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Nitric Acid-Tributyl Phosphate- Supercritical Carbon Dioxide System

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Nitric Acid-Tributyl Phosphate- Supercritical Carbon Dioxide System Investigation of the Uranimn(VI)-Nitric Acid-Tributyl Phosphate- Supercritical Carbon Dioxide System by Barbara Gauthier, B.Sc. Thesis submitted to the Faculty of Graduate Studies and Research in partial fulfilment of the requirements for the degree of Master of Science Department of Chemistry Carleton University Ottawa, Ontario June 24,2006 © Copyright 2006, B. Gauthier Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Library and Bibliotheque et Archives Canada Archives Canada Published Heritage Direction du Branch Patrimoine de I'edition 395 Wellington Street 395, rue Wellington Ottawa ON K1A 0N4 Ottawa ON K1A 0N4 Canada Canada Your file Votre reference ISBN: 978-0-494-18363-2 Our file Notre reference ISBN: 978-0-494-18363-2 NOTICE: AVIS: The author has granted a non­ L'auteur a accorde une licence non exclusive exclusive license allowing Library permettant a la Bibliotheque et Archives and Archives Canada to reproduce, Canada de reproduire, publier, archiver, publish, archive, preserve, conserve, sauvegarder, conserver, transmettre au public communicate to the public by par telecommunication ou par I'lnternet, preter, telecommunication or on the Internet,distribuer et vendre des theses partout dans loan, distribute and sell theses le monde, a des fins commerciales ou autres, worldwide, for commercial or non­ sur support microforme, papier, electronique commercial purposes, in microform, et/ou autres formats. paper, electronic and/or any other formats. The author retains copyright L'auteur conserve la propriete du droit d'auteur ownership and moral rights in et des droits moraux qui protege cette these. this thesis. Neither the thesis Ni la these ni des extraits substantiels de nor substantial extracts from it celle-ci ne doivent etre imprimes ou autrement may be printed or otherwise reproduits sans son autorisation. reproduced without the author's permission. In compliance with the Canadian Conformement a la loi canadienne Privacy Act some supporting sur la protection de la vie privee, forms may have been removed quelques formulaires secondaires from this thesis. ont ete enleves de cette these. While these forms may be included Bien que ces formulaires in the document page count, aient inclus dans la pagination, their removal does not represent il n'y aura aucun contenu manquant. any loss of content from the thesis. i *i Canada Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Abstract This work reports on the partitioning of the uranyl ion between nitric acid and supercritical carbon dioxide (SCCO 2 ) in the presence of tributyl phosphate (TBP) as a function of temperature and pressure. The distribution coefficients (Du) of uranium (0.2-2.5) were found to be highly dependent on the density of SCCO 2 . A decrease in Du was seen to correspond to a decrease in the concentration of TBP in the SCCO 2 phase while no corresponding decrease in the concentration of TBP in the aqueous phase was observed. The system was found to be non-ideal by comparison of the partition coefficients of TBP to the ratio of solubilities of TBP in pure SCCO 2 and water. In the uranium-nitric acid-scC 0 2 -TBP extraction system, up to 92% of the nitrate in SCCO 2 phase was due to the formation and partitioning of the HNO 3 TBP complex even though its distribution coefficient is two to three orders of magnitude lower than that of the U0 2 (N0 3 )2 '2 TBP complex. iii Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Acknowledgements Thank you to Dr. Bob Burk for the use of his lab and equipment, for his guidance throughout this project and excursions on the Shark. Thank you to Mohamed Abel Salaam, Helen Prochazka, Rana Zoka, Dave Blair, Amber Lemay, Alia Mahabir and Maria Russell for being such a fine lab group. Thank you to Jim Logan for his electronic expertise; to Tony O’Neil for always being willing to help; to Fred Cassalman for his TA support; to Peter Mosher, Keith Bourque and Wayne Archer for being so friendly; and to Elena, Tanya, Susa and Lisa for always being welcoming at stores and helpful in ordering needed supplies. Thank you to Dale Robertson for his personal attention to some difficult analyses and the excellent services of Paracel Laboratories; to Dr. DeSilva for his helpfulness and the use of his ICP-ES; to Clem Kazakoff for his MS expertise. Thank you to my father for his encouragement and support; to my sons Brett, Simon and Lewis for inspiring me with their courage and determination