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Insights into Diagenesis and Pore Structure of Opalinus Shale Through Comparative Studies of Natural and Reconstituted Materials

Published online by Cambridge University Press:  01 January 2024

Ali Seiphoori ,
Andrew J. Whittle ,
Konrad J. Krakowiak  and
Herbert H. Einstein
Ali Seiphoori*
Affiliation:
Department of Civil and Environmental Engineering, Massachusetts Institute of Technology (MIT), 02139, Cambridge, MA, USA
Andrew J. Whittle
Affiliation:
Department of Civil and Environmental Engineering, Massachusetts Institute of Technology (MIT), 02139, Cambridge, MA, USA
Konrad J. Krakowiak
Affiliation:
Department of Civil and Environmental Engineering, University of Houston, 77204, Houston, TX, USA
Herbert H. Einstein
Affiliation:
Department of Civil and Environmental Engineering, Massachusetts Institute of Technology (MIT), 02139, Cambridge, MA, USA
*
*E-mail address of corresponding author: [email protected]
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Abstract

Shales have undergone a complex burial diagenesis that involved a severe modification of the pore structure. Reconstituted shales can provide new insights into the nature of the pore structure in natural materials. The effects of diagenesis on the microfabric, pore size distribution, and porosity of Opalinus shale were measured by comparing the behavior of natural and reconstituted specimens. The parent material (Opalinus shale) was reconstituted through multiple grinding operations, sedimentation from a dispersed slurry, and one-dimensional isothermal consolidation. This process produced uniform specimens that were not cemented and had replicable microfabric and engineering properties. The microfabric and mineralogy of the materials were examined using high-resolution scanning/backscattered electron microscopy (SEM/BSEM) and energy-dispersive X-ray spectroscopy (EDS) for specimens with broken and milled surfaces. Mercury intrusion porosimetry (MIP) and N2 adsorption were used to assess the pore size distributions and specific surface areas of the materials. The microstructure of natural shale was characterized to be highly heterogeneous with significant concentrations of calcareous microfossils, calcite, and quartz particles embedded within the clay matrix. The microfossils were observed to be locally infilled and rimmed by a calcite cement that showed evidence of dissolution. The reconstituted specimens showed a double-structure microfabric that evolved with the level of consolidation stress and converged into a single-structure material (comparable to the natural shale) at a consolidation stress of more than twice the estimated maximum in situ effective stress. The natural shale had a lower specific surface area in comparison to the reconstituted material, which was consolidated at large effective stresses. These differences can be attributed to cementation at a submicron pore scale and highlight chemical diagenesis effects that were not replicated in the reconstituted specimens.

Keywords

Burial DiagenesisMercury Intrusion Porosimetry (MIP)MicrofossilsNitrogen Gas AdsorptionReconstituted SpecimensScanning/Backscattered Electron Microscopy(SEM/BSEM)
Type
Article
Information
Clays and Clay Minerals , Volume 65 , Issue 2 , April 2017 , pp. 135 - 153
Copyright
Copyright © Clay Minerals Society 2018

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References

Abdulhadi, N.O. Germaine, J.T. and Whittle, A.J., 2010 Experimental study of wellbore instability in clays Journal of Geotechnical and Geoenvironmental Engineering 137 766–776.CrossRefGoogle Scholar
Adams, A.L. Germaine, J.T. Flemings, P.B. and DayStirrat, R.J., 2013 Stress induced permeability anisotropy of oriented Boston Blue Clay Water Resources Research 49 6561–6571.CrossRefGoogle Scholar
