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U(VI) Retention by Ca-Bentonite and Clay Minerals at (Hyper)Alkaline Conditions

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U(VI) Retention by Ca-Bentonite and Clay Minerals at (Hyper)Alkaline Conditions U(VI) retention by Ca-bentonite and clay minerals at (hyper)alkaline conditions D I S S E R T A T I O N zur Erlangung des akademischen Grades Doctor rerum naturalium (Dr. rer. nat.) vorgelegt dem Bereich Mathematik und Naturwissenschaften der Technischen Universität Dresden von MSc. Angewandte Geowissenschaften, Thimo Philipp Geboren am 04.04.1988 in Linnich Eingereicht im am 23.10.2019 Disputation und Rigorosum am 28.01.2020 Erster Gutachter: Prof. Dr. Thorsten Stumpf, Technische Universität Dresden Zweiter Gutachter: Prof. Dr. Thorsten Schäfer, Friedrich-Schiller-Universität Jena Die Dissertation wurde in der Zeit von Dezember 2015 bis Mai 2019 im Institut für Ressourcenökologie des Helmholtz-Zentrums Dresden-Rossendorf angefertigt Acknowledgements First of all, I would like to thank Prof. Thorsten Stumpf for the supervision of my thesis and for offering the possibility to do my PhD at the Institute of Resource Ecology. Prof. Dr. Thorsten Schäfer is gratefully acknowledged for his interest in my work and his kind willingness to be the second referee. I would like to express my gratitude to my direct supervisor Dr. Katja Schmeide for permanent support, advice and proof reading. Dr. Andrea Cherkouk and Dr. Nina Huittinen are thanked for their help as co-supervisors of this thesis. Especially Nina added enormous value to this work by numerous discussions and spot on advices and consultancy. Special thanks go to Salim Shams Aldin Azzam for his invaluable assistance in the daily laboratory work. Without him, this thesis would not have been possible. Furthermore I would like to thank Dr. André Rossberg (EXAFS), Dr. Nina Huittinen (site- selective TRLFS), Dr. Robin Steudtner (TRLFS), Dr. Katharina Müller (ATR FT-IR), Dr. Moritz Schmidt (CTR/RAXR), Dr. Frank Bok (thermodynamic calculations) and Dr. Atsushi Ikeda (PXRD) for sharing their scientific expertise in the respective methods with me. I am very thankful for essential support in laboratory applications, which I got from Stephan Weiß, Carola Eckardt, Karsten Heim, Sabrina Beutner, Birke Pfützner, Stephanie Bachmann, Anette Rumpel, Susanna Jiminez, Christa Müller, Steffen Henke and Klaus Meier (Institut für Ressourcentechnologie, Freiberg). Measurements outside of Rossendorf were only possible thanks to the help of Peter Eng (at the APS) and the cooperation with Prof. Tobias Reich, Dr. Samer Amayri, Verena Häußler and Tobias Stern (all at JGU Mainz). Paul Dullies is acknowledged for his reliable work as a master student related to this thesis. Moreover, I appreciate the assistance of the following people, who all contributed to the scientific success of the thesis in some way: Dr. Vinzenz Brendler, Dr. Jan Tits (PSI), Julia Neumann, Dr. Canrong Qiu, Konrad Molodtsov, Dr. Bin Xiao, Henry Loesch, Dr. Natalia Mayordomo Herranz, Hannes Brinkmann, Kathrin Nebe, Jana Gorzitze and many more. The Federal Ministry of Economic Affairs (BMWi) is gratefully acknowledged for the funding of the project GRaZ (No. 02 E 11415B). I also want to thank all my colleagues and fellow PhD students for the daily exchange and the pleasant atmosphere at the institute. Special love goes to the Happy Thursday crew for sharing so many unforgettable moments with me. Finally I would like to thank my family, friends and Anna, who all contributed to the success of this thesis to an extent they might not imagine. I Content List of abbreviations and symbols........................................................................................ III Summary .................................................................................................................................. V 1. Introduction ..................................................................................................................... 1 1.1. Motivation ........................................................................................................................ 1 1.2. Aim and scope of the thesis ................................................................................................ 2 1.3. Radioactive waste disposal in Germany ............................................................................... 3 2. Theoretical Background ................................................................................................. 5 2.1. Chemistry of uranium and neptunium.................................................................................. 5 2.2. Clay mineralogy, bentonite, montmorillonite and muscovite ................................................. 9 2.3. Sorption mechanisms ....................................................................................................... 10 2.4. U(VI) and Np(VI) sorption on clay minerals – state of knowledge ...................................... 13 2.5. Fundamentals of spectroscopic techniques ......................................................................... 17 2.5.1. Time-resolved laser-induced luminsescence spectroscopy (TRLFS) ......................... 17 2.5.2. Extended X-ray absorption fine structure (EXAFS) spectroscopy ............................. 20 2.5.3. Attenuated total reflectance Fourier transform infrared (ATR FT-IR) spectroscopy ... 23 2.5.4. Crystal truncation rod (CTR) and resonant anomalous X-ray reflectivity (RAXR) ..... 24 3. Materials and Methods ................................................................................................. 27 3.1. Materials ......................................................................................................................... 27 3.2. Bentonite surface charge and stability at (hyper)alkaline conditions .................................... 29 3.2.1. Zeta potential ........................................................................................................ 29 3.2.2. Leaching at (hyper)alkaline conditions ................................................................... 29 3.2.3. X-ray diffraction (XRD) ........................................................................................ 29 3.3. Batch sorption experiments .............................................................................................. 30 3.3.1. S/L ratio dependence ............................................................................................. 33 3.3.2. Kinetic sorption experiments.................................................................................. 33 3.3.3. Sorption isotherms ................................................................................................ 33 3.3.4. pH dependency of sorption .................................................................................... 33 3.3.5. Desorption ............................................................................................................ 34 3.4. Solubility tests ................................................................................................................. 34 3.5. TRLFS ............................................................................................................................ 35 3.6. In situ ATR FT-IR spectroscopy ....................................................................................... 36 3.7. EXAFS spectroscopy ....................................................................................................... 36 3.8. CTR/RAXR .................................................................................................................... 38 II 4. Results and Discussion ................................................................................................. 39 4.1. Bentonite surface charge and stability at (hyper)alkaline conditions ..................................... 39 4.1.1. Zeta potential ........................................................................................................ 39 4.1.2. Powder X-ray diffraction (PXRD)........................................................................... 39 4.1.3. Leaching ............................................................................................................... 40 4.2. Sorption of U(VI) on Ca-bentonite at hyperalkaline conditions ............................................ 42 4.2.1. Batch sorption experiments .................................................................................... 42 4.2.1.1. S/L ratio dependence ...................................................................................... 42 4.2.1.2. Kinetic sorption experiments ........................................................................... 43 4.2.1.3. Sorption isotherms.......................................................................................... 43 4.2.1.4. pH dependency of sorption.............................................................................. 45 4.2.1.5. Desorption ..................................................................................................... 47 4.2.2. Aqueous speciation of U(VI) investigated with TRLFS ............................................ 49 4.2.3. Solubility of U(VI) ................................................................................................ 52 4.2.4. U(VI) surface speciation......................................................................................... 53 4.2.4.1. In situ ATR FT-IR spectroscopy ...................................................................... 53 4.2.4.2. Site-selective TRLFS ...................................................................................... 57 4.2.4.3. EXAFS spectroscopy .....................................................................................
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