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The Development of Electrochemical Tools For NEW METHODS IN BIOGEOCHEMISTRY: THE DEVELOPMENT OF ELECTROCHEMICAL TOOLS FOR THE MEASUREMENT OF DISSOLVED AND SOLID STATE COMPOUNDS IN NATURAL SYSTEMS Dissertation zur Erlangung des Doktorgrades der Naturwissenschaften am Fachbereich 5 der Universität Bremen Vorgelegt von Jochen Nuester Bremen 2005 Die vorliegende Arbeit wurde in der Zeit von Mai 2000 bis August 2005 am Max Planck Institut für Marine Mikrobiologie erstellt. 1. Gutachter: Prof. Dr. Bo Barker Jørgensen 2. Gutachter: Prof. Dr. Jörn Peckmann Prüfer: Prof. Dr. Achim Kopf Dr. Sabine Kasten Tag des Promotionskolloquium: 26. August 2006 II New Methods in Biogeochemistry III New Methods in Biogeochemistry IV New Methods in Biogeochemistry Acknowledgements Acknowledgements This PhD thesis deals with the development of new tools and methods to describe biogeochemical processes. Several aspects concerning the speciation have been studied; especially new methods were described for the determination of solid iron compounds, the detection of dissolved transition metals, and the complexation of such transition metals. The financial support for this thesis came from the Max Planck Society and the European Union is grateful acknowledged. First of all, I would like to thank Prof. Bo Barker Jørgensen for accepting me as his PhD student, and the opportunity to carry out this work at the Max Planck Institute. I am very grateful to my mentor and friend Dr. Ole Larsen for the initiation of the work, for the way he taught me to think interdisciplinary, for his supervision, and his support. He always had an open ear, and he usually had very inspiring answers to my questions. I like to thank Prof. Stan van den Berg at the University of Liverpool for the opportunity to stay at his laboratory and the fruitful cooperation. The work at the Oceanographic Laboratories in Liverpool was very inspiring, and supports my understanding of electrochemistry. Timothy Ferdelman, Michael Böttcher, and Dirk de Beer always had time for very fruitful discussions on various topics concerning electrochemical measurements and iron biogeochemistry. Their clear and critical analysis helps to structure my ideas and to develope new methods and tools. Dirk de Beer is also thanked for the opportunity to use the microsensor laboratories. My special thanks go to Gaby Eickert, Ines Schroeder, Cäcilia Wigand, Karin Hohmann, Vera Hübner, and Ingrid Dohrmann for accepting me somehow as a part of their microsensor laboratory, for their helping hand, for the introduction to construct microsensors, and also for the way they handle my impossibility to be tidy. Without the help of the Volker Meyer, Paul Färber, and Harald Osmers from the electronic workshop the microsensor development work would not have been possible. Thanks a lot! V New Methods in Biogeochemistry Acknowledgements Kirsten Imhoff, Swantje Lilienthal, Imke Busse, Gabi Schüssler, Gabi Klockgetter, and all the other technicians are thanked for their invaluable, never ending help in the laboratory. I like to thank Bernd Stickford for his help in the library, and for ordering so many articles and books not available, and to Ulrike Tietjen for all her organizing work. Many thanks to Jutta, Niko, Verona, Lev, Stanislav, Kyriakos, Solveig, Sandra, Eli, Fanny, Tina, Hans, Marcel, Stefan, Uschi, Felix, Alex, Susanne, Anna, Heiko, Nina, Helge, Peter and all the other nice people at the institute, who support me in those days when I could not laugh anymore about the problems I had with my work. They made this time at the Max Planck Institute very special in providing a nice working atmosphere and a very pleasant time. Especially I would like to thank the members of the cheerleading group and the boy group, who made my Julefrokost parties to very exciting events. I’m deeply grateful to Emily Fleming, who helped me in the last years with her support, her love, her patient, and also her knowledge about English language and grammar. Last but not least I like to thank my parents, my brother, and my grandma, who saw me struggle, but always support my work and my goals. Uncountable thanks! VI New Methods in Biogeochemistry Table of Contents Table of Contents Acknowledgements................................................................................................................................................V Table of Figures...................................................................................................................................................IX List of Tables ....................................................................................................................................................XIII List of Important Abbreviations..................................................................................................................... XIV Abstract............................................................................................................................................................. XVI Zusammenfassung......................................................................................................................................... XVIII Part 1: Introduction Chapter 1 In-Situ Applications to Modern Biogeochemistry.............................................................................................. 1 1.1 Introduction.................................................................................................................................................. 2 1.2 In-Situ Technologies .................................................................................................................................... 2 1.2 Thesis Outline .............................................................................................................................................. 4 Chapter 2 Iron and Manganese Biogeochemistry ................................................................................................................ 7 2.1 Introduction.................................................................................................................................................. 8 2.2 Iron and Sulfur Cycle ................................................................................................................................. 10 2.3 Iron Oxide Reactivity ................................................................................................................................. 15 2.4 Mechanism of Microbial Fe(III) Reduction ............................................................................................... 19 Chapter 3 Principles of Voltammetry ................................................................................................................................. 21 3.1 Introduction................................................................................................................................................ 22 3.2 Theory ........................................................................................................................................................ 25 3.3 Stripping Voltammetry............................................................................................................................... 27 3.4 Voltammetric Applications ........................................................................................................................ 33 Part 2: Publications Chapter 4 Electrochemical Determination of the Reactivity of Sedimentary Iron Minerals......................................... 43 Abstract ............................................................................................................................................................ 44 4.1 Introduction................................................................................................................................................ 45 4.2 Experimental Section ................................................................................................................................. 47 VII New Methods in Biogeochemistry Table of Figures 4.3 Results and Discussions ............................................................................................................................. 51 Chapter 5 Miniaturization of Voltammetric Microelectrodes for In-Situ Application in Natural Systems ................. 71 Abstract ............................................................................................................................................................ 72 5.1 Introduction................................................................................................................................................ 73 5.2 Experimental Section ................................................................................................................................. 74 5.3 Microlectrode Design................................................................................................................................. 76 5.4 Results and Discussions ............................................................................................................................. 82 5.5 Conclusion.................................................................................................................................................. 92 Chapter 6 Determination of Metal Speciation by Reverse Titrations .............................................................................. 93 Abstract ...........................................................................................................................................................
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