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Christopher Parsons Distribution et mobilité de l’arsenic dans les sols : effets de cycles redox successifs Christopher Parsons To cite this version: Christopher Parsons. Distribution et mobilité de l’arsenic dans les sols : effets de cycles redox suc- cessifs. Sciences de la Terre. Université de Grenoble, 2011. Français. NNT : 2011GRENU029. tel-00637484v2 HAL Id: tel-00637484 https://tel.archives-ouvertes.fr/tel-00637484v2 Submitted on 7 Dec 2011 HAL is a multi-disciplinary open access L’archive ouverte pluridisciplinaire HAL, est archive for the deposit and dissemination of sci- destinée au dépôt et à la diffusion de documents entific research documents, whether they are pub- scientifiques de niveau recherche, publiés ou non, lished or not. The documents may come from émanant des établissements d’enseignement et de teaching and research institutions in France or recherche français ou étrangers, des laboratoires abroad, or from public or private research centers. publics ou privés. THÈSE Pour obtenir le grade de DOCTEUR DE L’UNIVERSITÉ DE GRENOBLE Spécialité : Géochimie de l’Environnement Arrêté ministériel : 7 août 2006 Présentée par Christopher Parsons Thèse dirigée par Professeur Laurent Charlet et codirigée par Dr. Gabriela Roman-Ross préparée au sein de l’Institut des Sciences de la Terre dans l'École Doctorale : Terre, Univers, Environnement Distribution et mobilité de l’arsenic dans les sols: Effets de cycles redox successifs Cover Page Thèse soutenue publiquement le 19 Octobre 2011, devant le jury composé de : Prof. Laurent CHARLET Professeur à l’Université de Grenoble Directeur Dr. Gabriela ROMAN-ROSS Chercheur à AMPHOS 21, Barcelona Co-Directrice Prof. David POLYA Professeur à l’Université de Manchester Rapporteur Dr. Eric PILI Expert Senior au CEA, DAM-Île de France Président Dr. Benoit MADE Ingénieur, Direction Recherche et Développement, ANDRA Membre invité Synopsis Redox sensitive contaminants in complex, three phase biologically mediated systems are susceptible to a myriad of biogeochemical interactions including protonation/de-protonation, sorption/desorption, complexation with organic matter, precipitation/dissolution and methylation/de-methylation as well as direct changes to oxidation state. This plethora of often simultaneous processes makes predicting mobility of contaminants in soils and aquifers, and hence effective resource management, very challenging. This thesis aims to elucidate the key biogeochemical processes and physical factors which control the mobility and distribution of redox sensitive contaminants including arsenic, chromium, uranium and mercury in frequently flooded soils. The work presented spans the colloidal to field scale and uses a combination of spectroscopic, analytical, geo-statistical and computational tools. Particular attention is paid to arsenic and the role of cyclic redox conditions which are prevalent in a number of contaminated environments. Arsenic is an infamously toxic and carcinogenic metalloid which has received substantial attention from the international scientific community over the last two decades. This is principally due to the humanitarian disaster in southern Asia where tens of millions of people are affected by arsenic contaminated drinking water sourced from shallow alluvial aquifers. However, the threat posed by arsenic to human health is not limited to the sedimentary basins fed by the Himalaya. Sources of arsenic release to the environment are numerous and varied, with both anthropogenic and geogenic inputs a cause for concern. In Western Europe and North America the legacy of industrial activity and agricultural use of arsenic, compounded by natural geological input, has resulted in the contamination of many floodplain soils and wetlands. Contaminants are often concentrated in such sediments as their fine physical texture, and hence large surface area can retard the advective transport of arsenic in fluvial and groundwater systems. At the same time geothermal waters are often also loaded with As and may represent a threat to populations exposed through contaminated drinking water e.g. in the Atacama desert. Understanding the factors affecting arsenic mobility and toxicity in such systems is a challenge, demanding collaboration between traditionally separated academic fields. In addition to its current practical relevance, arsenic biogeochemistry is also of special academic interest due to the sensitivity of arsenic to solid and aqueous speciation changes within a range of Eh and pH conditions found in many near surface environments. The calcareous soils of the Saône floodplain in eastern France, close to the city of Macon, are known to host elevated concentrations of redox sensitive contaminants including arsenic and chromium. They are also subjected