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Lead and Arsenic Speciation and Bioaccessibility Following Sorption on Oxide Mineral Surfaces

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Lead and Arsenic Speciation and Bioaccessibility Following Sorption on Oxide Mineral Surfaces LEAD AND ARSENIC SPECIATION AND BIOACCESSIBILITY FOLLOWING SORPTION ON OXIDE MINERAL SURFACES Dissertation Presented in Partial Fulfillment of the Requirements for the Degree Doctor of Philosophy in the Graduate School of The Ohio State University By Douglas Gerald Beak, B.S. ***** The Ohio State University 2005 Dissertation Committee: Approved by Dr. Nicholas Basta, Co Advisor Dr. Samuel Traina, Co Advisor _________________________ Co Advisor Dr. Harold Walker Dr. Kirk Scheckel _________________________ Co Advisor Soil Science Graduate Program ABSTRACT The risk posed from incidental ingestion of arsenic-contaminated or lead- contaminated soil may depend on sorption of arsenate (As(V)) or lead (Pb(II)) to oxide surfaces in soil. Arsenate or lead sorbed to ferrihydrite, corundum, and birnessite model oxide minerals were used to simulate possible effects of ingestion of soil contaminated with As(V) or Pb(II). Arsenate or lead sorbed oxides were placed in a simulated gastrointestinal tract (in vitro) to ascertain the bioaccessibility of As(V) or Pb(II) and changes in As(V) or Pb(II) surface speciation. The speciation of As or Pb was determined using EXAFS and XANES analysis. The As(V) adsorption maximum was found to be 7.04 g kg-1, and 0.47 g kg-1 for ferrihydrite and corundum, respectively. The bioaccessible As(V) for ferrihydrite ranged form 0 to 5 % and for corundum ranged from 0 to 16 %. The surface speciation for ferrihydrite and corundum was determined to be binuclear bidentate. These results for As(V) sorbed to ferrihydrite and corundum suggest that the bioaccessibility of As(V) is related to the As(V) concentration, and the As(V) adsorption maximum. The bioaccessibility of As(V) sorbed to birnessite ranged from 16 to 28 % and the As(V) surface speciation was binuclear bidentate. The results for As (V) sorbed birnessite suggest that birnessite can reduce the bioaccessibility of As(V) in contaminated soil. Sorption of Pb(II) was significant for all the model oxides used. The sorption maximum was found to be 2.13 g kg-1 for corundum, 38.6 g kg-1 for ii ferrihydrite, and 127 g kg-1 for birnessite. The bioaccessible Pb(II) ranged from 53 to 88 % for ferrihydrite, Pb(II) concentrations greater than 200 mg kg-1 was greater than 85 % for corundum and below 200 mg kg-1 there was no bioaccessible Pb(II). There was no measurable bioaccessible Pb(II) for any concentration of Pb sorbed birnessite. The surface Pb(II) speciation was found to be: 1. Mononuclear bidentate for ferrihydrite, 2. Mononuclear bidentate and an outer-sphere complex for corundum, and 3. Binuclear bidentate, and trinuclear tridentate for birnessite. Ferrihydrite and corundum usefulness in Pb remediation would be limited when risk of incidental ingestion is of major concern. iii To Stephanie, Aislinn, and Delaney, my favorite girls iv ACKNOWLEDGEMENTS I wish thank my advisors, Nick Basta and Sam Traina, for providing opportunities to explore. Without their patience, input, guidance, and financial support none of this would be possible. I would also like to thank Hal Walker for his help and support throughout the process, but especially during the period between Sam’s leaving and Nick’s arrival. I would like to thank my other committee member, Kirk Scheckel for making the EXAFS analysis a reality and providing an opportunity that lead to securing a job. Thanks also to Sandy Jones and Jerry Bigham for the use of the XRD, Surface Area Analyzer and Thermal Analysis and their guidance in the mineralogical analysis. I sincerely appreciate the help Danold Golightly provided me in training on the ICP and ICP analysis in his and Hal Walker’s lab. Thanks to Dr. Fred Rhoton for providing the ferrihydrite used in this research and to Alcoa for supplying the T64-20 micron corundum used in this research. The use of the Advanced Photon Source was supported by the U. S. Department of Energy, Office of Science, Office of Basic Energy Sciences, under Contract No. W- 31-109-Eng-38. Portions of this work were performed at the DuPont-Northwestern-Dow Collaborative Access Team (DND-CAT) Synchrotron Research Center located at Sector 5 of the Advanced Photon Source. DND-CAT is supported by the E.I. DuPont de v Nemours & Co., The Dow Chemical Company, the U.S. National Science Foundation through Grant DMR-9304725 and the State of Illinois through the Department of Commerce and the Board of Higher Education Grant IBHE HECA NWU 96. Finally, I would like to thank my family for making all of this possible. To my wife Stephanie, thank you for your sacrifices, understanding, patience, love, encouragement, and gentle prodding. Your support over the years made this