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Extraction Chromatographic Studies of Rutherfordium and Dubnium Homologs

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Extraction Chromatographic Studies of Rutherfordium and Dubnium Homologs UNLV Theses, Dissertations, Professional Papers, and Capstones 5-2011 Extraction chromatographic studies of rutherfordium and dubnium homologs Megan E. Bennett University of Nevada, Las Vegas Follow this and additional works at: https://digitalscholarship.unlv.edu/thesesdissertations Part of the Analytical Chemistry Commons, Inorganic Chemistry Commons, Nuclear Commons, and the Radiochemistry Commons Repository Citation Bennett, Megan E., "Extraction chromatographic studies of rutherfordium and dubnium homologs" (2011). UNLV Theses, Dissertations, Professional Papers, and Capstones. 982. http://dx.doi.org/10.34917/2327114 This Dissertation is protected by copyright and/or related rights. It has been brought to you by Digital Scholarship@UNLV with permission from the rights-holder(s). You are free to use this Dissertation in any way that is permitted by the copyright and related rights legislation that applies to your use. For other uses you need to obtain permission from the rights-holder(s) directly, unless additional rights are indicated by a Creative Commons license in the record and/or on the work itself. This Dissertation has been accepted for inclusion in UNLV Theses, Dissertations, Professional Papers, and Capstones by an authorized administrator of Digital Scholarship@UNLV. For more information, please contact [email protected]. EXTRACTION CHROMATOGROPHIC STUDIES OF RUTHERFORDIUM AND DUBNIUM HOMOLOGS By Megan E. Bennett Bachelor of Science State University of New York College at Brockport 2005 Masters of Science Virginia Polytechnic Institute and State University 2007 A dissertation submitted in partial fulfillment of the requirements for the Doctor of Philosophy in Radiochemistry Department of Chemistry College of Science Graduate College University of Nevada, Las Vegas May 2011 Copyright by Megan E. Bennett 2011 All Rights Reserved iii THE GRADUATE COLLEGE We recommend the dissertation prepared under our supervision by Megan E. Bennett entitled Extraction Chromatographic Studies of Rutherfordium and Dubnium Homologs be accepted in partial fulfillment of the requirements for the degree of Doctor of Philosophy in Radiochemistry Ralf Sudowe, Committee Chair Kenneth Czerwinski, Committee Member Dawn Shaughnessy, Committee Member Steen Madsen, Graduate Faculty Representative Ronald Smith, Ph. D., Vice President for Research and Graduate Studies and Dean of the Graduate College May 2011 ii ABSTRACT Extraction Chromatographic Studies of Rutherfordium and Dubnium Homologs by Megan E. Bennett Dr. Ralf Sudowe, Examination Committee Chair Assistant Professor of Radiochemistry University of Nevada, Las Vegas Studying the chemistry of transactinide elements does not only allow for these elements to be properly placed in the Periodic Table, but it also permits for the extrapolation of the electronic structure based upon the position of the element in the Periodic Table. In addition it enable for the assessment of the role that relativistic effects play in the chemical behavior of the heaviest elements. An improved understanding of the role of relativistic effects in chemistry of the heaviest elements allows for a better understanding of the fundamentals principles that govern the Periodic Table. In order to investigate the chemistry of the transactinides, chemical studies on the homologs and pseudo-homologs of the element must first be performed. Chemical studies of the homologs and pseudo-homologs can be completed in a number of ways. Gas-phase chemistry, solvent extraction and ion-exchange chromatography have all been used to study a number of transactinide elements as well as their respective homologs and pseudo-homologs. No matter the method of study, a given system must fulfill the following requirements to be considered suitable; fast kinetics, high separation factors, large number of exchange steps, highly selective and samples easily prepared for alpha spectroscopy. The system must allow for rapid separation due to the short half- iii lives of transactinide elements (on the order of a few seconds up to a minute). A large number of exchange steps are necessary due to the fact there is only one atom present at a given time. In order for one atom to be statistically representative of a macroscopic amount the atom must undergo many interactions with the two phases of the separation system. The system should also be highly selective to ensure that background contamination is removed and separation of the transactinide from its homologs and pseudo-homologs is achieved. Finally, the samples generated from the separation must be easily and rapidly prepared for alpha spectroscopy so that the decay of the short lived transactinide element can be directly detected. The aim of this research is to develop two separation schemes for elements 104 and 105 that fulfill all of these requirements. For element 105 the proposed extractant molecule is a tetra diglycoloamide in a mixed acid matrix. In the case of element 104 crown ether based ligands of interest. The proposed separation schemes for element 104 and 105 are based on both commercially available and in-house synthesized resins. iv ACKNOWLEDGEMENTS I would like to thank Dr. Ralf Sudowe, Dr. Dawn Shaughnessy and Dr. Roger Henderson for their guidance, support, and encouragement during my graduate career. I would also like to thank Dr. Ken Czerwinski, Dr. Ken Moody, Dr. Julie Gostic, Dr. Sarah Nelson and Dr. Phil Wilk for their advice and encouragement. I would also like to thank the members of the UNLV Radiochemistry group. I extend a special thanks to Tom O’Dou, Trevor Low and Julie Bertoia for ensuring that we can do our experiments safely, no matter how crazy they maybe. Also, thanks to Dr. Nick Smith, Sherry Faye and John Despotopulos for their help in conducting experiments, the analysis of results, and assistance in writing this thesis. Finally, I would like to thank my parents and step-dad. Without their continuous support, encouragement, and love this would not have been possible. Thank you for always supporting me. v TABLE OF CONTENTS ABSTRACT ........................................................................................................................ ii ACKNOWLEDGEMENTS ................................................................................................ v LIST OF TABLES ........................................................................................................... viii LIST OF FIGURES ........................................................................................................... xi LIST OF EQUATIONS ................................................................................................... xiii CHAPTER 1 INTRODUCTION .................................................................................... 1 1.1 Historical Perspective ................................................................................... 1 1.2 Heavy Element Production ........................................................................... 6 1.3 Relativistic Effects ........................................................................................ 8 1.4.1 Atom-at-a-Time Chemistry ................................................................. 10 1.4.2 Extraction Chromatography .................................................................... 14 1.5 Chromatography Literature Review ........................................................... 16 1.5.1 Introduction ............................................................................................. 16 1.5.2 Group IV Liquid Phase Chemistry ...................................................... 17 1.5.3 Group V Liquid Phase Chemistry ....................................................... 20 1.6 Research Goals ........................................................................................... 24 CHAPTER 2 EXPERIMENTAL METHODS AND INSTRUMENTATION ........... 27 2.1 Off-Line Studies ...................................................................................................... 27 2.1.1 Method Selection .............................................................................................. 27 2.1.2 Reagents and Materials ..................................................................................... 30 2.1.2.1 Chemicals ................................................................................................... 30 2.1.2.2 Radionuclide Stock Solutions .................................................................... 30 2.1.2.2.1 95Zr and 95Nb Solutions ....................................................................... 30 2.1.2.2.2 175Hf, 182Ta, 233Pa Solutions ................................................................ 32 2.1.3 High Purity Germanium Gamma Spectroscopy ............................................... 32 2.1.3.1 Activity Measurements .............................................................................. 34 2.1.4 Extraction Chromatography ............................................................................. 35 2.1.4.1 Batch Method ............................................................................................. 35 2.1.4.2 Column Method ......................................................................................... 36 2.1.4.4.1 Electrospray-Mass Spectrometry ........................................................ 38 2.1.5 Synthesis of Resins ........................................................................................... 39 CHAPTER 3 EXTRACTIONS WITH EICHROM’S
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