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Based Filter Materials for the Removal of Fluoride from Drinking Water

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Based Filter Materials for the Removal of Fluoride from Drinking Water Eawag_08061 DISS. ETH NO. 20397 Optimization of co-precipitation processes in apatite- based filter materials for the removal of fluoride from drinking water A dissertation submitted to ETH ZURICH for the degree of Doctor of Sciences presented by VANESSA A. S. D. C. STERNITZKE Dipl.-Geoökol., Technical University of Braunschweig, Germany born on January 21, 1980 citizen of Germany accepted on the recommendation of Prof. Dr. Janet G. Hering, examiner Dr. C. Annette Johnson, co-examiner Dr. Markus Janousch, co-examiner Prof. Dr. Staffan Sjöberg, co-examiner 2012 ii Danksagung Meine Doktormutter, Janet Hering, hat mich in diesen vier Jahren meiner Promotion stets kompetent unterstützt, mit interessanten Diskussionen von unterschiedlichen Blickwinkeln immer wieder mein Interesse an dieser Forschung geweckt und mir gleichzeitig das Vertrauen gegeben, mit dem ich die Arbeit frei durchführen konnte. Annette Johnson, meine Direktbetreuerin, hat mich mit weiten Armen in ihre Gruppe aufgenommen, ihre Türe war stets für Diskussionen offen und sie hat sich viel für mich eingesetzt. Spannende XAFS Messungen durfte ich mit Markus Janousch durchführen. Ich danke ihm für diese Gelegenheit, für interessante Diskussionen bei der Datenauswertung und für die Übernahme des Co-Referates. Staffan Sjöberg danke ich herzlich für seinen Besuch aus Schweden zur Übernahme des externen Co-Referates. Ein grosses Dankeschön geht an Ralf Kägi für unzählige TEM/SEM Messungen, für wertvolle und motivierende Diskussionen, sein Vertrauen und Unterstützung bei der Verwirklichung einer „unmöglichen“ Idee sowie für das Herstellen von Kontaken zu verschiedenen Forschungspartnern. Dem originellsten Laborchef der Eawag, Hermann Mönch, danke ich herzlich für seine helfende Hand bei verschiedenen Laborarbeiten, sein stets offenes Ohr, seine Leckerli aus dem eigenen Garten sowie für seinen unbeschreiblich peruanischen Humor. Claire Farnsworth hat mich nicht nur mit wertvollen Diskussionen zu paper1 und dessen sprachlichen Feinschliff unterstützt, auch gemeinsame Mittagessen, Tee- und Schoggipausen, aber besonders die unzähligen Ausflüge in die Schweizer Bergwelt waren stets eine willkommende Abwechselung vom Labor- und Büroalltag. Die teils unglaublich witzigen Erlebnisse bleiben unvergesslich. iii Das Bonbon meines PhD habe ich durch Arno Gutleb und Jean-Nicolas Audinot erhalten. Sie haben die faszinierende NanoSIMS-Messung ermöglicht bzw. durchgeführt. Auch von der reichhaltig instrumentellen Ausstattung der Eawag und Empa habe ich viel profitiert. Für Messmöglichkeiten danke ich Stephan Hug (FTIR), Erik Lewin (XPS), Songhak Yoon, Petar Mandaliev und Gwenn Lesaout (XRD) und Lassi Karvonen (TGA). Sie waren auch wertvolle Ansprechpartner bei anschliessenden Dateninterpretationen. Brian Sinnet hatte kleine, aber feine Tipps zur Probenvorbereitung für TEM/SEM Messungen parat. Andreas Vögelin stand für Meinungsaustausch von x-ray Messungen zur Verfügung. Irene Brunner und dem AUA-Labor danke ich für einige C-Analysen und David Kistler und Thomas Rüttimann gaben mir viele Gelegenheiten, mich intensiv mit Messungen und Gerätefunktionen der ICP-OES und ICP-MS auseinanderzusetzen. Während der Laborumbauphase bekam ich die Möglichkeit, in einem „Wohncontainer“ in Ruhe meine Batchversuche durchführen zu können. Dafür danke ich Stefan Diener. Die Drei von der Werkstatt, besonders Peter Gäumann, haben meine Aufträge stets gründlich und schnell bearbeitet, eingerahmt in echten Schweizer Humor. Eine grandiose Unterstützung während und nach ihrer Masterarbeit bekam ich von Michèle Heeb. Besonders die fachlichen Diskussionen mit ihr, versüsst mit echter Schweizer Schoggi, waren stets eine willkommene Motivation. Jasmin Mertens danke ich für das Teilen des gleichen Bootes eines PhDs, für ihr stets offenes Ohr und die big hugs, welche ich immer wieder nötig hatte. Kleine, aber feine Chatts mit Maria Luisa Ruiz Ripoll, Saskia Zimmermann, Linda Roberts, Sabine Leisinger, Kim Müller, Lars Osterwalder, Anja Bretzler, Milena Miska, Manoucher Amini und Karin Lautenschlager machten den Alltag abwechselungsreicher. Nadine May, Susann Vollrath, Nadine iv Eickenscheidt und Tanja Müller danke ich für eine geckomässige Unterstützung und gegenseitige Motivieren. Meine Lieblingscousinen Christine und Alexandra ermöglichten mir unvergesslich schöne Momente in der Schweiz - ob beim Schlitteln ob Faulhorn, beim Pizzaessen mit „special shots“ während der Fussball-EM oder beim Wandern und Schneeschuhlaufen auf dem Gurten. Meine Tante und Onkel, Ann und Eckart, gaben mir bei jedem Wiedersehen ein grosszügig familiäres Gefühl. Letztlich danke ich meinem Bruder Christian für seine Unterstützung in