Allman, M. and Atkinson, J., 1992 Mechanical properties of reconstituted Bothkennar soil Géotechnique 42 289–301.CrossRefGoogle Scholar
Al-Mukhtar, M. Belanteur, N. Tessier, D. and Vanapalli, S., 1996 The fabric of a clay soil under controlled mechanical and hydraulic stress states Applied Clay Science 11 99–115.CrossRefGoogle Scholar
Ambrose, R.J. Haryman, R.C. Diaz-Campos, M. Akkutlu, I.Y. and Sondergeld, C.H., 2012 Shale gas in-place calculations part 1: New pore-scale considerations SPE Journal 17 219–229.CrossRefGoogle Scholar
Awwiller, D., 1993 Illite/smectite formation and potassium mass transfer during burial diagenesis of mudrocks; a study from the Texas Gulf Coast Paleocene-Eocene Journal of Sedimentary Research 63 501–512.Google Scholar
Barrett, E.P. Joyner, L.G. and Halenda, P.P., 1951 The determination of pore volume and area distributions in porous substances: I Computations from nitrogen isotherms. Journal of the American Chemical Society 723 373–380.Google Scholar
Bjerrum, L., 1967 Progressive failure in slopes of overconsolidated plastic clay and clay shales: Third Terzaghi Lecture Journal of Soil Mechanics and Foundations Division 93 1–49.CrossRefGoogle Scholar
Bjørlykke, K. Aagaard, P., D.W, H. and E.D, P., 1992 Clay minerals in North Sea sandstones Origin, Diagenesis, and Petrophysics of Clay Minerals in Sandstones 65–80.CrossRefGoogle Scholar
Bock, H., 2000.RA Experiment: Data report on rock mechanics - Mont Terri project NAGRA Technical Report TN00-02Google Scholar
Brunauer, S. Emmett, P.H. and Teller, E., 1938 Adsorption of gases in multimolecular layers Journal of the American Chemical Society 60 309–319.CrossRefGoogle Scholar
Budhu, M., 2000 Soil Mechanics and Foundations New York John Wiley and Sons, Inc..Google Scholar
Burland, J., 1990 On the compressibility and shear strength of natural clays Géotechnique 40 329–378.CrossRefGoogle Scholar
Burton, G.J. Pineda, J.A. Sheng, D. and Airey, D., 2015 Microstructural changes of an undisturbed, reconstituted and compacted high plasticity clay subjected to wetting and drying Engineering Geology 193 363–373.CrossRefGoogle Scholar
Chalmers, G.R. and Bustin, R.M., 2015 Porosity and pore size distribution of deeply-buried fine-grained rocks: Influence of diagenetic and metamorphic processes on shale reservoir quality and exploration Journal of Unconventional Oil and Gas Resources 12 134–142.CrossRefGoogle Scholar
Chandler, R. J., 2010 Stiff sedimentary clays: geological origins and engineering properties Géotechnique 60 891–902.CrossRefGoogle Scholar
Clarkson, C.R. Wood, J. Burgis, S.E. Aquino, S.D. Freeman, M. and Birss, V.I., 2012.Nanopore structure analysis and permeability predictions for a tight gas/shale reservoir using low-pressure adsorption and mercury intrusion techniques Proceedings SPE Americas Unconventional Resources Conference 2012CrossRefGoogle Scholar
Corkum, A.G. and Martin, C.D., 2007 The mechanical behaviour of weak mudstone (Opalinus Clay) at low stresses International Journal of Rock Mechanics and Mining Sciences 44 196–209.CrossRefGoogle Scholar
Cotecchia, F. and Chandler, R.J., 1997 The influence of structure on the pre-failure behaviour of a natural clay Géotechnique 47 523–544.CrossRefGoogle Scholar
Cruz, M.R. and Reyes, E., 1998 Kaolinite and dickite formation during shale diagenesis: Isotopic data Applied Geochemistry 13 95–104.CrossRefGoogle Scholar
Curtis, C., 1980 Diagenetic alteration in black shales Journal of the Geological Society 137 189–194.CrossRefGoogle Scholar
Das, B.M., 2008 Advanced Soil Mechanics 3 New York Taylor & Francis 25–27.Google Scholar
