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Characterisation and Remediation of Depleted Uranium Munitions Residues and Aqueous Chromium (VI)

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Characterisation and Remediation of Depleted Uranium Munitions Residues and Aqueous Chromium (VI) Characterisation and Remediation of Depleted Uranium Munitions Residues and Aqueous Chromium (VI) Daniel Edward Crean A thesis presented for the degree of Doctor of Philosophy October 2013 The University of Sheffield Faculty of Engineering Department of Materials Science and Engineering 2 Abstract Depleted uranium (DU) munitions particles and aqueous chromium(VI) are hazardous and challenging toxic metal contaminants. This thesis develops new approaches for remediating these pollutants, and provides insight into the long term behaviour of DU contamination by characterisation of environmentally aged residues. DU munitions particles exposed to the environment for ~25 years were studied using synchrotron X-ray chemical imaging. Micron-scale domains of U speciation were resolved in particles, indicating heterogeneous formation conditions and a variable extent of particle weathering. Two soil samples from a UK firing range were shown to have different U speciation, linked to environmentally mediated alteration in one soil. This study represents a novel application of X-ray chemical imaging to U in environmental materials, allowing domains of U(IV), U(V) and U(VI) to be resolved. An aged particle containing UFeO4 was shown to contain U(V), providing new evidence for the stability of this oxidation state under environmental conditions. Remediation of DU contaminated soils was studied by chemical extraction using bicarbonate, sulfric acid and citric acid lixivants. Single batch extraction in bicarbonate was the most effective, and able to remove 50% total DU. Residual particles showed partially leached microstructures, and the formation of secondary phases. An alternating pH multi-batch extraction was developed to promote secondary phase dissolution and improve the decontamination yield to a maximum of 87% total DU. In the last section, remediation of aqueous Cr(VI) was studied by reduction to insoluble Cr(III) using a hybrid Pd functionalised biomineral, magnetite. A means to increase the reactive capacity of the Pd-magnetite was demonstrated by addition of sodium formate, and the system performance was not affected by dissolved oxygen or nitrate. Using advanced spectroscopic and microscopic techniques, analysis of the reacted mineral showed Cr(III) was retained in the magnetite structure, and Pd recrystallisation resulted in a loss of reductive capacity. 3 Acknowledgements This thesis would not have been possible without the collaboration, input, advice and support of a number of people. First off, I want to sincerely thank my primary academic supervisor, Neil Hyatt, for the constant stream of technical advice, encouragement, guidance and inspiration - and for more than a few beers! Neil has always pushed me throughout my PhD, and opened more than a fair number of doors, and I’d really like to thank him for helping to make the past few years such an interesting and enjoyable time. I also thank my second supervisor, Francis Livens (University of Manchester) for his input, discussions and advice along the way, and for braving the Irish Sea to get stuck in with digging up soil at Eskmeals. I want to thank Daniel Grolimund and Camelia Borca at the Swiss Light Source for working with me on the microfocus X-ray experiments that make up a rather large portion of this thesis. It was a great opportunity to go out and do some work at SLS, and the efforts of Daniel and Camelia in obtaining and making the most out of this time are greatly appreciated. Thanks are also due to Mustafa Sajih (Manchester) for help getting the project going, Martin Stennett (Sheffield) for keeping me sane on beam time and help with all things XAS, and Paul Heath (Sheffield) for giving up his time to help out on our second trip to SLS. The final experimental chapter of this thesis is the product of some work done in the School of Earth and Atmospheric Sciences at the University of Manchester at the start of my PhD. I’d like to particularly thank Vicky Coker for her help in every aspect of this work, Jon Lloyd for his supervision during this time, and the geomicrobiology group for making it a great place to start! I’ve been very fortunate to be part of two interesting and dynamic research groups, the Immobilisation Science Laboratory here in Sheffield, and the Centre for Radiochemistry Research at the University of Manchester. Thanks to all the people who I’ve shared office space with over the past three years for plenty of welcome distraction, interesting chat and seriously strong rounds of coffee. Particular nods of thanks to the many ISL people - Kris, Paul H, Sam, 4 Martin, Jimmy, Claire, Amy, Laura G, Neda, Dans B and B, Swifty, Silvia and Oday, and Manchester chemists - Dan W, Kurt, Chris G, Mustafa, and Saif who have made the past few years substantially more fun than they otherwise might have been! The Engineering and Physical Sciences Research Council (EPSRC) are thanked for providing funding for my studentship through the Nuclear First DTC grant. Funding for the Swiss Light Source was provided through the Actinet i3 project, funded by the European Commission/Euratom. The work in Chapter 7 was supported by Nametech, a Collaborative Project co-funded by the Research DG of the European Commission, the EPSRC University of Manchester Knowledge Transfer Account (KTA) and the Leeds EPSRC Nanoscience and Nanotechnology Research Equipment Facility (LENNF). I want to say thanks to my family (Mum, Dad, Tom and Hannah) and friends for their support during my PhD studies. And finally to Emma, for her love and support throughout. 5 Table of Contents Abstract ......................................................................................................................................... 3 Acknowledgements ....................................................................................................................... 3 Table of Contents .......................................................................................................................... 6 List of figures with captions ........................................................................................................ 13 List of tables with captions .......................................................................................................... 17 Chapter 1 - Introduction .............................................................................................. 18 1.1 Background........................................................................................................................ 18 1.2 Depleted Uranium Particles - Characterisation and Remediation ..................................... 18 1.3 Remediation of Aqueous Chromium (VI) Contamination ................................................ 19 1.4 Aims and Objectives .......................................................................................................... 20 1.5 Thesis Structure ................................................................................................................. 21 1.6 References ......................................................................................................................... 22 Chapter 2 – Literature Review ................................................................................... 25 2.0 Introduction ....................................................................................................................... 25 2.1 Depleted Uranium Munitions Particles ............................................................................. 25 2.1.1 Uranium in the Environment ...................................................................................... 25 2.1.2 Natural and Depleted Uranium ................................................................................... 27 2.1.3 Depleted Uranium Munitions ..................................................................................... 28 2.1.4 DU Munitions in the Environment ............................................................................. 28 2.1.5 Characterisation of Depleted Uranium Munitions Particles ....................................... 30 2.1.5.1 Composition and Uranium Speciation ................................................................. 30 2.1.5.2 Morphology and Structure ................................................................................... 31 2.1.5.3 Formation Conditions .......................................................................................... 31 2.5.1.4 Short Term Environmental Stability .................................................................... 32 2.2 Remediation of Land Contaminated with DU Munitions Residues .................................. 32 2.2.1 Risks Associated with Exposure to DU ...................................................................... 32 2.2.2 Drivers for Remediation ............................................................................................. 33 6 2.2.3 Physical Separation Processes ................................................................................... 34 2.2.4 Chemical Extraction by Soil Washing ....................................................................... 35 2.2.4.1 Carbonate Leaching ............................................................................................ 36 2.2.4.2 Citrate Leaching .................................................................................................. 37 2.2.4.3 Mineral Acid Leaching ......................................................................................
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