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Part I: General Introduction ÉCOLE DOCTORALE SCIENCE FONDAMENTALES APPLIQUEÉS Géoazur UMR 7329 Thèse de doctorat Présentée en vue de l’obtention du grade de docteur en Chimie de L’UNIVERSITÉ COTE D’AZUR par Anna Maria ORANI Développements analytiques pour la détermination des concentrations et de l’origine des contaminants inorganiques dans des environnements marins Dirigée par Pr. Olivier THOMAS et codirigée par Dr. Emilia VASSILEVA et Dr. Aurélie BARATS Soutenue le 15 Décembre 2017 Devant le jury composé de : Dr. Aurélie BARATS, Maître de conférences, Géoazur, Université Côte d’Azur co-directrice de thèse Prof. Ewa BULSKA, Chemistry Department, University of Warsow rapporteur Prof. Veselin J. KMETOV, Analytical Chemistry Department, University of Plovdiv rapporteur Prof. Christophe RENAC, Géoazur, Université Côte d’Azur examinateur, président du jury Prof. Olivier P. THOMAS, National University of Ireland Galway directeur de thèse Dr. Emilia VASSILEVA, Research scientist, Environment Laboratories, IAEA co-directrice de thèse Development and application of analytical methodologies for trace elements pollution assessment in different compartments of the marine environment AKNOWLEDGMENTS First of all I would like to express my gratitude to Prof. Ewa Bulska, Prof. Veselin Kmetov, and Prof. Christophe Renac for their interest in my PhD work and for taking the time to review my thesis. I am confident that their suggestions will be of great help for my future. This PhD comes to an end after a tortuous path, full of challenges but most importantly full of interesting experiences. A real life-changing adventure during which I have learnt a lot! Many people helped me in this period, fighting for and with me and for this reason I will be forever grateful to each of them, starting from my supervisors: -My PhD director Olivier Thomas, who accepted this role and never gave up even in the middle of many administrative challenges! -My PhD co-director Emilia Vassileva, who encouraged me to start a PhD in the first place and with her precious teaching always supported my work and believed in me. -My second PhD co-director Aurélie Barats, who helped and encouraged me even during the most difficult periods, with many advices and positive attitude. Special thanks go to Prof Petko Mandjukov and Dr Irena Wysocka, for sharing their knowledge with me and for their crucial contribution to this PhD work and to Ms Sabine Azemard for her constant help. I would like to thank all the fellows and office mates I have been the pleasure to work with, in France and Ireland, which have contributed to accumulate many wonderful memories! Je voudrais remercier toute la famille Calabro, pour m’avoir accueilli à bras ouverts ces dernières années et pour être toujours un gros point de référence, ma deuxième famille ! Ancora una volta vorrei ringraziare la mia meravigliosa famiglia e le mie fantastiche amiche che mi sono stati vicino (da lontano). Il loro sostegno è stato fondamentale in questi anni, e lo sarà per sempre. Voglio dedicare questa tesi a Kevin, che mi ha supportato (e sopportato) in questi anni, garantendomi amore incondizionato, condividendo con me le tante soddisfazioni ma soprattutto insegnandomi a non mollare e perseverare sempre! CONTENTS PART I: GENERAL INTRODUCTION .............................................................................................................. 11 1. Trace elements in the environment.................................................................................................... 13 1.1. Trace elements in the aquatic system ........................................................................................ 13 1.2. Trace elements speciation .......................................................................................................... 16 1.2.1. Arsenic ................................................................................................................................. 17 1.2.2. Mercury ............................................................................................................................... 20 1.3. Trace elements isotopes ............................................................................................................. 22 1.3.1. Pb Isotopic ratios ................................................................................................................. 24 2. Trace elements monitoring programs ................................................................................................ 26 2.1. Trace elements in sediments ........................................................................................................... 27 2.1.1. Sediment components and classification ................................................................................. 27 2.1.2. Factors affecting TE accumulation in sediments ...................................................................... 29 2.1.3. TE monitoring in sediments ...................................................................................................... 32 2.2. Trace elements in marine organisms ............................................................................................... 33 2.2.1. Bivalves ..................................................................................................................................... 33 2.2.2. Sponges ..................................................................................................................................... 35 3. Trace elements analysis ...................................................................................................................... 38 3.1. Atomic Absorption Spectrometry .................................................................................................... 40 3.2. Inductively Coupled Plasma Mass Spectrometry ............................................................................. 41 REFERENCES ................................................................................................................................................ 44 PART II: SCIENTIFIC PUBLICATIONS ............................................................................................................. 69 FIRST BLOCK ................................................................................................................................................ 71 Paper 1 .................................................................................................................................................... 71 Paper 2 .................................................................................................................................................... 81 Paper 3 .................................................................................................................................................... 95 SECOND BLOCK ......................................................................................................................................... 115 Paper 4 .................................................................................................................................................. 115 Paper 5 .................................................................................................................................................. 150 THIRD BLOCK ............................................................................................................................................. 201 Paper 6 .................................................................................................................................................. 201 Paper 7 .................................................................................................................................................. 254 Conclusion and future perspectives ......................................................................................................... 297 11 PART I: GENERAL INTRODUCTION PART I: GENERAL INTRODUCTION In this first part of the thesis, some general information is discussed. These concepts are useful for the understanding of the general picture presented in this PhD. The origin and fate of TE in different compartments of the aquatic system are presented as well as a brief description of analytical techniques used during the present work. 12 PART I: GENERAL INTRODUCTION 13 PART I: GENERAL INTRODUCTION 1. TRACE ELEMENTS IN THE ENVIRONMENT The IUPAC Compendium of Chemical Terminology defines trace element as “any element having an average concentration of less than about 100 parts per million atoms or less than 100 µg g-1’’ (McNaught and Wilkinson, 1997). Among TE, some are oligo elements and are thus considered essential for various biochemical and physiological functions within a certain range of concentrations. Metals/metalloids considered by World Health Organization to be essential for human health are: chromium, cobalt, copper, iron, molybdenum, selenium and zinc (WHO, 1996)(WHO, 1996).On the other hand, other TE are considered toxic at any concentration (Hg, Pb, Cd) (WHO/FAO/IAEA, 1996). These elements are naturally present in the ecosystem because of natural processes such as weathering and erosion but also volcanic activity. Nevertheless, in the last decades, several anthropogenic activities have increased the loads of these elements in the environment (Bagul, 2015). Main anthropogenic sources of TE include metal mining, mineral processing, smelting, coal mining, power generation but also municipal waste incinerators, industrial waste of
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