MINERALOGIE DES ARGILES DANS LES DISPOSITIFS DE LONGUE DUREE : COMMENT ET POUR QUELLES INFORMATIONS?
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1 1 MINERALOGIE DES ARGILES DANS LES DISPOSITIFS DE LONGUE DUREE : COMMENT ET POUR QUELLES INFORMATIONS? F. Hubert & B. Lanson fabien.hubert@univ-poitiers.fr bruno.lanson@univ-grenoble-alpes.fr
2 42 PLOTS LONG-TERM EXPERIMENTAL SITE OF VERSAILLES 2 Silty loam Haplic Luvisol developed on aeolian loess Experiment design Collection of soil samples since 1929 Sample studied Surface horizon Reference plot
3 CLAY MINERALOGY OF REFERENCE PLOT (1929) Pernes-Debuyser A. et al., 2003, Clays & Clay Minerals 3 XRD analysis (<2µm, sat. Ca 2+ ) I/S AD I/S EG I K I K I I K Clay mineralogy (C, 2-5µm) kaolinite (K, minor) XRD data treatment Decomposition I/S I M I/S Calculated 1D XRD pattern of I/S illite and mica (I & M, minor) R0 illite-smectite (I/S, 50/50, 2-6 layers, minor) R0 illite-smectite (I/S, 50/50, 1-4 layers, major)
4 CLAY MINERALOGY OF REFERENCE PLOT (1929) Pernes-Debuyser A. et al., 2003, Clays & Clay Minerals 3 XRD analysis (<2µm, sat. Ca 2+ ) I/S AD I/S EG I K I K I I K Clay mineralogy (C, %?) XRD profile modelling of patterns Decomposition I/S I/S I M I/S Calculated 1D XRD pattern of kaolinite (K, %?) illite and mica (I & M, %?) R0 illite-smectite (I/S, 50/50, 2-6 layers, %?) R0 illite-smectite (I/S, 50/50, 1-4 layers,%?)
5 CLAY MINERALOGY OF REFERENCE PLOT (1929) Hubert et al., In preparation AD 4 <2µm sat. Ca 2+ <0,02µm sat. Ca 2+ <0.02 µm X 2 Crystal structures of finest clay minerals cannot be observed on the XRD patterns of bulk <2µm fraction whereas they represent about a third of the fraction mass
6 Particle fractionation µm µm µm METHODOLOGY Hubert et al., In preparation Ethylene Glycol (EG) Air Dried (AD) Ca-saturated XRD XRD profile modeling (00l) µm <0.02 µm sub fractions mass contribution (%wt) X Amount of each clay in sub-fraction (%)? Unknown clay mineralogy of the <2µm fraction Calculated clay mineralogy Close qualitative and quantitative results Fitted clay mineralogy Amount of each clay in the bulk (%) clay mineralogy of the <2µm fraction XRD profile modeling (00l)
7 XRD RESULTS OF REFERENCE PLOT (1929) Sub-fraction masses & XRD patterns of oriented slides % Mass recovery <2 mm = 99.9 ± 0.5 % Mass recovery = AD sat. Ca 2+ %wt = 17 Bulk µm %wt = µm %wt = µm %wt = µm <0.02 µm Hubert et al., In preparation
8 AD sat. Ca 2+ XRD RESULTS OF REFERENCE PLOT (1929) XRD profile modeling of 00l reflections Bulk 7 Rp = µm Rp = µm Rp = µm Rp = µm Rp = 2.1 <0.02 µm Rp = 3.4 Hubert et al., In preparation
9 XRD RESULTS OF REFERENCE PLOT (1929) XRD profile modeling of 00l reflections Bulk 8 Rp = µm Rp = µm Rp = µm Rp = µm Rp = 2.1 <0.02 µm Rp = 3.4 Hubert et al., In preparation
10 CLAY MINERALOGY OF REFERENCE PLOT (1929) Hubert et al., In preparation Structural model Relative proportions of clay minerals 9 < Bulk < Bulk C/S
11 CLAY MINERALOGY OF REFERENCE PLOT (1929) Hubert et al., In preparation Structural model Relative proportions of clay minerals 9 < Bulk < Bulk C/S
12 CLAY MINERALOGY OF LONG TERM EXPERIMETAL SITES XRD profile modeling Structural model Relative proportions %wt = plot experiment (Versailles) Luvisol - surface horizon CEC = 15.3cmol(c).kg -1 Hubert et al. In preparation C/S/I Lu Al Fe Lu Al Fe 10 SOERE FOREST Breuil-Chenue (Morvan) Aluminic cambisol - surface horizon CEC = 3.4 cmol(c).kg -1 Viennet et al. (2015) %wt = 16 ORE ACBB, INRA of Lusignan Ferralitic cambisol - deep horizon CEC = 7.9 cmol(c).kg -1 Hubert et al. (2012)