possible. Without you this would not have happened and I owe you big time. Thank you. I would like to thank my daughters Aislinn and Delaney. You tried really hard to understand what was going on while Daddy was at work or writing his “book”, and you did a great job of letting me get my “book” finished. Your smiling little faces always cheered me up. When this is over I owe you some time at the “roller slide”. vi VITA April 20, 1964 ……………………. Born- Honolulu Hawaii 1989 ………………………………. B.S. Education, The Ohio State University 1989- 1990 ………………………… Research Assistant, Environmental Soil Chemistry Laboratory The Ohio State University, Columbus, Ohio 1990- 2000 ………………………… Research Associate, Lab Manager, Environmental Chemistry Water Quality Laboratory The Ohio State University, Columbus, Ohio 2000- Present ……………………… Research Associate, Lab Manager Soil Physical Chemistry Laboratory The Ohio State University, Columbus, Ohio PUBLICATIONS Research Publications 1. Beak, Douglas G., and Nicholas T. Basta. 2005. Bioaccessibility of As bound to Ferrihydrite. 230th ACS National Meeting. Washington, DC. Aug. 28- Sept. 1, 2005. 2. Beak, Douglas G., Nicholas T. Basta, Kirk Schekel, and Samuel Traina. 2005. The bioaccessibility of As bound to ferrihydrite. 8th International Conference of the Biogeochemistry of Trace Elements (ICOBTE). Adelaide, Australia. April 3- 7, 2005. 3. Beak, Douglas G., Chia-Chen Chen, Jerry M. Bigham, and Samuel J. Traina. 1999. Synthesis and Properties of Hematite, Maghemite, and Their Chromium Substituted Analogs. In: Proceedings of the 36th Annual Meeting of the Clay Minerals Society, June 26- July 1, 1999. Purdue University, West Lafayette, IN. pg. 11. vii 4. Beak, Stephanie A., Douglas G. Beak, and Samuel J. Traina 1999. Gastrointestinal Adsorption of Lead From Soils and Associated Health Effects. Conference on Topics in Toxicology and Risk Assessment. April 1999. Wright Patterson Airforce Base, Fairborn, OH. 5. Springer, Abraham E., E. Scott Bair, and Douglas Beak. 1996. Natural Gradient, Surface Applied Tracer Test at the Ohio Management Systems Evaluation Area. Environmental & Engineering Geoscience. Vol. II, No. 4, Winter 1996. p. 453 - 464. 6. Logan, T. J., D. J. Eckert, and D. G. Beak. 1994. Tillage, Crop, and Climatic Effects on Runoff and Tile Drainage Losses of Nitrate and Four Herbicides. Soil and Tillage Res. Vol. 30. No. 1. p. 75 - 103. 7. Springer, A. E., E. S. Bair and D. Beak. 1993. Agricultural Chemical Transport Relative to a Tracer Under Natural Recharge Conditions in an Alluvial Valley Aquifer. EOS, Transactions, American Geophysical Union, vol. 74, No. 16. p. 129. 8. Logan, T. and D. Beak. 1993. The Sampling, Analytical, and Quality Control/ Quality Assurance Program of the Ohio MSEA. In: Proceedings of the Agricultural Research to Protect Water Quality Conference, February 21 - 24, 1993, Minneapolis, Minnesota. Published by the Soil and Water Conservation Society. p. 347 - 350. 9. Springer, A., S. Bair, and D. Beak. 1993. Transport of Atrazine, Alachlor, and Nitrate Relative to the Tracer Bromide at the Ohio Management Systems Evaluation Area. In: Proceedings of the Agricultural Research to Protect Water Quality Conference, February 21 - 24, 1993, Minneapolis, Minnesota. Published by the Soil and Water Conservation Society. p. 102 - 109. 10. White, D. A., A. D. Ward, and D. G. Beak. 1993. Bias in Field Sampling Techniques for Assessing Nitrate Concentrations in Groundwater. In: Proceedings of the Agricultural Research to Protect Water Quality Conference, February 21 - 24, 1993, Minneapolis, Minnesota. Published by the Soil and Water Conservation Society. p. 359 - 364. FIELDS OF STUDY Major Field: Soil Science viii TABLE OF CONTENTS Page Abstract ………………………………………………………………………………….. ii Dedication ………………………………………………………………………………. iv Acknowledgements ……………………………………………………………………… v Vita …………………………………………………………………………………….. vii List of Tables …………………………………………………………………………... xii List of Figures …………………………………………………………………………. xiv Introduction ……………………………………………………………………………… 1 Chapters 1. Bioaccessibility of Arsenate bound to ferrihydrite using a simulated gastrointestinal system …………………………………………………………... 2 Abstract ………………………………………………………………………….. 2 Key Words ………………………………………………………………………. 3 Introduction ……………………………………………………………………… 3 Materials and Methods …………………………………………………………... 6 Elemental Composition ………………………………………………….. 6 XRD Analysis …………………………………………………………… 7 Surface Area Measurements …………………………………………….. 7 Point of Zero Charge …………………………………………………….. 7 Determination of Fe and As by Inductively Coupled Plasma Atomic Emission Spectroscopy (ICP) ………………………….. 8 Arsenic Sorption Isotherms ……………………………………………... 8 Solid Preparation for Bioaccessibility and Speciation Determination …………………………………………………………… 9 Estimation of Bioaccessible Arsenic ……………………………………. 9 Solid Phase Speciation of Arsenic ……………………………………... 10 Results
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