Etude de l'ablation-ionisation résonante des oxydes de fer : spéciation et analyse in situ : application à l'étude des interactions biologiques en présence ou non d'hydrocarbures aromatiques polycycliques

Abstract : The first aim of this work was a physical characterization of iron oxides Fe1-[delta]O, Fe3O4 and Fe2O3 (microphotographies SEM, specific area, granulometry). Then, these oxides were studied by laser microprobe mass spectrometry (LMMS) in order to distinguish them by their fingerprint. Multiphoton ionization must be banished ; it is preferable to employ the RELAI ionization (resonant laser ablation/ionization) which permits to increase sensibility of the detection and to improve the difference between the iron oxides. Moreover, the Fe1-[delta]O, Fe3O4 and Fe2O3 oxides were synthesized from iron 54 and were characterized by X ray diffraction and by LMMS with RELAI mode. The differentiation of these three oxides was reinforced by statistical method (principal component analysis PCA). The second purpose is devoted to the understanding of the formation mechanisms of Fe2+ and Fe2O+ for which their intensity vary significantly according to the studied species. The results provided by LMMS and FT/ICR/MS analyses show that several mechanisms are possible : we can say that the dimer Fe2+ is provided by a reaction Fe2+ and neutral FeO, and the Fe2O+ ion arises at the same time from the reaction of the dimer Fe2+ with the singlet oxygen 1O2. These reactions are induced inside the gazeous cloud after the laser pulse and they are not ion/molecule reactions occuring in the FT/ICR/MS cell. Then, we accounted our protocol to examine the characteristics of particles descended from steel-works, blast furnace and ore agglomeration. Fe3O4 and Fe2O3 oxides are detected in contrary to Fe1-[delta]O which has never been observed. Besides, we analysed polycyclic aromatic hydrocarbons (PAH) by LAMMA and FT/ICR/MS in particles of steel-works. The presence of benzo[a]pyren (BaP) is confirmed in small size particles (0,7 - 1,1 um) containing a non negligible concentration of iron oxide. The identification of different PAH is confirmed by gas chromatography GC/FID. Finally, the studies allow us to show the biological transformation of iron oxides 56Fe3O4, 56Fe2O3, 54Fe3O4, 54Fe2O3 and of industrial particles in embryonic cells and macrophages by LMMS in RELAI mode. From the results, it can be shown a reduction of Fe3O4 AND Fe2O3 oxides when they are present in biological cells. The detection of BaP is also possible in biological tissu by an ionization with small wavelength
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Benoît Maunit. Etude de l'ablation-ionisation résonante des oxydes de fer : spéciation et analyse in situ : application à l'étude des interactions biologiques en présence ou non d'hydrocarbures aromatiques polycycliques. Autre. Université Paul Verlaine - Metz, 1996. Français. ⟨NNT : 1996METZ042S⟩. ⟨tel-01777151⟩

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