13 CLAY MINERALOGY OF LONG TERM EXPERIMETAL SITES XRD profile modeling Structural model Relative proportions %wt = plot experiment (Versailles) Luvisol - surface horizon CEC = 15.3cmol(c).kg -1 Hubert et al. In preparation C/S/I Lu Al Fe Lu Al Fe 10 SOERE FOREST Breuil-Chenue (Morvan) Aluminic cambisol - surface horizon CEC = 3.4 cmol(c).kg -1 Viennet et al. (2015) %wt = 16 ORE ACBB, INRA of Lusignan Ferralitic cambisol - deep horizon CEC = 7.9 cmol(c).kg -1 Hubert et al. (2012)
14 CLAY MINERALOGY OF LONG TERM EXPERIMETAL SITES XRD profile modeling Structural model Relative proportions %wt = plot experiment (Versailles) Luvisol - surface horizon CEC = 15.3cmol(c).kg -1 Hubert et al. In preparation C/S/I Lu Al Fe Lu Al Fe 11 SOERE FOREST Breuil-Chenue (Morvan) Aluminic cambisol - surface horizon CEC = 3.4 cmol(c).kg -1 %wt = 16 ORE ACBB, INRA of Lusignan Ferralitic cambisol - deep horizon CEC = 7.9 cmol(c).kg -1
15 CLAY MINERALOGY OF LONG TERM EXPERIMETAL SITES XRD profile modeling Structural model Relative proportions %wt = plot experiment (Versailles) Luvisol - surface horizon CEC = 15.3cmol(c).kg -1 Hubert et al. In preparation C/S/I Lu Al Fe Lu Al Fe 11 SOERE FOREST Breuil-Chenue (Morvan) Aluminic cambisol - surface horizon CEC = 3.4 cmol(c).kg -1 %wt = 16 ORE ACBB, INRA of Lusignan Ferralitic cambisol - deep horizon CEC = 7.9 cmol(c).kg -1
16 CLAY MINERALOGY OF LONG TERM EXPERIMETAL SITES XRD profile modeling Structural model Relative proportions 42 plot experiment (Versailles) Luvisol - surface horizon CEC = 15.3cmol(c).kg -1 Lu Al Fe Lu Al Fe 12 %wt = 50 C/S/I SOERE FOREST Breuil-Chenue (Morvan) Aluminic cambisol - surface horizon CEC = 3.4 cmol(c).kg -1 Viennet et al. (2015) %wt = 16 ORE ACBB, INRA of Lusignan Ferralitic cambisol - deep horizon CEC = 7.9 cmol(c).kg -1
17 CLAY MINERALOGY OF LONG TERM EXPERIMETAL SITES XRD profile modeling Structural model Relative proportions 42 plot experiment (Versailles) Luvisol - surface horizon CEC = 15.3cmol(c).kg -1 HIS/HIV Lu Al Fe Lu Al Fe 12 %wt = 50 C/S/I SOERE FOREST Breuil-Chenue (Morvan) Aluminic cambisol - surface horizon CEC = 3.4 cmol(c).kg -1 Viennet et al. (2015) %wt = 16 ORE ACBB, INRA of Lusignan Ferralitic cambisol - deep horizon CEC = 7.9 cmol(c).kg -1
18 CLAY MINERALOGY OF LONG TERM EXPERIMETAL SITES XRD profile modeling Structural model Relative proportions 42 plot experiment (Versailles) Luvisol - surface horizon CEC = 15.3cmol(c).kg -1 HIS/HIV Lu Al Fe Lu Al Fe 12 %wt = 50 C/S/I SOERE FOREST Breuil-Chenue (Morvan) Aluminic cambisol - surface horizon CEC = 3.4 cmol(c).kg -1 Viennet et al. (2015) %wt = 16 ORE ACBB, INRA of Lusignan Ferralitic cambisol - deep horizon CEC = 7.9 cmol(c).kg -1
19 CLAY MINERALOGY OF LONG TERM EXPERIMETAL SITES XRD profile modeling Structural model Relative proportions 42 plot experiment (Versailles) Luvisol - surface horizon CEC = 15.3cmol(c).kg -1 Lu Al Fe Lu Al Fe 13 %wt = 50 C/S/I SOERE FOREST Breuil-Chenue (Morvan) Aluminic cambisol - surface horizon CEC = 3.4 cmol(c).kg -1 %wt = 16 ORE ACBB, INRA of Lusignan Ferralitic cambisol - deep horizon CEC = 7.9 cmol(c).kg -1 Hubert et al. (2012)