jeglicher Hinsicht und zu jeder Stunde und besonders meinen Eltern, dafür dass sie für mich da sind und mir stets das geben, was einen am meisten stärkt - Liebe und Vertrauen. v Abstract Drinking water with elevated fluoride (F) concentrations affects the health of millions of people world-wide. Several techniques have been developed to remove F from drinking water. One viable, effective and inexpensive option, particularly for developing countries, is filtering using bone char. Fluoride uptake on bone char is primarily controlled by the main compound of bones, calcium hydroxyapatite (Ca10(PO4)6(OH)2, HAP), which forms fluorapatite (Ca10(PO4)6F2, FAP) in presence of F. The addition of solid calcium-phosphate pellets to the bone char filter media has significantly improved the F uptake capacity in these contact precipitation filters. The pellets dissolve, releasing calcium (Ca) and phosphate (PO4) to solution, which then can precipitate as a new phase incorporating F. However, these filters could still be optimized to improve their efficiency. This thesis investigates the uptake of F in apatitic systems under environmentally relevant conditions. The main aim of this work is to gain insights into the predominant processes controlling F uptake in bone char and contact precipitation filter systems to provide a basis for filter optimization. Fluoride uptake on synthetic HAP, as a proxy for bone char, was investigated under constant conditions over 28d as function of solution pH and initial F concentration, in presence and absence of the anions bicarbonate, sulfate and chloride. The F uptake was found to be predominantly controlled by adsorption processes onto the HAP surface, which allowed a subsequent substitution of OH by F within the HAP crystal structure. The F uptake increased with decreasing solution pH that controlled the surface sites species on the HAP crystals. The result of F uptake was the formation of an FAP-like surface layer on the nanosized HAP crystals. It was further observed that chloride, sulfate and bicarbonate did not affect F uptake capacity. Rapid decreases were observed vi in the initial dissolved concentrations of Ca and F but not of PO4. This indicated the initial precipitation of fluorite (CaF2), which subsequently dissolved to reprecipitate as the thermodynamically most stable phase FAP. In a further approach, the method of contact precipitation was modelled in batch studies. Dissolved Ca and PO4 (and F) were added independently to apatitic suspensions in various stoichiometric ratios corresponding to different calcium-phosphate phases in order to investigate whether or not these phases were formed in heterogeneous systems. The solutions were initially saturated with respect to brushite (CaHPO4*2H2O), β- tricalcium phosphate (Ca3(PO4)2, β-TCP), octacalcium phosphate (Ca8H2(PO4)6*5H2O, OCP), HAP, FAP, and CaF2 or with respect to brushite, β-TCP, OCP and HAP. The final phases were intensively investigated by various solid characterization techniques. Phase distinction was facilitated by the use of Ca-free seeding templates, strontium hydroxyapatite (Sr10(PO4)6(OH)2, SrHAP) and strontium carbonate (SrCO3). After 3d reaction time at neutral pH conditions, the final precipitate was found to be the thermodynamically most stable phase FAP when F was initially added, and HAP in the absence of added F. Thus, phase formation was independent of both added Ca/P or Ca/P/F ratios and the type of seeding template used. X-ray Absorption Spectroscopy indicated either the precipitates to be Ca-deficient (non-stoichiometric) HAP or to be mixtures of HAP and brushite and/or β-TCP. These phases were probably precipitated as intermediate phases, since solutions did not reach complete equilibrium conditions after 3d. Precipitates obtained in fluoridated systems, where solution composition was initially PO4-limited for stoichiometric FAP and excess Ca and F were stoichiometric for CaF2, showed shifts of atomic binding energies towards energy levels of CaF2 in X- ray Photoelectron Spectroscopy (XPS). Moreover, it was observed that Ca/P ratios vii estimated from elemental loss from solution do not necessarily provide sufficient identification of the final precipitate. viii Zusammenfassung Erhöhte Fluoridkonzentrationen in Trinkwasser gefährden weltweit die Gesundheit von Millionen von Menschen. Viele Technologien wurden entwickelt, um das Fluorid (F) aus dem Trinkwasser zu entfernen. Eine praktikable, effektive und gleichzeitig relativ kostengünstige Methode ist die Nutzung von Knochenkohle als Filtermaterial, welche besonders für Entwicklungsländer interessant ist. Die Fluoridaufnahme auf Knochenkohle wird vorrangig durch den Hauptbestandteil der Knochen bestimmt, dem Calciumphosphat-Mineral Hydroxyapatit (Ca10(PO4)6(OH)2, HAP), welches sich in Anwesenheit von Fluoridionen zu Fluorapatit (Ca10(PO4)6F2, FAP)
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