Transport in Porous Media

, Volume 121, Issue 1, pp 135–181 | Cite as

Comparative Study of Five Outcrop Chalks Flooded at Reservoir Conditions: Chemo-mechanical Behaviour and Profiles of Compositional Alteration

  • P. Ø. Andersen
  • W. Wang
  • M. V. Madland
  • U. Zimmermann
  • R. I. Korsnes
  • S. R. A. Bertolino
  • M. Minde
  • B. Schulz
  • S. Gilbricht


This study presents experimental results from a flooding test series performed at reservoir conditions for five high-porosity Cretaceous onshore chalks from Denmark, Belgium and the USA, analogous to North Sea reservoir chalk. The chalks are studied in regard to their chemo-mechanical behaviour when performing tri-axial compaction tests while injecting brines (0.219 mol/L \(\hbox {MgCl}_{2}\) or 0.657 mol/L NaCl) at reservoir conditions for 2–3 months (T = 130 \(^\circ \hbox {C}\); 1 PV/d). Each chalk type was examined in terms of its mineralogical and chemical composition before and after the mechanical flooding tests, using an extensive set of analysis methods, to evaluate the chalk- and brine-dependent chemical alterations. All \(\hbox {MgCl}_{2}\)-flooded cores showed precipitation of Mg-bearing minerals (mainly magnesite). The distribution of newly formed Mg-bearing minerals appears to be chalk-dependent with varying peaks of enrichment. The chalk samples from Aalborg originally contained abundant opal-CT, which was dissolved with both NaCl and \(\hbox {MgCl}_{2}\) and partly re-precipitated as Si-Mg-bearing minerals. The Aalborg core injected with \(\hbox {MgCl}_{2}\) indicated strongly increased specific surface area (from 4.9 \(\hbox {m}^{2}\hbox {/g}\) to within 7–9 \(\hbox {m}^{2}\hbox {/g}\)). Mineral precipitation effects were negligible in chalk samples flooded with NaCl compared to \(\hbox {MgCl}_{2}\). Silicates were the main mineralogical impurity in the studied chalk samples (0.3–6 wt%). The cores with higher \(\hbox {SiO}_{2}\) content showed less deformation when injecting NaCl brine, but more compaction when injecting \(\hbox {MgCl}_{2}\)-brine. The observations were successfully interpreted by mathematical geochemical modelling which suggests that the re-precipitation of Si-bearing minerals leads to enhanced calcite dissolution and mass loss (as seen experimentally) explaining the high compaction seen in \(\hbox {MgCl}_{2}\)-flooded Aalborg chalk. Our work demonstrates that the original mineralogy, together with the newly formed minerals, can control the chemo-mechanical interactions during flooding and should be taken into account when predicting reservoir behaviour from laboratory studies. This study improves the understanding of complex flow reaction mechanisms also relevant for field-scale dynamics seen during brine injection.


Chalk compaction Creep acceleration Dissolution–precipitation Core flooding at reservoir conditions Non-carbonate composition 

List of symbols

\(a _\mathrm{h}\)

Activity of \(\hbox {H}^{+}\)


Area (\(\hbox {m}^{2}\))

\(C _{i}\)

Concentration variable of species i (mol/L pore volume)


Core diameter (mm)

\(k _{1,i, } k _{2,i}\)

Reaction rate parameter for mineral i (mol/m\(^{2}\)/s)

\(k _\mathrm{o}\)

Original permeability (mD)

\(K _{i}\)

Solubility constant of mineral i (–)


Core length (mm)


Mass (g)

\(p _{i}, q _{i}, r _{i}, n _{i}\)

Reaction order parameters (–)


Injection rate (mL/d)


Volume (L or \(\hbox {cm}^{3}\))

\(\updelta ^{13}\hbox {C}\)

A measure of the ratio of stable isotopes \(^{13}\hbox {C}\) and \(^{12}\hbox {C}\) ( Open image in new window )

\(\updelta ^{18}\hbox {O}\)

A measure of the ratio of stable isotopes \(^{18}\hbox {O}\) and \(^{16}\hbox {O}\) ( Open image in new window )

\(\varepsilon \)

Axial creep strain (%)


Solid density (\(\hbox {cm}^{3}\hbox {/L}\))

\(\rho _{w}\)

Brine density (\(\hbox {cm}^{3}\hbox {/L}\))

\(\varPhi \)

Porosity (%)

\({\Omega }_i \)

Saturation state of mineral i (–)



Bulk volume (solids and pores)


Based on the core piece


Dry sample


State after compaction–flooding tests


Original/unflooded state


Based on pycnometry


Saturated sample







Below detection limit


Brunauer–Emmett–Teller theory

\(\hbox {DI-H}_{2}\hbox {O}\)

Deionized water


Distilled water


Energy-dispersive X-ray spectroscopy


Energy-dispersive X-ray


Field emission gun-scanning electron microscopy


Fluorinated ethylene propylene




High-performance liquid chromatography


Inductively coupled plasma atomic emission spectroscopy


Inductively coupled plasma mass spectrometry


Ion chromatography system






Loss on ignition (wt%)


Linear variable displacement transducer


(Automated SEM) mineral liberation analysis




Proportional integral derivative


Part per million


Pore volume




Stevns Klint


Standard mean ocean water composition in Vienna Pee Dee Belemnite


Specific surface area (\(\hbox {m}^{2}\hbox {/g}\))

Sup. Mat.