to follow their dreams. Thank you to Keith C. for impressing upon me the importance of finishing this degree; to Deirdre for her encouragement, receptive ear, expresso machine and last minute computer services; to Janet, Mona, Peggy, and Stuart and all my sailing buddies who were always willing to help restore my equilibrium out on Lac Deschenes. Thank you to Donna for her encouragement and views on how things look from the supervisor side of the equation. Thank you to Erika and Bob C. for foose training sessions in the Gatineau. There is nothing like climbing up to Pink’s Lake a few times on bike or skis to put life back into perspective. Without your support, this degree would not have been possible. iv Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Table of Contents Abstract iii Acknowledgements iv List of Tables xii List of Figures xiv List of Appendices xviii 1. Introduction 1.1. Supercritical Fluids - Introduction 1 1.1.1. Historical Background 1 1.1.2. Industrial Uses 2 1.2. Supercritical Fluids - Theory 4 1.2.1. Physical Properties of Supercritical Fluids 5 Density 6 Diffusivity 8 Viscosity 12 Polarity 15 Dielectric Constant 19 1.2.2. Gibbs Phase Rule 22 1.2.3. Solubility of Solids and Liquids in Supercritical Fluids 23 1.2.4. Thermodynamics of Solubility 25 1.3. Supercritical Carbon Dioxide 28 1.3.1. Phase Diagram of Carbon Dioxide 31 1.3.2. Carbon Dioxide/Water System 31 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. 1.3.2.1. Effect of Carbon Dioxide on pH of Aqueous Phase with change of Temperature and Pressure 31 1.3.2.2. Effect of Water on Supercritical Carbon Dioxide Phase 33 1.3,3. Solubilities in Supercritical Carbon Dioxide 34 1 .3.3.1, Case Study - Naphthalene 34 1.4. Extraction 3 9 1.4.1. Thermodynamics of Solubility 40 1.4.1.1, Liquid-liquid Extraction 41 1.4.1.2. Supercritical Carbon Dioxide Extraction 43 1.4.1.2.1. Effects of Temperature, Pressure, and pH 43 14.2. Complexation and Extraction of Uranium 44 14,2.1. Agents Used for Complexation of Uranium 44 1.4.2.1.1. Crown Ethers and Synergists 44 1.4.2.1.1.1. Literature Review of Extraction of Uranium with Crown Ethers and Synergists 46 1.4.2.1.2. Calixarene 47 14.2.1.2.1. Literature Review of Extraction of Uranium with Calixarene 48 1.4.2.1.3. Tributyl Phosphate 49 1.4.2.2. Literature Review of Extraction of Uranium 50 Historical Early Work 51 Dissolving and Reprocessing Spent Waste 52 Chemistry of Complexes 53 vi Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Ultrasonication 54 Separation of Metals 54 Distribution Coefficient of Uranium 55 Chelating Agents and Modifiers 56 Detection Methods 57 Solubility 58 Others 58 1.4.3. Industrial Processing of Uranium 59 1.5. Uranium / Tributyl Phosphate / Supercritical Carbon Dioxide System 59 1.5.1. Distribution of Species among Phases 60 1.6 . Selectivity of Extraction of Uranium to Supercritical Carbon Dioxide 61 1.6 .1. Theory of Selectivity 61 1.6.2. Importance of Selective Extraction of Uranium 62 1.7. Statement of Purpose 65 2. Equipment and Methods 67 2.1. Equipment 67 2.1.1. Description of Supercritical Fluid Extraction Apparatus 67 2.1.2. Sampling Apparatus for Solubility of Dibenzo-24-crown-8 in Supercritical Carbon Dioxide 72 2.1.3. Sampling Apparatus for Solubility of l,4,I0,13-Tetraoxo-7,16- diazacyclooctadecane 74 2.1.4. Sampling Apparatus for Solubility of Tributyl Phosphate 74 2.1.5. Sampling Apparatus for Uranium Extraction Experiments 76 vii Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. 2.1.6. Sampling Apparatus for Nitrate Concentration Experiments 79 2.2. Methods 80 2.2.1. Thermodynamic Properties of Complexing Agents 80 2.2.1.1. Solubility of 1,4,10,13-Tetraoxa-7,16- diazacyclooctadecane in Water 80 2.2.1.2. Solubility of 1,4,10,13-Tetraoxa-7,16- diazacyclooctadecane in Hexane 80 2.2.1.3. Solubility ofDibenzo-24-crown-8 in Supercritical Carbon Dioxide 81 2 2.1.4. Solubility of Tributyl Phosphate in Supercritical Carbon Dioxide 81 2.2.2. Extraction of Uranium with Crown Ethers, Calixarene, and Synergists 82 2.2.3. Extraction of Uranium with Tributyl Phosphate 84 2.2.3.1. Sampling of Aqueous Phase for Tributyl Phosphate at Atmospheric Pressure 84 2.2.3.2. Sampling of Aqueous Phase for Tributyl Phosphate at High pressure 8 6 2.2.3.3. Sampling of Aqueous Phase for Hydrogen Ion and Nitrate at Atmospheric Pressure 86 2.2.3.4. Sampling of Aqueous Phase for Nitrate at High Pressure 87 2.2.3.5. Sampling of Aqueous Phase for Hydrogen Ion and Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Uranium at High Pressure 8 8 3. Results and Discussion 89 3.1. Thermodynamic Properties of Complexing Agents 89 3.1.1.
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