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Soluble Phosphate Amendments for Metal and Radionuclide

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Soluble Phosphate Amendments for Metal and Radionuclide SOLUBLE PHOSPHATE AMENDMENTS FOR METAL AND RADIONUCLIDE IMMOBILIZATION by FRANTISEK MAJS (Under the Direction of William P. Miller) ABSTRACT Intensive mining and processing of metals and radionuclides have resulted in significant soil and sediment contamination. Phosphate-based in-situ immobilization of the metals and radionuclides has been proposed as an alternative to disruptive and expensive cleanup strategies. This dissertation summarizes results of two experiments, which tested potential of four phosphate amendments [trisodium trimetaphosphate, dodecasodium phytate (Na-IP6), calcium phytate (Ca-IP6) and hydroxyapatite] to immobilize Cu, Zn, and Pb in soil and Ni and U in sediment. Stability of immobilized contaminants was tested by selective leaching and solid phase speciation techniques. Hydroxyapatite lowered trace metal and U solubility with increasing treatment level and Ca-IP6 behaved in general similarly, except for a slight increase in Ni and Cu solubilities at higher amendment levels, presumably due to the chelation potential of phytate. Application of metaphosphate and Na-IP6 were proven unsuitable due to dispersion of soil organic matter and colloidal particles, which had a negative impact on contaminant solubility. Leaching techniques revealed amendment-derived changes in element fractionation and indicated that HA was suitable for Cu, Zn, and Pb immobilization, whereas Ca-IP6 only for Pb and U immobilization, and brought into question the efficacy of applying phosphates for immobilization of Ni. Qualitative spectroscopy disclosed Pb speciation in solid phase in the untreated soil and mechanisms of its transformation upon phosphate addition, but failed to identify any crystalline form of U in the sediment. Unamended Pb-contaminated soil showed strong diffraction patterns for anglesite, cerussite, and plumbojarosite. Hydroxyapatite and Ca-IP6 amendments facilitated precipitation of corkite and to a lesser extent drugmanite and pyromorphite. This is significant because pyromorphite is usually proposed as the main sink of Pb in the amended soils. INDEX WORDS: µ-XRD, µ-XRF, apatite, copper, corkite, drugmanite, lead, nickel, phytate, plumbojarosite, pyromorphite, trimetaphosphate, uranium, zinc SOLUBLE PHOSPHATE AMENDMENTS FOR METAL AND RADIONUCLIDE IMMOBILIZATION by FRANTISEK MAJS B.S., Mendel Agriculture and Forestry University, Czech Republic, 1996 M.S., Mendel Agriculture and Forestry University, Czech Republic, 1999 M.S., University of Minnesota, 2003 A Dissertation Submitted to the Graduate Faculty of The University of Georgia in Partial Fulfillment of the Requirements for the Degree DOCTOR OF PHILOSOPHY ATHENS, GEORGIA 2009 © 2009 Frantisek Majs All Rights Reserved SOLUBLE PHOSPHATE AMENDMENTS FOR METAL AND RADIONUCLIDE IMMOBILIZATION by FRANTISEK MAJS Major Professor: William P. Miller Committee: Miguel L. Cabrera Brian P. Jackson David E. Radcliffe Aaron Thompson Electronic Version Approved: Maureen Grasso Dean of the Graduate School The University of Georgia December 2009 DEDICATION I would like to dedicate this work to my wife and to my parents. I would not be here without you. iv ACKNOWLEDGEMENTS I would like to thank my advisor Dr. Bill Miller, who joined my doctoral advisory committee after it was well under way and eventually took over its leadership. I certainly would not be where I am today without his support, guidance, and encouragement. His help and critical evaluation made it possible for me to navigate the final stages of my dissertation writing. I would also like to extend my thanks to all my committee members – Dr. Miguel Cabrera, Dr. Brian Jackson, Dr. David Radcliffe, and Dr. Aaron Thompson – for their support throughout my years at University of Georgia. Financial assistance was provided through Financial Assistance Award number DE-FC09-07SR22506 from the U.S. Department of Energy to the University of Georgia Research Foundation and by the Department of Crop and Soil Sciences at the University of Georgia. Research was performed in part at Beamline X26A, National Synchrotron Light Source (NSLS), Brookhaven National Laboratory. Beamline X26A is supported by the Department of Energy (DOE) – Geosciences (DE-FG02-92ER14244 to the University of Chicago – CARS) and DOE – Office of Biological and Environmental Research, Environmental Remediation Sciences Division (DE-FC09-96-SR18546 to the University of Georgia). Use of the NSLS was supported by DOE under Contract No. DE-AC02- 98CH10886. v TABLE OF CONTENTS Page ACKNOWLEDGEMENTS.................................................................................................v LIST OF TABLES........................................................................................................... viii