Supplementary Material


Total dissolved solids (g/L)


Transmission electron microscopy


Total carbon (wt%)


Weight per cent


X-ray diffraction



The authors thank the Faculty of Science and Technology for the PhD grant for W. Wang. Thanks are due to the SEM work (AA5) done by Tania Hildebrand–Habel. The authors thank COREC for financial support for this research study and acknowledge the Research Council of Norway and the industry partners: ConocoPhillips Skandinavia AS, BP Norge AS, Det Norske Oljeselskap AS, Eni Norge AS, Maersk Oil Norway AS, DONG Energy A/S, Denmark, Statoil Petroleum AS, ENGIE E&P NORGE AS, Lundin Norway AS, Halliburton AS, Schlumberger Norge AS, Wintershall Norge AS of The National IOR Centre of Norway for support. The research presented is integral part of the PhD thesis of W. Wang at UiS.

Supplementary material

11242_2017_953_MOESM1_ESM.docx (6.6 mb)
Supplementary material 1 (docx 6746 KB)
11242_2017_953_MOESM2_ESM.docx (133 kb)
Supplementary material 2 (docx 133 KB)


  1. Andersen, P.Ø., Evje, S., Madland, M.V., Hiorth, A.: A geochemical model for interpretation of chalk core flooding experiments. Chem. Eng. Sci. 84, 218–241 (2012). CrossRefGoogle Scholar
  2. Andersen, P.Ø., Evje, S.: A model for reactive flow in fractured porous media. Chem. Eng. Sci. 145, 196–213 (2016). CrossRefGoogle Scholar
  3. Appelo, C.A.J., Postma, D.: Geochemistry, Groundwater and Pollution. Taylor & Francis Group, Boca Raton (2005)CrossRefGoogle Scholar
  4. Bertolino, S.A.R., Zimmermann, U., Madland, M.V., Hildebrand-Habel, T., Hiorth, A., Korsnes, R.I.: Mineralogy, geochemistry and isotope geochemistry to reveal fluid flow process in flooded chalk under long term test conditions for EOR purposes. In: XV International Clay Conference, Brasil, vol. 676 (2013)Google Scholar
  5. Bjørlykke, K., Høeg, K.: Effects of burial diagenesis on stresses, compaction and fluid flow in sedimentary basins. Mar. Petrol. Geol. 14, 267–276 (1997). CrossRefGoogle Scholar
  6. Bjørlykke, K.: Relationships between depositional environments, burial history and rock properties. Some principal aspects of diagenetic process in sedimentary basins. Sediment. Geol. 301, 1–14 (2014). CrossRefGoogle Scholar
  7. Brindley, G.W., Brown, G.: Crystal structure of clay minerals and their X-ray identification. In: Brindley, G.W., Brown, G. (eds.) Mineralogical Society Monograph, vol. 5, pp. 361–410. Mineralogical Society, London (1980)Google Scholar
  8. Collin, F., Cui, Y.J., Schroeder, C., Charlier, R.: Mechanical behaviour of Lixhe chalk partly saturated by oil and water: experiment and modelling. Int. J. Numer. Anal. Methods 26, 897–924 (2002). CrossRefGoogle Scholar
  9. Engstrøm, F.: Rock mechanical properties of Danish North Sea chalk. In: Proceedings of 4th North Sea Chalk Sym, Deauville (1992)Google Scholar
  10. Fabricius, I.L.: Compaction of microfossil and clay-rich chalk sediments. Phys. Chem. Earth Part A 26, 59–62 (2001). CrossRefGoogle Scholar
  11. Fabricius, I.L., Borre, M.K.: Stylolites, porosity, depositional texture, and silicates in chalk facies sediments. Ontong Java Plateau–Gorm and Tyra fields, North Sea. Sedimentology 54, 183–205 (2007). CrossRefGoogle Scholar
  12. Fabricius, I.L., Hoier, C., Japsen, P., Korsbech, U.: Modelling elastic properties of impure chalk from South Arne field, North Sea. Geophys. Prospect. 55, 487–506 (2007). CrossRefGoogle Scholar
  13. Fjær, E., Holt, R.M., Horsrud, P., Raaen, A.M., Risnes, R.: Petroleum Related Rock Mechanics, 2nd edn, pp. 491–492. Elsevier, Amsterdam (2008)Google Scholar
  14. Frykman, P.: Spatial variability in petrophysical properties in Upper Maastrichtian chalk outcrops at Stevns Klint, Denmark. Mar. Petrol. Geol. 18, 1041–1062 (2001). CrossRefGoogle Scholar
  15. Gaviglio, P., Vandycke, S., Schroeder, C., Coulon, M., Bergerat, F., Dubois, C., Pointeau, I.: Matrix strains along normal fault planes in the Campanian white chalk of Belgium: structural consequences. Tectonophysics 309, 41–56 (1999). CrossRefGoogle Scholar
