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Download (4Mb) A Thesis Submitted for the Degree of PhD at the University of Warwick Permanent WRAP URL: http://wrap.warwick.ac.uk/108024/ Copyright and reuse: This thesis is made available online and is protected by original copyright. Please scroll down to view the document itself. Please refer to the repository record for this item for information to help you to cite it. Our policy information is available from the repository home page. For more information, please contact the WRAP Team at: [email protected] warwick.ac.uk/lib-publications Chain Processes in the Tc(VII)-Catalysed Oxidation of Hydrazine by Nitrate and Perchlorate Ions by Aubrey Maurice Thyer A thesis submitted to the University of Warwick in partial fulfilaent of the requirements for the degree of Doctor of Philosophy Department of Chemistry University of Warwick Coventry CV4 7AL May 1990 ACKNOWLEDGEMENTS I uould like to thank Professor T. J. Keep for his encouragement and continued Interest throughout the work and also for providing le with the opportunity to study for ey Ph.D. I thank Dr. J. B. Raynor and Dr. D. Rehorek for conducting the e.s.r experleents. I acknowledge financial support froe the Science and Engineering Research Council and British Nuclear Fuels p.l.c. (Sel lafleld) In the fore of a C.A.S.E. studentship. I would also like to thank ey Industrial supervisor Dr. P. D. Wilson for his help with soee of the technical problems of the work and for providing the basic computer simulation program. I thank Dr. M. Kennedy and other members of the Mining Explosives Section at Buxton. I uould like to thank my fellow-student, Mr. P. A. Read for his many helpful comments on my work whilst In the laboratory and also for his help and that of Miss J. Ward for acting as couriers for draft chapters of ay thesis. Finally I would like to thank Mrs. J. Poole for typing this thes1s . ABBREVIATIONS 1AR column 1A raffinate or waste solution IAS column 1A solvent scrubbing state. 1AX column LA solvent extraction stage BNFL British Nuclear Fuels pic 1 BP. solvent product from column IB containing purified Pu 1BJCX. column IB second solvent extraction stage. Column IA the first bank of three solvent extraction columns. Column IB the second bank of three solvent extraction columns. Column 1C the third bank of three solvent extraction columns. 1-C.R. spent solvent from column 1C 1CU an aqueous nitric acid stream from column 1C containing purified uranium. CAT. electron spin resonance spectroscopy FP*s fission products g.c.m.s. gas chromatography mass spectroscopy G Gauss HA. high active, highly radioactive HAN hydroxyamine nitrate Magnox fuel a fuel made of non-enriched uranium metal which contains less than 1% for use in Magnox reactors, minutes ms millisecond Nox nitrogen oxides OJC odourless kerosine org organic oxidised oxide fuel a fuel for use in gas cooled reactors or light water reactors which consists of uranium oxide pellets which have been enriched to increase the content to 2-3% PBN benzylidine nitrone PDMAB para-dimethyl aminobenzaldéhyde P.R. plutonium purification PUREX Process Plutonium Uranium Recovery by Solvent Extraction. Raffinate term for discribing a waste solution in nuclear fuel reprocessing s seconds THORP Thermal Oxide Reprocessing Plant THORP Process modified PUREX process to be utilised in the THORP plant TBP Tri-n-butylphosphate UP uranium purification U.V.-vis. ultra violet and visible spectroscopy absorption maximum of U.V. or visible light by a xmax molecule or ion ionic strength of a solution ABSTRACT Studies of the reaction between pertechnetate Ion and hydrazine In solutions In several different acids have been carried out In order to establish the reaction mechanism and, where possible, the Individual rate constants of each step. Computer simulation of the expertaental data has been utilised to enable the foraulatlon of reaction scheaes for these very coaplex chain reactions. In nitric acid the reaction typically exhibits an Induction period of variable length depending on the acidity and concentrations of nitrate, hydrazine and technetlua. This is followed by a stage of rapid loss of hydrazine froa the solution due to Its oxidation by TcVI, while the Tc*v produced is re-oxidised to TcVI by nitrate. The termination step is considered to be the acid-catalysed oxidation of TcVI to TCO4- by nitrate. The effect of Increasing acidity Is to Increase the length of the induction stage and to decrease the rate of hydrazine oxidation during the fast reaction stage* this causes the reaction to be terminated with increasingly greater residual concentrations of unoxidlzed hydrazine* at 5 aol da-3 HN03 no loss of N2h4 from the solution is observed. Replacing nitric acid by acids such as HCIO4 , HBF4 , HC1 or CF3COOH shows that nitric acid Is unique in Its inhibiting effect on the hydrazine destruction reaction. In the presence of these acids the length of the Induction stage is decreased, and the rate of the fast reaction stage is increased, with Increasing acidity, l.e. In direct contrast to the