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Thermodynamic Investigation on As(III) and As(V) in Aqueous Solution and Extraction from Natural Water Samples by Polymer Inclusion Membranes (Pims)

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Thermodynamic Investigation on As(III) and As(V) in Aqueous Solution and Extraction from Natural Water Samples by Polymer Inclusion Membranes (Pims) UNIVERSITÀ DEGLI STUDI DI MESSINA Dipartimento di Scienze Chimiche, Biologiche, Farmaceutiche e Ambientali DOTTORATO DI RICERCA IN SCIENZE CHIMICHE XXXII CICLO Thermodynamic investigation on As(III) and As(V) in aqueous solution and extraction from natural water samples by Polymer Inclusion Membranes (PIMs) Donatella Chillé Supervisor Prof. Claudia Foti Coordinator Prof. Paola Dugo Academic Year 2018 – 2019 This thesis was finantial supported by FSE (Fondo Sociale Europeo) regional fund. Project: Dottorati FSE XXXII Ciclo Unime CIP 2014.IT.05.SFOP.014/3/10.5/9.2.02/0006 CUP G47E16000030009 “Tenta l’incompiuto, lo straordinario Vivi in eccesso, cominciando adesso Goditi il trionfo, crea il tuo miracolo Cerca il vero amore dietro ad ogni ostacolo!” (Il mestiere della vita – Tiziano Ferro) Acknowledgements Three years could appear like an infinitely long period of time but now that I am going to write my doctoral thesis, I realize that they have passed really quickly. During this period, I had the pleasure to meet so many people who have enriched me from a professional but mainly human point and to them I address my thanks. However, there are people who deserve to be mentioned as they were pillars for me during this experience. In particular, my supervisor Prof. Claudia Foti, a very important person who, every day, guided my research activity always providing me with valuable advices. Also every single member of the analytical research group and especially Anna, Rosalia and Antonio with whome, having to share the office, I also shared “joys and sorrows”. Thank you very much for EVERYTHING. I spent part of the second year of my PhD at the University of Girona (Spain), guest of the Prof. Clàudia Fontàs. A kind person, always available both at work and out, who allowed me to know, appreciate and even "export" a research line very far from mine. Receiving compliments, especially in the context of an international congress, was a great satisfaction for me! Many thanks also to Laura, Gemma and Ruben. You were really important figures for me because you made me feel like home from the first day I have been there, alleviating the lack of all the affections I had left in my beloved Sicily (or Chichilia), where you will always be welcome. Thanks also to Soetkin, Ibrahim, Marta and Mayra, who accompanied my days in the laboratory between a PIM and a laugh! Of course, I cannot fail to mention Enriqueta, always friendly and present for any suggestion, and Eva who patiently explained to me the principles of EDXRF, helping to carry out part of my research work. All of you will always have a special place in my heart! Among the special thanks, I cannot fail to include Fausta, my so-called left arm (since she is left-handed). We shared high school, graduation years and part of the PhD period, thus we can say that we have been supporting each other for more than half of our lives! Thanks for all the tips, relative to work and life, and to always being there even when we have been located in different countries. A deserved thanks goes to my FAMILY. My parents and my sister know that I am not a person of many words, but on this occasion I want to say that a good part of my success is due to them, to their advices, to their continuous encouraging me to overcome the limits that I have often imposed myself unjustifiably. Finally, I want also thank all the people who, in part, contributed to my research work. Especially, Prof. Anna Napoli and Dr. Donatella Aiello for the mass spectrometry measurements; Prof. Carmelo Sgarlata and Prof. Ottavia Giuffré for the calorimetric titrations; Dr. Franz Sajia, Dr. Sebastiano Trusso, Dr. Rosina Ponterio, Dr. Viviana Mollica Nardo and Dr. Fausta Giacobello for the computationl and Raman studies, as well as Dr. Giuseppe Cassone for the molecular dynamics simulations. Thank you so much! Index Aim of the work ........................................................................................................................ 1 Introduction .............................................................................................................................. 5 Section I: Experimental Section ............................................................................................ 13 1 Chemicals, analytical techniques, mathematical and computational approaches used for thermodynamic studies .................................................................................................... 14 1.1 Chemicals .......................................................................................................................... 14 1.2 Potentiometry ................................................................................................................... 16 1.2.1 General aspects ............................................................................................................... 16 1.2.2 Potentiometric equipment and procedure ....................................................................... 17 1.3 UV-Vis spectrophotometry ............................................................................................. 20 1.3.1 General aspects ............................................................................................................... 20 1.3.2 UV-Vis equipment and procedure ................................................................................... 21 1.4 Calorimetry ...................................................................................................................... 23 1.4.1 General aspects ............................................................................................................... 23 1.4.2 Instrumental equipment and procedure ........................................................................... 23 1.5 Raman Spectroscopy ....................................................................................................... 27 1.5.1 General aspects ............................................................................................................... 27 1.5.2 Instrumental equipment ................................................................................................... 27 1.6 Mass Spectrometry .......................................................................................................... 28 1.6.1 General aspects ............................................................................................................... 28 1.6.2 Instrumental equipment ................................................................................................... 29 1.7 Computational methods ................................................................................................... 30 1.7.1 Ab initio molecular dynamics .......................................................................................... 30 1.7.2 Ab initio molecular dynamics simulations of acid-base properties of As(III) and As(V) 30 1.7.3 Ab initio molecular dynamics simulation of As(III)- tla, tma and dmsa systems ............ 31 1.8 Calculations ....................................................................................................................... 32 1.8.1 Computer programs ......................................................................................................... 32 1.8.2 Equilibrium constants ...................................................................................................... 34 1.8.3 Dependence of the stability constants on the ionic strength ........................................... 35 1.8.4 Dependence of the stability constants on the Temperature ............................................ 37 1.9 Sequestering ability .......................................................................................................... 38 2 Analytical techniques for arsenic determination in water samples ................................ 39 2.1 Chemicals .......................................................................................................................... 39 2.2 Inductive Coupled Plasma - Optical Emission Spectroscopy (ICP-OES) .................. 40 2.2.1 General aspects ............................................................................................................... 40 2.2.2 Instrumental equipment and procedure ........................................................................... 41 2.3 Energy Dispersive X-Ray Fluorescence (EDXRF) Spectrometry ............................... 42 2.3.1 General aspects ............................................................................................................... 42 2.3.2 Instrumental equipment and procedure ........................................................................... 43 Section II: Arsenic(III): acid-base properties and interaction with different classes of ligands in aqueous solution .................................................................................................... 44 1 As(III) acid-base properties: results and discussion ........................................................ 45 1.1 Computational results ...................................................................................................... 46 1.2 Experimental results ........................................................................................................ 47 1.2.1 Protonation constants determination .............................................................................. 47 1.2.2 Dependence on ionic strength ........................................................................................
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