table 10. Electron microprobe results for arsenic in pyrites and phosphate matrix in sample 5-1-235 for the undifferentiated Arcadia Formation (wt. %) 48 Table 11. Electron microprobe results for arsenic in pyrites and hydrous ferric oxides in sample 4-1-501 for the undifferentiated Arcadia Formation (in weight percent) 49 Table 12. Probability of arsenic concentrations being larger than corresponding values throughout the Hawthorn Group 62 Table 13. Measured bulk arsenic concentrations and calculated arsenic in pyrite 75 iv LIST OF FIGURES Figure 1. Map of the research area including the ROMP locations, numbers, names, and the FGS well numbers of the 16 cores that were sampled 5 Figure 2. Lithostratigraphic and hydrogeologic units of the study area 12 Figure 3. Geological cross sections of southwestern Florida 15 Figure 4. Geological cross sections of southwestern Florida Hillsborough and Manatee Counties 16 Figure 5. Backscattered images of framboidal pyrite (py) in carbonate matrix (carb) from sample 20-143 (Arcadia Formation) 29 Figure 6. Scanning electron micrograph of framboidal pyrite (py) onto kaolinite (kaol) in sample 22-170 from the Tampa Member (arsenic concentration is 14.0 ppm) 31 Figure 7. Scanning electron micrograph of euhedral pyrite (py) in sample 4-1-599 from the Arcadia Formation (arsenic concentration is 7.5 ppm) 31 Figure 8. Diagrams showing correlation between Fe and S in the Hawthorn Group all data (A) and without the outlier (B) 34 Figure 9. Correlation between Fe and S for the Hawthorn Group interval samples 35 Figure 10. Correlation between Fe and S for the Undifferentiated Arcadia Formation 37 Figure 11. Correlation between Fe and S for the Tampa Member 39 Figure 12. Correlation between As and S for the Tampa Member 40 Figure 13. Correlation between Fe and S for the Nocatee Member 41 Figure 14. Diagrams showing correlation between Fe and S in the Peace River Formation for all data set (A) and with removed outlier (B) 44 v Figure 15. Elemental mapping of phosphorite in sample 5-1-235 (Arcadia Formation) 47 Figure 16. (A) Photograph of sample 4-1-501 (undifferentiated Arcadia Formation); (B) Backscattered image of pyrites (py), hydrous ferric oxides (HFO), and carbonate matrix (carb) 48 Figure 17. (A) Photograph of sample 12 – 125 (Peace River Formation) composed of clays (1 = 12 – 125(1)) and pyrite – phosphate matrix (2 = 12-125(2)); (B) Photomicrograph of contact between sample (1) and (2); (C) Backscattered image of pyrite (py), clay (cl) and phosphate (ph) 51 Figure 18. Elemental mapping of pyrite in sample 12-125 (Peace River Formation) 52 Figure 19. Frequency histogram and normal P-P plot of log-transformed arsenic concentrations from the Hawthorn Group 53 Figure 20. Frequency histogram and normal P-P plot of log-transformed sulfur concentrations from the Hawthorn Group 54 Figure 21. Frequency histogram and normal P-P plot of log-transformed iron concentrations from the Hawthorn Group 54 Figure 22. Cumulative distribution function of log-transformed arsenic concentrations for the all Hawthorn Group 55 Figure
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