Desbois, G. Urai, J.L. and Kukla, P.A., 2009 Morphology of the pore space in claystones — evidence from BIB/FIB ion beam sectioning and cryo-SEM observations eEarth 4 15–22.CrossRefGoogle Scholar
Desbois, G. Urai, J.L. Hemes, S. Brassinnes, S. De Craen, M. and Sillen, X., 2014 Nanometer-scale pore fluid distribution and drying damage in preserved clay cores from Belgian clay formations inferred by BIB-cryo-SEM Engineering Geology 179 117–131.CrossRefGoogle Scholar
Desbois, G. Urai, J.L. Kukla, P.A. Konstanty, J. and Baerle, C., 2011 High-resolution 3D fabric and porosity model in a tight gas sandstone reservoir: a new approach to investigate microstructures from mm- to nm-scale combining argon beam cross-sectioning and SEM imaging Journal of Petroleum Science and Engineering 78 243–257.CrossRefGoogle Scholar
Diamond, S., 1970 Pore size distributions in clays Clays and Clay Minerals 18 7–23.CrossRefGoogle Scholar
Dræge, A. Jakobsen, M. and Johansen, T.A., 2006 Rock physics modelling of shale diagenesis Petroleum Geoscience 12 49–57.CrossRefGoogle Scholar
Dullien, F.A., 1975 New network permeability model of porous media AIChE Journal 21 299–307.CrossRefGoogle Scholar
Favero, V. Ferrari, A. and Laloui, L., 2016 On the hydromechanical behaviour of remoulded and natural Opalinus Clay shale Engineering Geology 208 128–135.CrossRefGoogle Scholar
Freivogel, M. and Huggenberger, P., 2003 Modellierung bilanzierter profile im gebiet Mont Terri-La Croix (Kanton Jura): Mont Terri Project-Geology, paleohydrogeology and stress field of the Mont Terri region Federal Office for Water and Geology Rep 4 7–44.Google Scholar
Gaupp, R. Matter, A. Platt, J. Ramseyer, K. and Walzebuck, J., 1993 Diagenesis and fluid evolution of deeply buried Permian (Rotliegende) gas reservoirs, northwest Germany AAPG Bulletin 77 1111–1128.Google Scholar
Germaine, J.T., 1982 Development of the Directional Shear Cell for Measuring Cross Anisotropic Clay Properties Cambridge, MA Dept. Civil & Environmental Engineering, MIT.Google Scholar
Gregg, S.J. and Sing, K.S.W., 1983 Adsorption, Surface Area, and Porosity 2 New York Academic Press.Google Scholar
Hillier, S., 1993 Origin, diagenesis, and mineralogy of chlorite minerals in Devonian lacustrine mudrocks, Orcadian Basin, Scotland Clays and Clay Minerals 41 240–240.CrossRefGoogle Scholar
Hong, Z.-S. Yin, J. and Cui, Y.-J., 2010 Compression behaviour of remoulded soils at high initial water contents Géotechnique 60 691–700.CrossRefGoogle Scholar
Houben, M.E. Desbois, G. and Urai, J.L., 2014 A comparative study of representative 2D microstructures in shaly and sandy facies of Opalinus Clay (Mont Terri, Switzerland) inferred form BIB-SEM and MIP methods Marine and Petroleum Geology 19 143–161.CrossRefGoogle Scholar
Houben, M. Desbois, G. and Urai, J., 2013 Pore morphology and distribution in the shaly facies of Opalinus Clay (Mont Terri, Switzerland): Insights from representative 2D BIB-SEM investigations on mm to nm scale Applied Clay Science 71 82–97.CrossRefGoogle Scholar
Howard, J.J., 1991 Porosimetry measurement of shale fabric and its relationship to illite/smectite diagenesis Clays and Clay Minerals 39 355–361.CrossRefGoogle Scholar
Huggett, J.M., 1993 Diagenesis of mudrocks and concretions from the London Clay formation in the London Basin Clay Minerals 29 693–707.CrossRefGoogle Scholar
Kim, J.-W. Bryant, W. Watkins, J. and Tieh, T., 1998 Electron microscopic observations of shale diagenesis, offshore Louisiana, USA, Gulf of Mexico Geo-Marine Letters 18 234–240.CrossRefGoogle Scholar
Koliji, A. Vulliet, L. and Laloui, L., 2010 Structural characterization of unsaturated aggregated soil Canadian Geotechnical Journal 47 297–311.CrossRefGoogle Scholar
