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D. A. Wardle, Communities and Ecosystems: Linking the Aboveground and Belowground Components, 2002.

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, Bilan final

, Dans de nombreuses analyses, il est parfois difficile de différencier les traitements de sol les uns des autres

L. Toutefois, Cette observation a particulièrement été faite pour le carbone organique extractible à l'eau. La quantité de substances humiques également n'a pas retrouvé sa valeur de référence (celle des témoins), même 16 ans après le passage d'un feu de forêt. Signalons également que l'on observe une forte variabilité des résultats par type de traitement, complexifiant ainsi l'interprétation quantitative et qualitative des résultats. Concernant les substances humiques, il semble que les résultats en spectrométrie UV montrent une variabilité entre les traitements plus marquée que pour la spectrométrie fluo

, Globalement les résultats obtenus montrent que l'impact du feu affecte essentiellement la surface du sol par rapport à l'horizon plus profond, que ce soit au niveau qualitatif mais également au niveau quantitatif. A la suite d'un feu de forêt, on observe une homogénéisation de la colonne de sol, avec un horizon de surface dont la composition se rapproche de

, Ceci peut s'expliquer probablement par une modification du complexe argilo-humique. En effet, les ammoniums sont stockés par ce complexe et restitués dans la phase aqueuse du sol selon les besoins de la végétation et la capacité d'échange du complexe. Cette capacité d'échange dépend des groupements fonctionnels présents dans le complexe argilo-humique, qui paraît donc avoir évolué. Les ammoniums étant le réservoir des nitrates avant la dernière étape de la minéralisation, Quant aux éléments nutritifs, il est difficile, pour la majorité des éléments, d'observer des différences significatives. Pour le magnésium on observe des valeurs plus basses pour les parcelles ayant subi des nombreux feux

G. R. Aiken, D. M. Mcknight, K. A. Thorn, and E. M. Thurman, Même s'il a été parfois difficile de montrer des différences probantes, on peut donc conclure que concernant les paramètres analysés : ? L'âge du dernier affecte plus le sol que le nombre de feux ? Les 5 premiers cm sont affectés alors que l'horizon suivant n'est pas concerné par les changements Références, Org. Geochem, vol.18, pp.567-573, 1992.

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J. A. Baldock and R. J. Smernik, Chemical composition and bioavailability of thermally altered Pinus resinosa (Red pine) wood, Org Geochem, vol.33, pp.1093-1109, 2002.

G. Certini, Effects of fire on properties of forest soils: a review, Oecologia, vol.143, pp.1-10, 2005.

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R. Chen and J. L. Bada, The fluorescence of dissolved organic matter in pore waters of marine sediments, Mar. Chem, vol.45, pp.31-42, 1994.

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J. P. Croue, M. F. Benedetti, D. Violleau, and J. A. Leenheer, Characterization and copper binding of humic and non humic organic matter isolated from the south platte river: evidence for the presence of nitrogenous binding site, Environ. Sci. Technol, vol.37, pp.328-336, 2003.

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H. Knicker, G. Almendros, F. J. Gonzalez-vila, F. Martin, and H. D. Lüdemann, 13 C-and 15 N-NMR spectroscopic examination of the transformation of organic nitrogen in plant biomass during thermal treatment, Soil Biol. Biochem, vol.28, pp.1053-1060, 1996.

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F. J. Stevenson and H. Chemistry, , vol.2, 1994.

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A. *. Zsolnay, B. E. Jimenez, M. Steinweg, B. Saccomandi, and F. , Differentiating with Fluorescence Spectroscopy the sources of dissolved organic matter in soils subjected to drying, Chemosphere, vol.38, issue.1, pp.45-50, 1999.

, Annexe 5.5: Substances toxiques et matière organique dans

, Analyse des Hydrocarbures Aromatiques Polycycliques dans les sols

. Ong, en utilisant 4 g de silice désactivée à 10%, puis 15 g d'échantillon mélangé à 7,5 g de Na 2 SO 4 activé. L'extrait obtenu est ensuite concentré sur TurboVap TM . La substitution de solvant pour l'analyse finale HPLC (hexane par acétonitrile) a été réalisée sous azote, sans séchage à sec grâce à l'ajout de DMF, afin de minimiser les pertes au niveau des HAP les plus volatils. L'échantillon ainsi préparé est ensuite analysé par HPLC couplée à un détecteur fluorimétrique programmable (HPLC-Fluo/UV). Les rendements d'extraction et la validation globale de la méthode ont été réalisés sur des sols de référence certifiés (CRM 131 COA), Les échantillons de sol ont été séchés à 40°C, puis broyés. La première étape de la procédure d'analyse des Hydrocarbures Aromatiques Polycycliques (HAP) est une extraction solide/liquide par l'hexane avec un robot d'extraction ASE 200, 2003.