LIST OF FIGURES ........................................................................................................... ix CHAPTER 1 INTRODUCTION .............................................................................................1 Problem Definition........................................................................................2 2 LITERATURE REVIEW..................................................................................5 Risk Assessment of Metal and Radionuclide Contaminated Soil and Sediment..................................................................................................5 Lead in Soil .................................................................................................13 Uranium in Sediment...................................................................................17 Phosphate Additions to Soil and Sediment .................................................19 Objectives of this Study ..............................................................................23 3 MATERIALS AND METHODS.....................................................................24 Sample Description .....................................................................................24 Total Digestion............................................................................................27 Batch Equilibration......................................................................................28 Toxicity Characteristic Leaching Procedure ...............................................29 Sequential Extraction ..................................................................................30 vi X-ray Spectrometry in the Electron Microscope.........................................32 Synchrotron Element Mapping and X-Ray Micro-Diffraction ...................34 4 RESULTS AND DISCUSSION......................................................................37 A Lead Immobilization in Phosphate Amended Soil.................................37 B Solid Phase Speciation of Lead in Soil...................................................60 C Uranium Immobilization in Phosphate Amended Sediment ..................91 5 SUMMARY AND CONCLUSIONS ............................................................112 REFERENCES ................................................................................................................117 APPENDICES .................................................................................................................138 A Detail Calculation of pH-Dependent Solubility of Common Lead Minerals 138 B Soil Particle Selection for Synchrotron Analysis...........................................140 C Metal Trends in Batch Equilibration of the Uranium and Nickel Contaminated Sediment....................................................................................................142 vii LIST OF TABLES Page Table 1: Selected physical and chemical properties collected for the contaminated soil from a decommissioned lead-acid battery recycling plant (Jacksonville, FL)..25 Table 2: Selected physical and chemical properties of the contaminated sediment collected from the surface soil in the lower Tims Branch watershed on the Savannah River Site near Aiken, SC.................................................................26 Table 3: Sequential extraction steps used to asses trace element partitioning listed from least to most aggressive (Arey et al., 1999; Miller et al., 1986)........................31 Table 4: Composition of coatings recorded on ten mineral grains from a hydroxyapatite and calcium phytate amended contaminated soil collected at a decommissioned lead-acid battery recycling plant (Jacksonville, FL). ........................................62 Table 5: Crystalline lead-bearing and associated phases identified from eleven synchrotron micro-X-ray diffraction patterns obtained for untreated, Pb contaminated soil (Jacksonville, FL).................................................................70 Table 6: Crystalline lead-bearing and associated phases identified from nine synchrotron micro-X-ray diffraction patterns for Pb contaminated soil (Jacksonville, FL) treated with hydroxyapatite...............................................................................76 Table 7: Crystalline lead-bearing and associated phases identified from sixteen synchrotron micro-X-ray diffraction patterns for Pb contaminated soil (Jacksonville, FL) treated with precipitated calcium phytate............................83 viii LIST OF FIGURES Page Figure 1: Solubility of common lead minerals plotted as a function of soil pH................15 Figure 2: Phytic acid – myoinositol hexakis dihydrogen phosphate. ................................21 Figure 3: Effect of addition of calcium phytate (Ca-IP6),
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