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Download (8MB) https://theses.gla.ac.uk/ Theses Digitisation: https://www.gla.ac.uk/myglasgow/research/enlighten/theses/digitisation/ This is a digitised version of the original print thesis. Copyright and moral rights for this work are retained by the author A copy can be downloaded for personal non-commercial research or study, without prior permission or charge This work cannot be reproduced or quoted extensively from without first obtaining permission in writing from the author The content must not be changed in any way or sold commercially in any format or medium without the formal permission of the author When referring to this work, full bibliographic details including the author, title, awarding institution and date of the thesis must be given Enlighten: Theses https://theses.gla.ac.uk/ [email protected] DEVELOPMENT AND APPLICATION OF METHODS FOR THE ASSAY OF NEPTUNIUM IN ENVIRONMENTAL MATRICES Andrew Stefan Hursthouse BSc (Hons) (Reading) A thesis presented for the degree of Doctor of Philosophy University of Glasgow Scottish Universities Research and Reactor Centre May 1990 ®A.S. Hursthouse, 1990 ProQuest Number: 11007382 All rights reserved INFORMATION TO ALL USERS The quality of this reproduction is dependent upon the quality of the copy submitted. In the unlikely event that the author did not send a com plete manuscript and there are missing pages, these will be noted. Also, if material had to be removed, a note will indicate the deletion. uest ProQuest 11007382 Published by ProQuest LLC(2018). Copyright of the Dissertation is held by the Author. All rights reserved. This work is protected against unauthorized copying under Title 17, United States C ode Microform Edition © ProQuest LLC. ProQuest LLC. 789 East Eisenhower Parkway P.O. Box 1346 Ann Arbor, Ml 48106- 1346 ACKNOWLEDGEMENTS This thesis is the result of the help, advice and encouragement of many people too numerous to mention. It could not have been attempted or completed without the supervision of Prof Murdoch Baxter and Drs Francis Livens and Harry Duncan for which I am very grateful. They provided the correct amount of advice and many useful suggestions and of course the occassional nudge in the right direction. The SURRC and ITE (Merlewood) were exciting and enjoyable places in which to work. Many people from a wide range of disciplines helped to create a stimulating atmosphere and without doubt provided much of the inspiration for the research described in this volume. Thanks go to all the academic staff, technicians, research assisstants and students (permanent and migratory) who put up with my continual pestering with remarkable tolerance. In particular Gus MacKenzie, Roger Scott, Gordon Cook, David Sanderson and Tony Fallick at the SURRC helped to guide me through a minefield of problems during my stay. I will always be indebted to Mr Keith McKay for holding my hand through much of the lab work and for some very sound advice. Paul, Joe, Phil, Ihsan, Tracy and Margaret were great people to work with and bore the brunt of many of my practical problems both in the lab and at the typewriter, thanks. I could not forget Uncle Pizza, who has shared many of my experiences in EK and the SURRC, thanks for all your help Pete. My family, Mike, Hanna, Martin, Annelene and Robin have always given me all the support and encouragement anybody could need and their love and inspiration, for which I cannot thank them enough. I would also like to thank all my friends and collegues from the University of Reading, in particular JET who inspired my research career and set such high standards. He has always given me much to aim for. Finally, I would like to thank Caroline, Darren, Ross and Michelle. They have helped me to complete this thesis in so many ways and also improved my snooker. Thanks for all the fun and your love and concern and above all helping me to keep it all in perspective. I acknowledge the financial support of the Natural Environment Research Council. This work was carried out in the laboratories of the SURRC, the Department of Agricultural Chemistry, University of Glasgow and the NERC ITE Merlewood Research Station. TABLE OF CONTENTS CHAPTER 1 .............................................................................................................................................. 1 1.1 INTRODUCTION AND A IM S ............................................................................................ 2 1.2 THE CHEMISTRY OF NEPTUNIUM ............................................................................ 3 1.2.1. HISTORICAL PERSPECTIVE - THE DISCOVERY OF NEPTUNIUM .............................................................................................. 3 1.2.2 NUCLEAR PROPERTIES, PREPARATION AND ISOLATION............... 4 1.2.3 NEPTUNIUM IN NATURE ............................................................................ 