, Chacun des sols a été analysé en triplicat, entrainant de nombreux résultats. Ainsi, pour le traitement de ces résultats, nous utiliserons une Analyse en Composantes Principales (ACP)

, Le gaz vecteur est l'hélium (mode débit constant), la température de l'injecteur (splitless) est de 300°C, la colonne chromatographique est en silice fondue J&W DB 5 MS (30 m x 0,25 mm x 0,25 µm). La programmation en température est de 40°C (iso 1 min) à 110°C (50°C/min) puis, 110°C à 290°C par 5°C/min (iso 30 min). Les modes d'acquisitions sont à la fois le courant ionique total (full scan) et SIM avec des ions caractéristiques. Analyse des sols par spectroscopie Proche Infra Rouge L'acquisition des spectres Proche Infra Rouge (PIR) a été réalisée à l'aide d'un spectromètre Infrarouge à Transformée de Fourier (Antaris, Nicolet) en mode réflexion avec une sphère d'intégration. Les spectres ont été enregistrés avec 8 cm -1 de résolution, Analyse des extraits organiques purifiés par GC/MS Les extraits ont été réalisés de la même façon que ceux pour l'analyse des HAP. L'analyse des fractions organiques extraites des sols a été réalisée sur une unité GC-MS/MS

S. Bibliographie-buco, M. Moragues, P. Doumenq, A. Noor, and G. Mille, Analysis of polycyclic aromatic hydrocarbons in contaminated soil by Curie point pyrolysis coupled to gas chromatography-mass spectrometry, an alternative to conventional methods, J. Chomatogr. A, vol.1026, pp.223-229, 2004.

B. M. Didyk, B. R. Simoneit, L. A. Pezoa, M. L. Riveros, and A. A. Flores, Urban aerosol particles of Santiago, Chile: organic content and molecular characterization, Atmospheric Environment, vol.34, pp.1167-1179, 2000.

J. Dorado, G. Almendros, J. A. Field, and R. Sierra-alvarez, Infrared spectroscopy analysis of hemp (Cannabis sativa) after selective delignification by Bjerkandera sp. At different nitrogen levels, Enzyme and Microbial Technology, vol.28, pp.550-559, 2001.

R. M. Duarte, E. B. Santos, C. A. Pio, and A. C. Duarte, Comparison of structural features of watersoluble organic matter from atmospheric aerosols with those of aquatic humic substances, Atmosph. Environ, vol.41, pp.8100-8113, 2007.

T. Dupuis and P. Jambu, Etude par spectroscopie infrarouge des produits de l'humification en milieu hydromorphe calcique, Science du Sol, vol.1, pp.23-35, 1969.

R. Hartmann, Polyzyklische aromatische Kohlenwasserstoffe (PAK) in Waldboden, Bayreuther Bodenkd, p.117, 1995.

E. J. Kim, J. E. Oh, and Y. S. Chang, Effects of forest fire on the level and distribution of PCDD/Fs and PAHs in soil, Sci. Total Environ, vol.311, pp.177-189, 2003.

R. Ong, S. Lundstedt, P. Haglund, and P. Marriott, Pressurised liquid extraction-comprehensive twodimensional gas chromatography for fast-screening of polycyclic aromatic hydrocarbons in soil, J. Chromatogr. A, vol.1019, pp.221-232, 2003.

T. Ramdahl, Retene: a molecular marker of wood combustion in ambient air, Nature, vol.306, pp.580-582, 1983.

B. R. Simoneit, W. F. Rogge, Q. Lang, and R. Jaffé, Molecular characterization of smoke from campfire burning of pine wood (Pinus elliottii), Chemosphere -Global Change Science, vol.2, pp.107-122, 2000.

P. Tinoco, G. Almendros, J. Sanz, R. Gonzalez-vasquez, and F. J. Gonzalez-vila, Molecular descriptors of the effect of fire on soils under pine forest in two continental Mediterranean soils, Org. Geochem, vol.37, 1995.

F. Wania and D. Mackay, Tracking the distribution of persistent organic pollutants, Environ. Sci. Technol, vol.30, pp.390-396, 1996.

W. Wilcke and W. Zech, Polycyclic aromatic hydrocarbons (PAHs) in forest floors of the northern Czech mountains, Z. Pflanzenernahr. Bodenkd, vol.160, pp.369-378, 1997.

S. Buco, M. Moragues, M. Sergent, P. Doumenq, and G. Mille, An experimental design approach for optimizing polycyclic aromatic hydrocarbon analysis in contaminated soil by pyrolyser-gas chromatography-mass spectrometry, Environmental Research, vol.104, pp.209-215, 2007.

, Annexe 5.6: Analyse de Carbone Organique par Résonance Magnétique Nucléaire (RMN)

, Afin de déterminer les mécanismes dans lesquels elles sont impliquées, il est indispensable de caractériser les phases organiques présentes dans le sol. Actuellement, des outils analytiques complémentaires très efficaces (RMN ; InfraRouge, UV-Visible, Pyrolyse-GC-MS) permettent de caractériser la MO, Un des challenges majeurs en biogéochimie aujourd'hui reste l'identification du rôle de la matière organique (MO) dans le fonctionnement des sols, 2000.

