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Options for Treatment of Legacy and Advanced OPTIONS FOR TREATMENT OF LEGACY AND ADVANCED NUCLEAR FUELS A thesis submitted to the University of Manchester for the degree of in the Faculty of Engineering and Physical Sciences. 2014 CHRIS MAHER SCHOOL OF CHEMICAL ENGINEERING AND ANALYTICAL SCIENCE TABLE OF CONTENTS 1. INTRODUCTION ............................................................................ 22 2. OVERALL OBJECTIVES .................................................................. 26 3. TECHNOLOGY FOR THE HEAD-END TREATMENT OF LEGACY, CURRENT AND FUEL ADVANCED NUCLEAR FUELS ......................... 27 3.1. Aims and objectives .................................................................. 27 3.2. Science and technology of Head-End and influence of potential future challenges ............................................................................... 27 3.2.1. Introduction ..................................................................... 28 3.2.2. Current practice ................................................................ 31 3.2.2.1. Fuel conditioning ....................................................... 32 3.2.2.2. Dissolution ............................................................... 33 3.2.2.3. Dissolver liquor conditioning ....................................... 40 3.2.2.4. Accountancy and buffer storage .................................. 42 3.2.3. Potential developments to meet future challenges ................. 43 3.2.3.1. Dissolution chemistry of alternative fuel types .............. 44 3.2.3.2. Fuel conditioning - potential benefits of fuel pre-treatment .............................................................................. 49 3.2.3.3. Developments in dissolution chemistry and technology .. 54 3.2.4. Summary and future developments ..................................... 57 3.3. Summary of key issues in the development of flowsheets for processing legacy, current and future advanced fuels .................... 58 4. DIRECT DISSOLUTION OF OXIDE IN NITRIC ACID ....................... 60 4.1. Summary of literature relevant to the direct dissolution of uranium, plutonium and mixed uranium plutonium oxides in nitric acid ......... 60 4.1.1. Background chemistry ....................................................... 60 4.1.1.1. Nitric acid ................................................................ 60 4.1.1.2. Chemistry of uranium oxide ....................................... 65 4.1.1.3. Chemistry of plutonium oxide ..................................... 67 4.1.1.4. Chemistry of mixed uranium plutonium oxides .............. 67 4.1.2. Dissolution chemistry ........................................................ 68 4.1.2.1. Dissolution chemistry of metals .................................. 68 4.1.2.2. Chemistry of oxide dissolution .................................... 70 4.1.2.3. Uranium oxide dissolution in nitric acid ........................ 71 4.1.2.4. Plutonium oxide dissolution in nitric acid ...................... 75 4.1.2.5. Mixed uranium plutonium dioxide dissolution in nitric acid .............................................................................. 75 4.1.3. Summary of dissolution literature ....................................... 77 4.2. Aims and objectives .................................................................. 78 2 4.3. Experimental ............................................................................ 79 4.3.1. Dissolution apparatus and methodology ............................... 79 4.3.2. Off-line analytical methods ................................................. 85 4.3.2.1. Uranium dioxide experiments ..................................... 85 4.3.2.2. MOx experiments ...................................................... 86 4.3.3. Characterisation of materials .............................................. 86 4.3.3.1. Uranium dioxide powders ........................................... 86 4.3.3.2. MOx powder ............................................................. 87 4.3.3.3. MOx pellets .............................................................. 88 4.4. The thermodynamics of actinide dioxide dissolution in nitric acid .... 88 4.4.1. Introduction ..................................................................... 88 4.4.2. Methodology ..................................................................... 89 4.4.3. Dissolution in nitric acid ..................................................... 90 4.4.3.1. Individual actinide dioxides ........................................ 90 4.4.3.2. Mixed uranium plutonium dioxide ................................ 93 4.4.4. Enhanced dissolution with oxidising and reducing agents ....... 95 4.4.5. Summary ....................................................................... 100 4.5. The effect of stirring and sparging upon uranium dioxide dissolution in nitric acid ............................................................................... 101 4.5.1. Introduction ................................................................... 101 4.5.2. Experimental .................................................................. 103 4.5.2.1. Materials ................................................................ 103 4.5.2.2. Apparatus and methodology ..................................... 103 4.5.2.3. Analysis methods .................................................... 104 4.5.3. Results and Discussion .................................................... 105 4.5.4. Summary ....................................................................... 110 4.6. The role of nitrous acid in the dissolution of uranium plutonium mixed oxide powder ......................................................................... 110 4.6.1. Introduction ................................................................... 110 4.6.2. Experimental .................................................................. 112 4.6.2.1. Materials ................................................................ 112 4.6.2.2. Apparatus and methodology ..................................... 112 4.6.2.3. Analysis methods .................................................... 113 4.6.3. Results and Discussion .................................................... 113 4.6.4. Summary ....................................................................... 120 4.7. Dissolution kinetics of 5 % plutonium content mixed oxide pellets in nitric acid ............................................................................... 121 4.7.1. Introduction ................................................................... 121 4.7.2. Experimental .................................................................. 122 3 4.7.2.1. Materials ................................................................ 122 4.7.2.2. Apparatus and methodology ..................................... 122 4.7.2.3. Analysis methods .................................................... 123 4.7.2.4. Dissolution rate interpretation .................................. 123 4.7.3. Results and Discussion .................................................... 124 4.7.3.1. Multi-component UV-Vis calibration ........................... 124 4.7.3.2. Effect of cell conditions ............................................ 125 4.7.3.3. Effect of nitric and nitrous acid concentration ............. 127 4.7.3.4. Effect of temperature .............................................. 129 4.7.3.5. Comparison of dissolution rates with previously published results ................................................................... 131 4.7.4. Summary ....................................................................... 132 4.8. Summary of direct dissolution of oxides in nitric acid ................... 133 5. APPLICATION OF MEDIATED ELECTROCHEMICAL OF SILVER(II) FOR FUEL DISSOLUTION ............................................................. 135 5.1. Summary of literature relating to mediated electrochemical dissolution ............................................................................. 135 5.1.1. Review of the development leading MEO dissolution processes for plutonium dioxide ...................................................... 135 5.1.1.1. Silver(II) chemistry in nitric acid ............................... 138 5.1.2. Electrochemical generation of silver(II).............................. 142 5.1.3. Summary of silver(II) mediated electrochemical processes .. 145 5.2. Aims and objectives ................................................................ 145 5.3. Experimental .......................................................................... 148 5.3.1. Apparatus and methods ................................................... 148 5.3.1.1. Glassware .............................................................. 148 5.3.1.2. Power supply and voltage meters .............................. 151 5.3.1.3. Electrodes .............................................................. 153 5.3.1.4. Redox potential measurements ................................. 154 5.3.1.5. Temperature measurement ...................................... 155 5.3.1.6. Inline UV-Vis spectrometry ....................................... 155 5.3.1.7. Silver(II) by sampling .............................................. 155 5.3.2. Initial testing .................................................................. 156 5.3.3. Linear Staircase Voltammetry ........................................... 157 5.3.4. Bulk electrolysis .............................................................. 159 5.3.5. Dissolution apparatus and methodology ............................. 163 5.4.
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