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Decay Scheme Data of Neptunium Isotopes

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Decay Scheme Data of Neptunium Isotopes Decay Scheme Data of Neptunium Isotopes A thesis submitted to the University of London for the degree of Doctor of Philosophy Ian Michael Lowles July 1991 Imperial College Reactor Centre Imperial College of Science, Technology and Medicine Dedicated to my Parents Persons attempting to find a motive in this narrative will be prosecuted; persons attempting to find a moral in it will be banished; persons attempting to find a plot in it will be shot. Mark Twain The Adventures of Huckleberry Finn. Acknowledgments I would like to thank Dr. T.D. MacMahon for the help and encouragement he has given during the course of this work, but above all for his friendship. I am very grateful to Mr. R. Benzing, Dr. A.H. Naboulsi, Mr. I.W. Sinclair and Dr. A.W. Glauert for their many useful suggestions and comments, in areas which included: spectroscopy; statistics; chemistry and computing. I would also like to thank the Reactor Operations staff, without whose help much of this work would have been impossible. Thanks also to Dr. A.J. Fudge, Mr. R.A.P. Wiltshire and Mr. I.D. Jackson for their help and advice during my time at Harwell. Finally, I must thank Alison Smith whose love and support has helped me through the difficult times in this work. She has also had the unenviable task of reading the rough drafts of this thesis, and for that she must be pitied. Abstract The purpose of this research was to investigate the decay scheme parameters fy\n ryx o of Np and Np, and in particular their half-lives and gamma-ray emission probabilities. The work was prompted by the International Atomic Energy Agency, Coordinated Research Programme (IAEA-CRP) request for more accurate actinide decay data in order to: i. assess accurately the effects of these data on thermal and fast reactor fuel cycles ii. aid in the evaluation of nuclear waste management procedures iii. provide reliable data for nuclear safeguards iv. extend the knowledge of actinide decay parameters required in scientific research Several authors have recently reported precise measurements of alpha- particle, gamma-ray and conversion electron emission probabilities in the decay of 937 Np. An attempt to construct a self-consistent decay scheme from these data has failed. The author believes that the anomalous decay scheme is due, not to what has been measured, but is a consequence of what has previously gone undetected. Prime candidates for these missing data are several very low-energy, high-intensity gamma-ray transitions. An experiment was undertaken to analyse the low-energy gamma-ray spectrum of Np, in an attempt to determine the existence of these transitions, and so resolve the anomalous decay scheme. The only available precise measurement of the half-life of Np is that of Brauer et al. (1960). As a consequence of this radionuclide's importance in fission reactors, the IAEA-CRP requested a confirmatory measurement of the half-life of 237Np. In this present determination the specific activity of 37 alpha-particle sources, prepared from known weights of high purity Np solution, have been measured. Accurate concentration analysis of the solution was provided by controlled-potential coulometry. Source activities were measured by a-particle counting in two gas flow proportional counters of known geometry. The measured specific activity and half-life are in excellent agreement with the value reported by Brauer et al. (1960). Moreover, the validity of many of the assumptions used in this present measurement have been verified experimentally. Attempts to produce a self-consistent decay scheme for Np have relied exclusively on gamma-ray emission probability measurements. However, the precision with which the intensity of the principle gamma-ray transition has been measured, has varied between 1.45 and 3.80%. This was considered unacceptable by the IAEA-CRP, who called for a further measurement of the gamma-ray emission probabilities of 239Np, requesting a precision of 1% for the principle transition. In this present determination, Np has been prepared by radiochemical noo separation from neutron irradiated U, and by separation from its equilibrium parent, 243Am. Photopeak areas were determined using two different analytical peak fitting routines and source activities were measured using a 4jtp-y coincidence system, which utilised the efficiency extrapolation technique. The measured gamma-ray emission probabilities are consistent with those of previous workers. Moreover, the intensity of the principle transition has been measured with a precision of greater than 1%, satisfying the original aims of the IAEA-CRP. Contents 4 Contents Acknowledgements ....... 1 Abstract ........ 2 Contents ........ 4 List of Tables ........ 8 List of Figures ....... 