to regular redox oscillations due to seasonal flooding and form the focus of the experimental and field investigations presented in this thesis. Summary Figure 1: The flooded alluvial plain of the Saône close to Macon during the winter. i During periods of flooding, pores in surface soils become saturated with water and diffusion of oxygen from the atmosphere to the soil is restricted. This forces soil bacterial communities to consume successively less efficient terminal electron acceptors and causes a progressive decrease in oxidation/reduction potential in the soil solution. Summary Figure 2: How soil saturation causes changes to redox conditions in soils via limiting diffusion of oxygen from the surface to aerobic soil bacteria resulting in rapid oxygen depletion. Summary Figure 3: The succession of terminal electron acceptors used by soil bacteria during oxidation of organic matter governed by energetic efficiency. This microbially mediated redox shift causes changes in chemical equilibria and hence mineralogy, sorption processes and aqueous speciation, all of which impact arsenic mobility. A great deal of work has already been conducted over the last years to establish release mechanisms and sorbents of arsenic under reducing conditions. However, relatively limited attention has been paid to the cumulative effects of periodic redox cycling on soil mineralogy, the bacterial community, organic matter lability and ultimately, arsenic distribution and mobility. Neglecting cycling conditions represents an important gap in our understanding of a variety of both natural and anthropogenically influenced environments, including floodplains, rice paddies and shallow aquifers. ii At the field scale, a critical evaluation of the analytical capability of field-portable X-ray fluorescence (FP-XRF) spectrometry for the standard-less, quantitative analysis of arsenic in soils was performed. It was found that due to recent improvements to hand held technology, instrumentation limitations were a secondary concern to sample preparation. Existing literature pertaining to the use of FP-XRF on soils has comprehensively investigated factors such as sample heterogeneity and particle size. However, results presented in this thesis suggest that the most important practical factor affecting precision and accuracy of FP-XRF analysis of trace arsenic concentrations in soils is the presence of soil pore water, even in comparatively dry soils. In order to maximise the accuracy of in situ analysis, a field-based sample preparation method was developed. This method allows the quantitative, multi-elemental analysis of soils and was validated by both lab based X-ray fluorescence and inductively coupled plasma mass spectrometry (ICP-MS) analysis. Applying this sample preparation method, data obtained during field investigations were used to determine inter-elemental relationships in top soils, in addition to spatial and physical controls on arsenic distribution on the local field scale. It was found that one of the best predictors of arsenic concentrations was the particle size distribution within the finest soil fraction (less than 500 µm). Arsenic was associated most strongly with the finest clay / colloid fractions and strongly anti-correlated with very fine sands. Particle size distribution in the larger fractions (above 500 µm) appeared to have little effect on arsenic concentration. Summary Figure 4: Comparison of particle size distributions between average low arsenic and high arsenic soils illustrating the importance of the clay fraction to arsenic distribution. iii Strong correlations were also found between total arsenic, iron and manganese concentrations. Weak correlations were found between arsenic concentrations and other indicators of soil hydrological conditions suggesting that hydraulic spatial redistribution of arsenic may be of limited importance within this area. The active carbonate and solid organic matter fractions were found to be poorly linked to arsenic concentration. This suggests that despite recent spectroscopic and modelling evidence demonstrating arsenic immobilization within the calcite structure, arsenic association with calcite may be of limited importance when metal oxides are also present in calcareous soils. Summary Figure 5: Correlation matrix demonstrating inter- elemental relationships in soils on the Saône floodplain. Square size and colour corresponds to the correlation coefficient between elemental pairs (blue positively correlated, red negatively correlated). At the batch scale, laboratory experiments were conducted using osmotic diffusion pore- water sampling devices to determine the extent of redox change experienced by temporally flooded soils on the Saône floodplain. Using this information a custom system
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