Kuila, U. and Prasad, M., 2013 Specific surface area and poresize distribution in clays and shales Geophysical Prospecting 61 341–362.CrossRefGoogle Scholar
Larson, R. and Morrow, N., 1981 Effects of sample size on capillary pressures in porous media Powder Technology 30 123–138.CrossRefGoogle Scholar
Laurich, B. Urai, J.L. Desbois, G. Klaver, J. Vollmer, C. and Nussbaum, C., 2017 Lessons learned from electron microscopy of deformed Opalinus clay Advances in Laboratory Testing and Modelling of Soils and Shales 345–350.CrossRefGoogle Scholar
Leroueil, S. and Vaughan, P., 1990 The general and congruent effects of structure in natural soils and weak rocks Géotechnique 40 467–488.CrossRefGoogle Scholar
Loucks, R.G. Reed, R.M. Ruppel, S.C. and Jarvie, D.M., 2009 Morphology, genesis, and distribution of nanometerscale pores in siliceous mudstones of the Mississippian Barnett Shale Journal of Sedimentary Research 79 848–861.CrossRefGoogle Scholar
Marschall, P. Horseman, S. and Gimmi, T., 2005 Characterisation of gas transport properties of the Opalinus Clay, a potential host rock formation for radioactive waste disposal Oil and Gas Science and Technology 60 121–139.CrossRefGoogle Scholar
Mazurek, M. Hurford, A.J. and Leu, W., 2006 Unravelling the multistage burial history of the Swiss Molasse Basin: Integration of apatite fission track, vitrinite reflectance and biomarker isomerisation analysis Basin Research 18 27–50.CrossRefGoogle Scholar
Mesri, G., 1973 Coefficient of secondary compression Journal of Soil Mechanics and Foundations Division 99 123–137.CrossRefGoogle Scholar
Morgan, S.P., 2015 An Experimental and Numerical Study on the Fracturing Processes in Opalinus Shale Cambridge, Massachussetts, USA Dept. Civil and Environmental Engineering, MIT.Google Scholar
Ninjgarav, E. Chung, S.-G. Jang, W.-Y. and Ryu, C.-K., 2007 Pore size distribution of Pusan clay measured by mercury intrusion porosimetry KSCE Journal of Civil Engineering 11 133–139.CrossRefGoogle Scholar
Nygård, R. Gutierrez, M. Gautam, R. and Høeg, K., 2004 Compaction behavior of argillaceous sediments as function of diagenesis Marine and Petroleum Geology 21 349–362.CrossRefGoogle Scholar
Ortega, J.A. Ulm, F.J. and Abousleiman, Y., 2011 The nanogranular origin of friction and cohesion in shale - A strength homogenization approach to interpretation of nanoindentation results International Journal of Numerical and Analytical Methods in Geomechanics 35 1854–1876.Google Scholar
Parker, S. P., 1997.McGraw-Hill Dictionary of Geology and MineralogyGoogle Scholar
Péron, H. Laloui, L. and Hueckel, T., 2006 An improved volume measurement for determining soil water retention curves Geotechnical Testing Journal 30 1–8.Google Scholar
Potter, P.E. Maynard, J.B. and Depetris, P.J., 2005.Mud and Mudstones: Introduction and OverviewCrossRefGoogle Scholar
Romero, E. and Simms, P.H., 2008 Microstructure investigation in unsaturated soils: A review with special attention to contribution of mercury intrusion porosimetry and environmental scanning electron microscopy Geotechnical and Geological Engineering 26 705–727.CrossRefGoogle Scholar
Rossi, C. and Alaminos, A., 2014 Evaluating the mechanical compaction of quartzarenites: The importance of sorting (Llanos foreland basin, Colombia) Marine and Petroleum Geology 56 222–238.CrossRefGoogle Scholar
Rutqvist, J., 2012 The geomechanics of CO2 storage in deep sedimentary formations Geotechnical and Geological Engineering 30 525–551.CrossRefGoogle Scholar
Sasanian, S. and Newson, T., 2013 Use of mercury intrusion porosimetry for microstructural investigation of reconstituted clays at high water contents Engineering Geology 158 15–22.CrossRefGoogle Scholar