10 1. Introduction ....... 13 1.1 The I A E A - C R P ............................................................ 13 1.2 Nuclear Decay Data of Neptunium Isotopes . 14 2. The Chemistry of Neptunium .... 18 2.1 The Placement of Actinides in the Periodic Table 18 2.2 The Discovery of Neptunium ..... 18 2.3 The Similarities Between the Lanthanide and Actinide Elements 22 2.3.1 Oxidation States ..... 22 2.3.2 The Lanthanide and Actinide Contractions 22 2.4 The Solution Chemistry of Neptunium 25 2.5 Ion-Exchange Chromatography .... 29 2.6 Separation of Neptunium by Ion—Exchange Chromatography 33 3. Counting and Spectroscopy Techniques . 38 3.1 Introduction ....... 38 3.2 Proportional Counters ...... 38 3.2.1 Operating Voltage ..... 39 3.2.2 Alpha-Particle Counting .... 41 3.2.3 Beta-Particle Counting .... 43 Contents 5 3.3 Solid State Detectors ....... 45 3.3.1 Gamma-ray Interactions ..... 45 3.3.2 Photoelectric Absorption ..... 45 3.3.3 Compton Scattering ...... 46 3.3.4 Pair Production ...... 47 3.3.5 Nal(Tl) Scintillation Detectors ..... 48 3.3.6 Semiconductor Detectors . 51 3.3.7 Peak Area Determination ..... 55 3.3.8 Sampo Routine ...... 57 3.3.9 Omnigam Routine ...... 57 3.3.10 Gamanal Routine ...... 59 3.3.11 Peak Anomalies ...... 60 3.3.12 Detector Efficiency . 61 3.4 Coincidence Counting ....... 67 3.4.1 Conversion Electrons ...... 68 3.4.2 Gamma Sensitivity of the p-detector .... 69 3.4.3 Beta Sensitivity of the y-detector . 70 3.4.4 Complex Decay Schemes ..... 70 3.4.5 47tP~y Coincidence System . 71 3.4.6 Dead Time and Resolving Time Corrections . 74 3.4.7 Corrections to the Coincidence Formulae . 77 3.4.8 Data Analysis . 78 4. Low-energy Gamma-ray Analysis of Np . 80 4.1 Introduction ........ 80 4.2 Review of Alpha-Particle Decay Data .... 80 4.2.1 Review of Gamma-Ray Decay Data .... 86 4.2.2 Review of Alpha-Gamma Coincidence Data . 88 4.2.3 Review of Gamma-Gamma Coincidence Data . 91 Contents 6 4.2.4 Review of Conversion Electron Data 95 4.3 Evaluation .... 96 4.4 Experimental .... 99 4.5 Results ..... 106 4.6 Discussion .... 109 4.7 Conclusion .... 113 5. The Half-life of 237Np 114 5.1. Introduction ..... 114 5.2 Review of Previous Measurements 114 5.3 Controlled-Potential Coulometry 116 5.4 Experimental ..... 121 5.4.1 Preparation of Np Standards 121 5.4.2 The Analysis of Neptunium by Controlled-Potential Coulometry 122 5.4.3 Source Preparation 124 5.5 Results ...... 126 5.5.1 Concentration Analysis 126 5.5.2 Source Count Rate 127 5.5.3 Specific Activity 127 5.6 Discussion ..... 136 5.6.1 Alpha-Particle Self-Absorption Correction 136 5.6.2 Source Uniformity Correction . 136 5.6.3 Beta-Particle Sensitivity 140 5.6.4 Alpha-Particle Backscattering . 140 5.7 Conclusion ..... 144 6. Gamma-ray Emission Probabilities of 239Np 145 6.1 Introduction ..... 145 Contents 7 6.2 Review of Previous Measurements . 145 6.2.1 Half-life Measurements ..... 145 6.2.2 (3-Particle Emission Probabilities .... 145 6.2.3 Internal Conversion Coefficients . 147 6.2.4 y-ray Emission Probability Measurements . 147 6.3 Experimental . 151 6.3.1 Thermal Neutron Irradiation of 238U02 Spheres . 151 6.3.2 Thermal Neutron Irradiation of 238U02 Powder . 155 6.3.3 Separation 239Np from242Am . 159 6.4 Results ......... 161 6.4.1 Absolute Disintegration Rates . 161 6.4.2 Absolute y-ray Emission Probabilities . 163 6.5 Conclusion . 168 7. Summary and Conclusions ...... 169 References . 173 Contents 8 List of Tables 1.1 Nuclear Decay Data and Their Applications .... 15 2.1 The Periodic Table ....... 20 2.2 Electronic Configuration of the Elements . 21 2.3 The Oxidation States of the Lanthanides and Actinides . 23 2.4 Neptunium Ions in Aqueous Solution ..... 28 3.1 Isotopes Used for the Calibration of a Semiconductor Detector . 63 4.1 Measured a-particle Emission Probabilities . 81 4.2 Evaluated a-particle Emission Probabilities .... 83 4.3 a-particle Emission Probabilities determined by CBNM and CIEMAT, Together with Their Recommended Pa Values . 85 4.4 Energy Levels of 233Pa ....... 85 4.5 Absolute y-ray Emission Probabilities ..... 87 4.6 a-y Coincidence Data (Gonzalez et al., 1979) .... 89 4.7(a) y-y Coincidence Data (Skalsey and Connor, 1976) . 92 4.7(b) y-y Coincidence Data (Gonzalez et al., 1979) . 92 4.7(c) y-y Coincidence Data (Woods et al., 1988) .... 92 4.8 Conversion Electron Measurements of Woods et al. (1988) . 95 4.9 Total Transition Probabilities of 237Np ..... 96 4.10 Purity of the Neptunium Sample ..... 99 4.11 Measured Relative y-ray Emission Probabilities of'I'M Np Normalised to P-^(86.5) = 12.3% . 108 4.12 ICC's for the 5.18 keV T r a n s itio n................................................I ll 4.13 ICC's for the 8.69 keV Transition . I ll 4.14 ICC's for the 36.20 keV T ran sition................................................I ll Contents 5.1 Purity of the Neptunium Sample 5.2 Results of the CPC Analysis ...
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