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The Kinetic and Radiolytic Aspects of Control of the Redox Speciation of Neptunium in Solutions of Nitric Acid

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The Kinetic and Radiolytic Aspects of Control of the Redox Speciation of Neptunium in Solutions of Nitric Acid AN ABSTRACT OF THE DISSERTATION OF Martin Precek for the degree of Doctor of Philosophy in Chemistry presented on August 29, 2012. Title: The Kinetic and Radiolytic Aspects of Control of the Redox Speciation of Neptunium in Solutions of Nitric Acid Abstract approved: ________________________________________________ Alena Paulenova Neptunium, with its rich redox chemistry, has a special position in the chemistry of actinides. With a decades-long history of development of aqueous separation methods for used nuclear fuel (UNF), management of neptunium remains an unresolved issue because of its not clearly defined redox speciation. Neptunium is present in two, pentavalent (V) and hexavalent (VI) oxidation states, both in their dioxocation O=Np=O neptunyl form, which differ greatly in their solvent extraction behavior. While the neptunium(VI) dioxocation is being very well extracted, the dioxocation of pentavalent neptunium is practically non-extractable by an organic solvent. As a result, neptunium is not well separated and remains distributed in both organic and aqueous extraction phases. The aim of this study was to develop or enhance the understanding of several key topics governing the redox behavior of neptunium in nitric acid medium, which are of vital importance for the engineering design of industrial-scale liquid-liquid separation systems. In this work, reactions of neptunium(V) and (VI) with vanadium(V) and acetohydroxamic acid - two redox agents envisioned for adjusting the neptunium oxidation state in aqueous separations – were studied in order to determine their kinetic characteristics, rate laws and rate constants, as a function of temperature and nitric acid concentration. Further were analyzed the interactions of neptunium(V) and (VI) with nitrous acid, which is formed as a product of radiolytic degradation of nitric acid caused by high levels of radioactivity present in such systems. Once HNO3 is distributed between both the aqueous solutions and organic solvent, nitrous acid is also formed in both phases and has a key influence on redox speciation of neptunium; therefore, the effects of gamma-radiation on the redox speciation of neptunium were investigated. The work also includes the results of examination of scavenging of nitrous acid by hydrogen peroxide, which is generated along with nitrous acid during radiolysis of aqueous solutions of nitric acid, and also by chemical reactions with added scavenging agents (methylurea, acetohydroxamic acid). ©Copyright by Martin Precek August 29, 2012 All Rights Reserved The Kinetic and Radiolytic Aspects of Control of the Redox Speciation of Neptunium in Solutions of Nitric Acid by Martin Precek A DISSERTATION submitted to Oregon State University in partial fulfillment of the requirements for the degree of Doctor of Philosophy Presented August 29, 2012 Commencement June 2013 Doctor of Philosophy dissertation of Martin Precek presented on August 29, 2012. APPROVED: Major Professor, representing Chemistry Chair of the Department of Chemistry Dean of the Graduate School I understand that my dissertation will become part of the permanent collection of Oregon State University libraries. My signature below authorizes release of my dissertation to any reader upon request. Martin Precek, Author ACKNOWLEDGEMENTS Firstly, I would like to express my deep appreciation to Dr. Alena Paulenova, who has more than fulfilled her duties of an academic advisor, who has never failed in arranging for my financial support, and who has always made herself available to provide academic and personal guidance through my doctoral studies. I would also like to extend my appreciation to the past and present members of my doctoral committee at OSU: Dr. James D. Ingle, Dr. Walter D. Loveland, Dr. Philip R. Watson, Dr. Manish Gupta, Dr. Taifo Mahmud, and Dr. Abi T. Farsoni, who have found time in their busy schedules to supervise the progression of my degree. My additional thanks are directed at my collaborators and co-advisors Dr. Bruce J. Mincher from the Idaho National Laboratory and Dr. Stephen Mezyk from the California State University, Long Beach, for creating a wonderful and exciting atmosphere of cooperation and for treating me as their equal. I have been very lucky in getting to work in the wonderful collective of Dr. Paulenova’s research group. I would like to especially acknowledge the support I had from the following colleagues: Dr. Peter Tkac (the group “postdoc”), graduate students M. Alex Brown, Vanessa E. Holfeltz, Joseph L. Lapka, and Brent S. Matteson, and also from undergraduate researchers Kyle C. Hartig, Nathan Knapp, and Corey