Schneider, J. Flemings, P.B. Day-Stirrat, R.J. and Germaine, J.T., 2011 Insights into pore-scale controls on mudstone permeability through resedimentation experiments Geology 39 1011–1014.CrossRefGoogle Scholar
Schüth, F. Sing, K.S.W. and Weitkamp, J., 2002 Handbook of Porous Solids, Volume 1 Weinheim Wiley - VCH.CrossRefGoogle Scholar
Scotchman, I., 1989 Diagenesis of the Kimmeridge clay formation, onshore UK Journal of the Geological Society 146 285–303.CrossRefGoogle Scholar
Seiphoori, A., 2014.Thermo-hydro-mechanical Characterisation and Modelling of MX-80 Granular BentoniteGoogle Scholar
Seiphoori, A. Ferrari, A. and Laloui, L., 2014 Water retention behaviour and microstructural evolution of MX- 80 bentonite during wetting and drying cycles Géotechnique 64 721–734.CrossRefGoogle Scholar
Seiphoori, A. Moradian, Z. Whittle, A.J. and Einstein, H.H., 2016.Microstructural Characterization of Opalinus Shale 50th US Rock Mechanics/Geomechanics Symposium, the American Rock Mechanics AssociationGoogle Scholar
Shaw, H. and Primmer, T., 1991 Diagenesis of mudrocks from the Kimmeridge clay formation of the Brae area, UK North Sea Marine and Petroleum Geology 8 270–277.CrossRefGoogle Scholar
Sheldon, H.A. Wheeler, J. Worden, R.H. and Cheadle, M.J., 2003 An analysis of the roles of stress, temperature, and pH in chemical compaction of sandstones Journal of Sediment Research 73 64–71.CrossRefGoogle Scholar
Simms, P. and Yanful, E., 2002 Predicting soilùwater characteristic curves of compacted plastic soils from measured pore size distributions Géotechnique 52 269–278.CrossRefGoogle Scholar
Skempton, A.W., 1953 The Colloidal Activity of Clay Proc. 3rd International Conference on Soil Mechanics and Foundation Engineering 1 57–61.Google Scholar
Skempton, A.W., 1969 The consolidation of clays by gravitational compaction Quarterly Journal of the Geological Society 125 373–411.CrossRefGoogle Scholar
Skempton, A.W. and Jones, O., 1944 Notes on the compressibility of clays Quarterly Journal of the Geological Society 100 119–135.CrossRefGoogle Scholar
Slatt, R.M. and O’Brien, N.R., 2011 Pore types in the Barnett and Woodford gas shales: Contribution to understanding gas storage and migration pathways in fine-grained rocks AAPG bulletin 95 2017–2030.CrossRefGoogle Scholar
Snyder, R.L., 1992 The use of reference intensity ratios in Xray quantitative analysis Powder Diffraction 7 186–193.CrossRefGoogle Scholar
Thommes, M. Kaneko, K. Neimark, A.V. Oliver, J.P. Rodriguez-Reinoso, F. Rouquerol, J. and Sing, K.S.W., 2015 Physisorption of gases, with special reference to the evaluation of surface area and pore size distribution (IUPAC Technical Report) Pure and Applied Chemistry 87 1051–1069.CrossRefGoogle Scholar
Thompson, M.L. McBride, J.F. and Horton, R., 1985 Effects of drying treatments on porosity of soil materials Soil Science Society of America Journal 49 1360–1364.CrossRefGoogle Scholar
Touret, O. Pons, C.H. Tessier, D. and Tardy, Y., 1990 Etude de la répartition de l’eau dans des argiles saturées Mg2+ aux fortes teneurs en eau Clay Minerals 25 217–223.CrossRefGoogle Scholar
Tourtelot, H.A., 1979 Black shale - its deposition and diagenesis Clays and Clay Minerals 27 313–321.CrossRefGoogle Scholar
Washburn, E.W., 1921 The dynamics of capillary flow Physical Review 17 273–283.CrossRefGoogle Scholar
Webb, P.A. and Orr, C., 1997 Analytical Methods in Fine Particle Technology Georgia, USA Micromeritics, Norcross.Google Scholar
William, E. and Airey, D., 2009.The role of fabric in evaluating the failure mode of the stiffened Bringelly Shale 10th IAEG International Congress. IAEG 2006Google Scholar
Yu, C.Y. Chow, J.K. and Wang, Y.-H., 2016 Pore size changes and responses of kaolinite with different structures subject to consolidation and shearing Engineering Geology 202 22–131.CrossRefGoogle Scholar