. Dans, P. R. Na, and P. A. Et, est en général pas présente de manière isolée, mais associée à des phases minérales. Le cas idéal est d'observer un système avec le moins d'étapes préparatives possibles pouvant affecter le C organique. La spectroscopie RMN, puisque spécifique d'un noyau donné, présente l'attrait de pouvoir se passer de préparation d'échantillons dans un certain nombre de situation. Des échantillons de chacunes des modilités NR

, Les conditions opératoires étaient les suivantes: Les spectres RMN 13 C en phase solide ont été enregistrés avec un spectromètre Bruker Avance WB-400 avec un sonde de 4 mm, Ils ont été obtenus en mode CP-MAS

, Le nombre de scans allait de 2k à 8k pour cette phase exploratoire. La quantitativité de l'analyse a été améliorée en utilisant une séquence d'impulsion particulière. En effet, l'impulsion appliquée au proton n'est pas statique mais est appliqué selon un schéma de rampe décroissante de 100% à 50% pendant le temps de contact. Ce type d'impulsion permet de mieux respecter la condition de Hartmann-Hahn, donc d'assurer un transfert d'aimantation plus efficace comparé à une séquence de CP classique où l'impulsion 1 H est une fonction créneau. Ceci se traduit par une meilleure quantitativité, notamment pour les C en hydridation sp 2 , sachant tout de même que les proportions relatives sont données avec une erreur estimée de ± 10%, MHz, rotation à 10 kHz, temps de recyclage de 3s, temps de contact CP 2ms

. Cependant,

, La figure 1 montre l'aspect typique des spectres. En effet, d'une manière générale, l'étude de la matière organique associée aux phases minérales est souvent peut être compliquée en raison (1) des faibles quantités de C et inversement (2) des quantités trop importantes de phases minérales qui masquent le signal des phases organiques lors de son analyse à la IR-TF et Py-CG/SM ou (3) de la présence d'éléments paramagnétiques (surtout le fer) qui affectent les spectres de RMN 13 C en causant une modification et, Aucun des spectres obtenus dans ces conditions ne présente un signal exploitable. L'augmentation du nombre d'accumulations n'a pas amélioré le rapport signal/bruit, 1999.

L. Dans-le-cas-présent and . Fort, bruit ainsi que les ondulations de la ligne de base indique que c'est certainement la présence de fer qui responsable de la mauvaise qualité des spectres. -l'acidification à pH=1 est susceptible de solubiliser des formes inorganiques du Fe, qui se retrouvent donc dans le surnageant après centrifugation (et donc dans le lyophilisat) et gênent ainsi l'observation des C fulviques. -les espèces fer ne sont pas dissoutes mais on une taille trop faible (colloïdes)

, Quel que soit le mécanisme impliqué, cette présence de fer implique un traitement supplémentaire

J. De, L'HF réagit avec les silicates pour former du SiF 4 qui est un gaz volatile (Robl and Davis, 1993) et permet ainsi de dissoudre les minéraux silicatés et indirectement certains minéraux possédant du fer. La qualité des spectres de RMN 13 C de la MO est ainsi améliorée grâce à (i) la dissolution d'une partie du matériel paramagnétique ; et (ii) l'enrichissement en C de la fraction organique, Une des techniques couramment utilisée consiste à dissoudre les phases minérales avec de l'acide fluorhydrique (HF), 2000.

. Schmidt, Le rapport molaire C/Fe est souvent mis en avant comme étant un paramètre important pour l'obtention de spectre 13 C exploitables. Les valeurs de ce rapport C/Fe pour lesquelles on obtient des données de bonne qualité sont variables: ainsi Gonçalves et al. (2000) obtiennent des spectres avec C/Fe = 2.8, alors que d'autres auteurs estiment qu'il faut des valeurs bien supérieures, La problématique de l'analyse de la matière organique par RMN a été étudié par plusieurs auteurs, 1997.

. Rumpel, En effet, le but même des traitements est d' obtenir des phases organiques "propres", et cela doit se traduire par des temps d'analyses plus court. Il apparaît rapidement que l'on ne peut pas définir de protocole strandard applicable à tous les échantillons; 4 traitements HF peuvent être suffisant pour un échantillon donné, alors que ceci se revèle insuffisant pour un autre échantillon. Dès lors, toute comparaison de la nature de la matière organique entre les différentes placettes et même modalités devient impossible, puisque les protocoles sont différents. Par ailleurs, multiplier les traitements HF induit i)de fortes pertes en C organique (50-85%); on est alors en droit de s'interroger sur la représentativité de la MO observée dans ces conditions, et ii) une modification possible de la nature de la matière organique; dans certaines études HF n'a pas d'effects notables sur la nature et structure de la MO, Ces spectres sont enregistrés dans des conditions identiques que précédemment, à l'exception du nombre de scans qui a été réduit à typiquement 8k, 1997.

, L'aspect structuration par la matière organique est très difficile à aborder compte tenu des difficultés rencontrées pour l'isoler. Il n'apparaît pas pertinent d'entreprendre des expériences visant à se prononcer sur le rôle structurant de la MO lorsqu'il subsiste des interrogations sérieuses quant à la représentativité et l'intégrité même des phases organiques isolées

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