situation for HNO3 media A reaction schene has been proposed for the coaplex of processes that occur in perchloric acid or tetrafluoroborlc acld-sodlua nitrate aedia. In these systeas It is proposed that the increases In the reaction rates with increasing acidity is due to protonatlon of the highly reactive TcVI species, which is stabised towards oxidation to Tc04~, l.e. the essence of the terainatlon process. The kinetic situation in perchloric acid appears to be even sore coaplex, and several interaedlate complexes of TcIV appear to be produced. It is proposed that the sharp peak in the tiae-proflle of the concentration of TcIV at the onset of the fast reaction stage is due to the presence of the TcO(OH)2 coaplex. In later stages of the reaction the hydroxide ligands are replaced by chloride ion, which is produced by the reduction of perchlorate. The oxochlorotechnetlua(IV) coaplexes so produced are aore resistant to oxidation than siaple oxo coaplexes and are not re-oxidised to Tc04~ on terainatlon of the reaction. The coaputer siaulation of these results has led us to invoke the production of an interned!ate Tc* 1 1 coaplex. The results of the work in HNO3 and HC104 aedia were presented as an oral coaaunicatlon at the Third International Syaposlua on Technetiua in Chenlstry and Nuclear Medicine held at Montegrotto Terae in Septeaber 1989. The abstract included in the conference proceedings is presented in the appendix. CONTENTS Page Chapter 1 Introduction 1 - 3 3 1.1 Isotopes of Technetium 1 - 4 12 Redox Chemistry of Technetium 4 - 1 4 13 The Reprocessing of Nuclear Fuel 15 - 22 1.4 The Coextraction of Technetium 22 - 25 1.5 Reactions of Hydrazine with Metal Ions 2 5 -2 7 1.6 The Technetium-Hydrazine Reaction 2 8 -3 2 1.7 Objects of the Present Work 32 - 33 Chapter 2 Kinetics of the TcO^'-Hydrazinc Reaction in Nitrate Containing Media 3 4 -7 7 2.1 The Effect of Nitric Acid Concentration 35 • 37 2.1.1 The Effect of Nitric Acid at [Tc] - 7 2 x KT4 mol dm’3 37 - 38 2.1.2 The Effect of Nitric Acid at [Tel “ 1-6 x 10’3 mol dm*3 42 - 43 22.1 Study of the Acidity Dependence in a Tc-N2H4-0.6 mol dm’3 NaN03-HBF4 System 43 - 52 2^2 Study of the Acidity Dependence in a Tc-N2H4-2.0 mol dm'3 NaN03-HBF4 System 52 - 55 23 The Effect of Nitrate Ion on the Tc-Hydrazine Reaction (using NaBF4 to maintain ionic strength) 56 - 58 2.4 Computer Simulation of the Tc-Hydrazine Reaction in a Nitric Acid-NaN03 System 59 - 69 2.4.1 Simulation of the Effects of Nitric Acid 60 - 61 2.4.2 Simulation of Varying the Initial Concentration of Hydrazine 61 - 64 Page 2.43 Simulation of the Effects if Technetion Concentration on the Hydrazine Oxidation Profile 64 - 68 2.4.4 Simulation o f the Effects of adding Uranium or Plutonium on the Kinetics of the Tc-Hydrazine Reaction 68 * 69 23 Discussion 70 - 77 2.6 Conclusion 7 7 -7 8 Chapter 3 The Effects of Added Anions on the Tc-Hydrazine Reaction Kinetics and Profiles 7 9 -9 6 3.1 The Effect of Nitrate Ion on the Tc-Hydrazine Reaction (using N a d 0 4 to maintain ionic strength) 79 - 84 32 The Effect on Reaction Kinetics of Increasing Ionic Strength using Sodium Perchlorate 85 - 92 33 The Tc-Hydrazine Reaction in Mixed Nitric Acid- Hydrochloric Acid Systems 93 - 94 3.4 Conclusion 95-96 Chapter 4 The Tc-Hydrazine Reaction in Perchlorate Media 97 - 137 4.1 The Tc-Hydrazine Reaction in Perchlorate Media with an ionic strength of 1.1 mol dm'^ 9 8 - 102 42 The Effect of Perchloric Acid Concentration on the Tc-Hydrazine Reaction in Perchlorate Media with an Ionic Strength of 7.0 mol dm*^ 102 - 104 43 The Use o f U.V.-Visible Spectroscopy to Monitor the Rate of Tc04* ion reduction during the early Stages of the Reaction 104 - 108 4.4 The Effect of Temperature on the Kinetics of the Tc-Hydrazine Reaction in Perchlorate Media 109 - 113 Page 45 The Effects on Reaction Kinetics of Adding Chlorate and Hypochlorite to Tc04 '-N2 H4 -HOO4 Solutions 114 - 120 4.6 The Formation of Coloured Complexes during the Tc-Hydrazine Reaction in Perchloric Acid 120 • 128 4.7 The Computer Simulation of the Tc-Hydrazine Reaction in H a 0 4 -NaQ04 Systems 128 - 131 4.8 Discussion 132 - 135 4.9 Conclusion 136 - 137 Chapter 5 A Study of the Reaction Kinetics and Intermediate Species Produced during the Tc-Hydrazine Reaction in the presence of a Variety o f Adds 138 • 152 5.1 An investigation into the Reaction Kinetics of the Tc-Hydrazine Reaction in Trifluoroacetic Add 138 - 142 52 An Investigation into the Reaction Kinetics of the Tc-Hydrazine Reaction in Tetrafluoroboric Acid 143 - 145 53 An Investigation into the Nature of the Tc*v Complexes produced by the Reduction of Tc04* by Hydrazine in Hydrochloric Acid 146 - 148 5.4 Conclusion 148 • 152 Chapter 6 Reactions between Technetium and the Azide Ion 153-162 6.1 The Tc^-Azide Reaction 153 - 157 6.1.1 Discussion 157 • 158 6.2 The Destruction of Azide by Photolysis in NaN3 -Tc04 '-H N 0 3 Solutions 158 - 162 1.1 Isotopes of Technetium Technetium, element 43, was the first element to be produced artificially before it was discovered in nature.
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