R. Wright. My work would not be possible without the support work of the personnel of the OSU Radiation Center, especially Scott A. Menn who facilitated my use of the Co-60 irradiator and provided necessary radiation protection oversight over my work. I also address many thanks to the community of people of the town of Corvallis, Oregon, especially to the international students of the European Student Association of OSU, to Stephen Howell for the I.H.O.P., to Penelope Wollf and the Pro Musica Corvallis String Orchestra, and to the Rebhuhn family, all of whom have allowed me to develop a very fulfilling social life in what was initially a strange and foreign country to me. Last, but not least, I need to express my thanks to the members of my family, especially to my mother Katalin, father Zdeněk and sister Tamara, who have remotely supported me during all the years while I left Europe in pursuit of my doctoral studies. The Author CONTRIBUTION OF AUTHORS Dr. Peter Tkac and Nathan Knapp have undertaken the preliminary work on the effects of nitric acid radiolysis, production of nitrous acid and effectiveness of small doses of methylurea in scavenging nitrous acid. Dr. Brent S Matteson has performed the initial kinetic experiments of Np(VI) reduction by acetohydroxamic acid in nitric acid environment. Dr. Bruce J Mincher – has provided for use the scientific equipment and the irradiator at Idaho National Laboratory, and performed the irradiation of aqueous and organic nitric acid solutions – and, together with Dr. Stephen Mezyk, has helped with the interpretation of the data on kinetics of the reaction of H2O2 with HNO2. TABLE OF CONTENTS Page 1 Introduction ............................................................................................................................... 1 1.1 General Background ................................................................................................. 1 1.2 Motivation ................................................................................................................. 1 1.3 Expected Outcomes ................................................................................................... 2 1.4 Overview of the Dissertation .................................................................................... 3 2 Review of Literature .................................................................................................................. 5 2.1 Importance of Neptunium ......................................................................................... 5 2.1.1 Discovery ........................................................................................................ 5 2.1.2 Neptunium in the nuclear fuel cycle ................................................................ 6 2.1.3 Long-term Radiotoxicity of Neptunium in SNF ............................................. 7 2.1.4 Non-proliferation issues .................................................................................. 8 2.1.5 Potential Uses of Neptunium ........................................................................... 9 2.2 General chemical properties of neptunium among the actinide elements ............... 11 2.3 Neptunium in Reprocessing of Used Nuclear Fuel ................................................. 20 2.3.1 PUREX Process ............................................................................................. 20 2.3.2 Advanced PUREX processes ........................................................................ 24 2.4 Control of the oxidation state of neptunium by redox reagents .............................. 27 2.4.1 Neptunium disproportionation and reaction with HNO3 ............................... 27 2.4.2 Uranium(IV) .................................................................................................. 33 2.4.3 Iron(II) ........................................................................................................... 34 2.4.4 Plutonium(III) ................................................................................................ 35 2.4.5 Hydrazine ...................................................................................................... 36 2.4.6 Hydrogen peroxide ........................................................................................ 38 2.4.7 Hydroxylamine .............................................................................................. 40 2.4.8 New prospective reducing agents .................................................................. 43 2.4.9 Vanadium(V) as a prospective oxidizing agent............................................. 50 2.5 Radiation chemistry of neptunium in nitric acid ..................................................... 54 2.5.1 Radiolysis of water ........................................................................................ 54 2.5.2 The radiation chemistry of actinides in
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