20 CLAY MINERALOGY OF LONG TERM EXPERIMETAL SITES XRD profile modeling Structural model Relative proportions 42 plot experiment (Versailles) Luvisol - surface horizon CEC = 15.3cmol(c).kg -1 Lu Al Fe Lu Al Fe 13 %wt = 50 C/S/I SOERE FOREST Breuil-Chenue (Morvan) Aluminic cambisol - surface horizon CEC = 3.4 cmol(c).kg -1 %wt = 16 ORE ACBB, INRA of Lusignan Ferralitic cambisol - deep horizon CEC = 7.9 cmol(c).kg -1 Hubert et al. (2012)
21 CLAY MINERALOGY OF LONG TERM EXPERIMETAL SITES XRD profile modeling Structural model Relative proportions %wt = plot experiment (Versailles) Luvisol - surface horizon CEC = 15.3cmol(c).kg -1 Hubert et al. In preparation C/S/I Lu Al Fe Lu Al Fe 14 SOERE FOREST Breuil-Chenue (Morvan) Aluminic cambisol - surface horizon CEC = 3.4 cmol(c).kg -1 Viennet et al. (2015) %wt = 16 ORE ACBB, INRA of Lusignan Ferralitic cambisol - deep horizon CEC = 7.9 cmol(c).kg -1 Hubert et al. (2012)
22 CLAY MINERALOGY OF LONG TERM EXPERIMETAL SITES XRD profile modeling Structural model Relative proportions %wt = plot experiment (Versailles) Luvisol - surface horizon CEC = 15.3cmol(c).kg -1 Hubert et al. In preparation C/S/I Lu Al Fe Lu Al Fe 14 SOERE FOREST Breuil-Chenue (Morvan) Aluminic cambisol - surface horizon CEC = 3.4 cmol(c).kg -1 Viennet et al. (2015) %wt = 16 ORE ACBB, INRA of Lusignan Ferralitic cambisol - deep horizon CEC = 7.9 cmol(c).kg -1 Hubert et al. (2012)
23 Luvisol CLAY MINERALOGY OF LONG TERM EXPERIMETAL SITES Bakker et al., 2018, Soil Systems 40 % wt Morrow Plots CEC (ceq.kg -1 ) % CF RU Série1 Série
24 CONCLUSION 16 - Qualitative agreement is not sufficient to provide an accurate structural characterization of mixed layers clay minerals - XRD full-profile fitting combined to size fractionation is the optimum way to quantitatively determine soil clay mineralogy including i) the finest and most reactive fraction and ii) mixed layers minerals - Cross-constraints from the modelling of different size fractions and multispecimen approach are essential to the validity of the model. Additional constraints from usual sample processing are needed too. - The proposed approach provides key information on the nature of clay mineral phases present, on their proportions, on their crystal chemistry - This information provides essential constraints on the parent material, on (paleo-) conditions of formation, on pedogenetic processes, on the impact of plant nutrition, on soil chemical and physical properties, etc BIBLIOGRAPHY Bakker, E., Hubert, F., Wander, M. & Lanson, B. (2018) Soil Development under Continuous Agriculture at the Morrow Plots Experimental Fields from X-ray Diffraction Profile Modelling. Soil Systems 2, 46. Hubert F. et al. Investigation of the soil clay mineralogy at the 42 plots long-term site of Versailles (France) using X-ray diffraction profile modeling. In preparation Hubert F., Caner L., Meunier A. & Ferrage E. (2012) Unraveling complex < 2 µm clay mineralogy from soils using x-ray diffraction profile modeling on particle-size sub-fractions: Implications for soil pedogenesis and reactivity. American Mineralogist, 97, Pernes-Debuyser, A., Pernes, M., Velde, B., Tessier, D. (2003) Soil mineralogy evolution in the INRA 42 plots experiment (Versailles, France). Clays and Clay Minerals, 51, Viennet J.C., Hubert F., Ferrage E., Tertre E., Legout A. & Turpault M.P. (2015) Investigation of clay mineralogy in a temperate acidic soil of a forest using X-ray diffraction profile modeling: Beyond the HIS and HIV description. Geoderma, ,
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