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Docteur De L'universite D'aix-Marseille THÈSE Pour l’obtention du grade de DOCTEUR DE L’UNIVERSITE D’AIX-MARSEILLE en Sciences de l’Environnement Préparée au sein de l’Ecole Doctorale Sciences de l’Environnement (ED251) au Laboratoire de Chimie de l’Environnement (LCE) Présentée par Rana CHEHAB Développement de systèmes automatisés pour l’analyse des chloramines inorganiques et des trihalométhanes dans les eaux Soutenue le 19 Décembre 2019, devant le jury composé de : Président du jury Stephan BROSILLON, Professeur des Universités, Université de Montpellier et Rapporteur Victor CERDÀ, Professeur Émérite, Université des îles Baléares, ESPAGNE Rapporteur Valérie PICHON, Professeur des Universités, Sorbonne Université Examinateur Justine CRIQUET, Maître de Conférences, Université de Lille Examinateur Jean-Luc BOUDENNE, Professeur des Universités, Aix-Marseille Université Directeur Fabien ROBERT-PEILLARD, Maître de Conférences, Aix-Marseille Université Co-Directeur Remerciements Cette étude a été effectuée au Laboratoire Chimie de l’Environnement (LCE) au sein de l’équipe Transfert, Réactivité et Analyse des Micropolluants dans l’Environnement (TRAME) à l’Université Aix-Marseille. Je remercie Henri Wortham, Directeur de LCE, pour la confiance qu’il m’a accordée en m’accueillant au sein de laboratoire. Mes sincères remerciements seraient accordés à mes directeurs de thèse Jean-Luc Boudenne et Fabien Robert Peillard. D’abord, un grand merci à Jean-Luc, pour m’avoir donné la chance de vivre cette expérience fructueuse, pour la confiance et les conseils qu’il m’a donnés et pour l’accompagnement qu’il a fait pour moi tout au long de la réalisation de cette thèse, je n’oublierais pas ses encouragements qui m’ont motivée dès la première réunion, lors des congrès jusqu’au dernier moment d’encadrement. Je tiens à remercier énormément Fabien, pour son soutien qui m’a toujours poussée à avancer dans mes recherches, pour ses conseils et ses connaissances qu’il a partagées avec moi. Je n’oublierais pas sa disponibilité à toutes heures pendant les trois années. Je vous remercie, mes directeurs, pour tout petit coup de main que vous m’avez donné pendant la rédaction de ce rapport ainsi que pour les réunions et les discussions qui font que ce travail soit réalisé. Je tiens à remercier vivement les membres de jury de cette thèse : Victor Cerdà et Stephan Brosillon d’avoir accepté de juger et rapporter ce travail ; Ainsi que, Valérie Pichon et Justine Criquet pour avoir bien voulu examiner et juger ce travail. J’ai été accueillie pendant trois ans au sein d’une équipe que je considère comme ma famille en France. Je remercie tous les personnels notamment mes amis Mira, Elodie et Maxime ; je n’oublie pas également Bruno, Laurence, Carine, Didier, Laurent, Elodie, Pascale, Nadia, Etienne, Anne et Sylvain. Vous faites tous une belle partie de cette aventure. Enfin, je tiens à remercier ma famille, notamment mon père et ma mère, je ne pourrais rien faire sans votre amour, confiance et soutien tout au long de ma vie. Et finalement, je remercie mon amour qui a été présent pour moi dans chaque étape dès que je suis arrivée en France. Table des Matières Liste des Figures ......................................................................................................................7 Liste des Tableaux ............................................................................................................... 11 Liste des Abréviations ........................................................................................................ 13 Introduction Générale ........................................................................................................ 17 CHAPITRE I : État de l’art ................................................................................................... 23 I.1. Les sous-produits de désinfection dans les eaux .................................................................... 23 I.1.1. Généralités sur les sous-produits de désinfection ......................................................... 23 I.1.2. Formation et spéciation .............................................................................................................. 24 I.1.3. Propriétés chimiques et physiques ....................................................................................... 31 I.1.4. Toxicité et risques sanitaires .................................................................................................... 33 I.1.5. Réglementations ............................................................................................................................. 37 I.2. Les méthodes de quantification des chloramines et bromamines inorganiques et des trihalométhanes dans les eaux ................................................................................................................ 42 I.2.1. Méthodes de quantification des chloramines inorganiques...................................... 42 I.2.2. Méthodes de quantification du brome et des bromamines inorganiques .......... 55 I.2.3. Méthodes de quantification des trihalométhanes .......................................................... 57 I.3. Les Systèmes d’analyse en flux ........................................................................................................ 63 I.3.1. Présentation des principaux systèmes d’analyse en flux ............................................ 64 I.3.2. Techniques avancées d’analyse en flux pour la séparation et la préconcentration d’analytes ................................................................................................................ 67 I.3.3. Méthodes par analyse en flux appliquées à l’analyse des chloramines inorganiques ou des trihalométhanes. ............................................................................................ 69 I.4. Conclusion du chapitre ........................................................................................................................ 71 CHAPITRE II : Analyse des chloramines et des bromamines inorganiques dans les eaux .......................................................................................................................................... 75 II.1. Introduction ............................................................................................................................................. 75 II.2. Matériels et méthodes ........................................................................................................................ 76 II.2.1. Réactifs .............................................................................................................................................. 76 II.2.2. Préparation des chloramines inorganiques ..................................................................... 77 5 II.2.3. Préparation des bromamines inorganiques .................................................................... 82 II.2.4. Analyse par HPLC avec détection directe ......................................................................... 85 II.2.5. Spectrophotométrie UV et spectroscopie de fluorescence en microplaques. 85 II.2.6. Instrumentation pour le système de chromatographie multi-seringues .......... 86 II.3. Développement de l’analyseur de type Chromatographie Multi-seringues ............. 87 II.3.1. Principe du système .................................................................................................................... 87 II.3.2. Optimisations préalables au développement de l’analyseur : séparation et détection des chloramines inorganiques ....................................................................................... 89 II.3.3. Application au système d’analyse en flux ...................................................................... 108 II.4. Réaction des espèces réactives du chlore et du brome avec l’ABTS et détection directe par spectrophotométrie ........................................................................................................... 125 II.4.1. Etude des conditions expérimentales .............................................................................. 125 II.4.2. Performances analytiques ..................................................................................................... 129 II.5. Conclusion du chapitre .................................................................................................................... 131 CHAPITRE III : Développement d’une méthode d’analyse des trihalométhanes ................................................................................................................................................. 135 III.1. Introduction ........................................................................................................................................ 135 III.2. Matériels et méthodes .................................................................................................................... 136 III.2.1. Réactifs et solutions ................................................................................................................ 136 III.2.2. Instrumentation ........................................................................................................................ 137 III.3. Développement méthodologique ............................................................................................. 138 III.3.1. Optimisation de la réaction de Fujiwara ....................................................................... 138 III.3.2. Extraction et préconcentration des Trihalométhanes
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