7 1.2.4 CHEMICAL PROPERTIES OF NEPTUNIUM ........................................... 8 (a) the position of neptunium in the actinide series .......................... 8 (b) chemical beh aviou r .......................................................................... 10 1.2.5 AQUEOUS CHEMISTRY OF NEPTUNIUM ........................................... 11 (a) redox tre n d s ...................................................................................... 11 (b) complex form ation ............................................................................ 13 1.3 THE ENVIRONMENTAL BEHAVIOUR OF NEPTUNIUM ...................................... 18 1.3.1 IN TR O D UC TIO N ........................................................................................... 18 1.3.2 THE IMPORTANCE OF NEPTUNIUM IN THE LONG-TERM DISPOSAL OF RADIOACTIVE WASTES ........................................... 20 1.3.3 THEORETICAL SPECIATION AND EXPECTED BEHAVIOUR OF NEPTUNIUM IN THE ENVIRONMENT .............................................. 21 1.3.4 SOURCES OF NEPTUNIUM IN THE ENVIRONMENT....................... 23 (a) weapons fa llo u t ................................................................................. 24 (b) releases from laboratories and the processing of nuclear fu els .............................................................................................. 26 (c) the physico-chemical nature and behaviour of neptunium in sellafield discharges released into the marine environment ................................................................................. 29 (d) the availability and uptake of neptunium by marine biota . 37 p 7 7 (e) the potential impact of the Chernobyl accident on Np inventories .................................................................................... 38 1.3.5 LABORATORY STUDIES ON THE ENVIRONMENTAL BEHAVIOUR OF NEPTUNIUM ......................................................................................... 38 (a) adsorption/ desorption studies ........................................................ 39 (b) behaviour in studies of groundwater/ rock interactions .... 40 (c) laboratory and field studies of water-soil-plant translocation and u p take .................................................................................... 42 CHAPTER 2 .............................................................................................................................................. 44 2.1 THE APPROACH TO ENVIRONMENTAL TRACE ANALYSIS OF 237Np _____ 45 2.1.1 SENSITIVITY AND DETECTION .................................................................. 46 2.1.2 SAMPLE COLLECTION AND PREPARATION ......................................... 47 (a) S o ils ........................................................................................................ 48 (b) Unconsolidated sedim ents ................................................................ 48 (c) Water samples .................................................................................... 49 (d) Biological m aterials ............................................................................ 49 (e) Laboratory procedures ....................................................................... 49 2.1.3 STANDARDISATION AND TRACEABILITY...... ........................................... 50 2.2 THE PRECONCENTRATION OF SAMPLES FOR 237Np ANALYSIS ..................... 51 2.2.1 SAMPLE D IS S O L U T IO N ............................................................................... 53 2.2.2 COPRECIPITATION AND PRECIPITATION METHODS ......................... 54 2.2.3 LIQUID-LIQUID EXTRACTION OF NEPTUNIUM .................................... 56 (a) Neptunium/chelate system s ............................................................. 57 (b) Neptunium-ion association s y s te m s .............................................. 60 (c) high molecular weight amines ........................................................ 65 (d) alcohols, ketones, esters and a m id e s ............................................ 68 (e) mixed extractants and the synergistic effect ............................... 71 iv 2.2.4. ION EXCHANGE CHROMATOGRAPHY................................................ 74 (a) cation exchange of neptunium ...................................................... 76 (b) anion exchange of neptunium ..................................................... 77 (c) inorganic ion exchangers ................................................................ 78 2.2.5 EXTRACTION CHROMATOGRAPHY ................................................... 79 2.3 METHODS FOR THE QUANTIFICATION OF 237Np IN ENVIRONMENTAL M A TR IC E S ..............................................................................................................
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