  16. Hart, M.B., Feist, S.E., Price, G.D., Leng, M.J.: Reappraisal of the K–T boundary succession at Stevns Klint, Denmark. J. Geol. Soc. Lond. 161, 885–892 (2004). CrossRefGoogle Scholar
  17. Hart, M.B., Feist, S.E., Håkansson, E., Heinberg, C., Price, G.D., Leng, M.J., Watkinson, M.P.: The Cretaceous–Palaeogene boundary succession at Stevns Klint, Denmark: foraminifers and stable isotope stratigraphy. Palaeogeogr. Palaeoecol. 224, 6–26 (2005). CrossRefGoogle Scholar
  18. Havmøller, O., Foged, N.: Review of rock mechanical data for chalk. In: Proceedings of 5th North Sea Chalk Sym, Reims (1996)Google Scholar
  19. Hellmann, R., Renders, P., Gratier, J., Guiguet, R.: Experimental pressure solution compaction of chalk in aqueous solutions Part 1. Deformation behavior and chemistry. In: Hellmann, R., Wood., S.A. (eds.) Water–Rock Interactions, Ore Deposits, and Environmental Geochemistry: A Tribute to Davod A. Crerar, vol. 7, pp. 129–152 (2002).
  20. Hermansen, H., Thomas, L.K., Sylte, J.E., Aasboe, B.T.: Twenty five years of Ekofisk reservoir management. In: SPE Annual Technical Conference and Exhibition San Antonio, Texas, vol. 873–885 (1997).
  21. Hermansen, H., Landa, G.H., Sylte, J.E., Thomas, L.K.: Experiences after 10 years of waterflooding the Ekofisk Field, Norway. J. Petrol. Sci. Eng. 26, 11–18 (2000). CrossRefGoogle Scholar
  22. Hiorth, A., Jettestuen, E., Cathles, L.M., Madland, M.V.: Precipitation, dissolution, and ion exchange processes coupled with a lattice Boltzmann advection diffusion solver. Geochim. Cosmochim. Acta 104, 99–110 (2013). CrossRefGoogle Scholar
  23. Hjuler, M.L.: Diagenesis of upper cretaceous onshore and offshore chalk from the North Sea area. PhD thesis, Technical University of Denmark, pp. 11–23 (2007)Google Scholar
  24. Hjuler, M.L., Fabricius, I.L.: Engineering properties of chalk related to diagenetic variations of Upper Cretaceous onshore and offshore chalk in the North Sea area. J. Petrol. Sci. Eng. 68, 151–170 (2009). CrossRefGoogle Scholar
  25. Jarvis, I.: The Santonian–Campanian phosphatic chalks of England and France. Proc. Geol. Assoc. 117, 219–237 (2006). CrossRefGoogle Scholar
  26. Korsnes, R.I., Strand, S., Hoff, Ø., Pedersen, T., Madland, M.V., Austad, T.: Does the chemical interaction between seawater and chalk affect the mechanical properties of chalk? In: The International Symposium of the International Society for Rock Mechanics (2006a).
  27. Korsnes, R.I., Madland, M.V., Austad, T.: Impact of brine composition on the mechanical strength of chalk at high temperature. In: The International Symposium of the International Society for Rock Mechanics. Liége, Belgium (2006b).
  28. Korsnes, R.I., Madland, M.V., Austad, T., Haver, S., Røsland, G.: The effects of temperature on the water weakening of chalk by seawater. J. Petrol. Sci. Eng. 60(3), 183–193 (2008)CrossRefGoogle Scholar
  29. Madland, M.V., Midtgarden, K., Manafov, R., Korsnes, R.I., Kristiansen, T., Hiorth, A.: The effect of temperature and brine composition on the mechanical strength of Kansas chalk. In: International Symposium SCA (2008)Google Scholar
  30. Madland, M.V., Hiorth, A., Omdal, E., Megawati, M., Hildebrand-Habel, T., Korsnes, R.I., Evje, S., Cathles, L.M.: Chemical alterations induced by rock-fluid interactions when injecting brines in high porosity chalks. Transp. Porous Med. 87, 679–702 (2011). CrossRefGoogle Scholar
  31. McLennan, S.M., Taylor, S.R., Hemming, S.R.: Composition, differentiation, and evolution of continental crust: constraints from sedimentary rocks and heat flow. In: Brown, M., Rushmer, T. (eds.) Evolution and Differentiation of the Continental Crust, pp. 92–134. Cambridge Univ Press, Cambridge (2006)Google Scholar
  32. Megawati, M., Andersen, P. Ø., Korsnes, R.I., Evje, S., Hiorth, A., Madland, M.V.: The effect of aqueous chemistry pH on the time-dependent deformation behaviour of chalk experimental and modelling study. In: Pore2Fluid International Conference. Paris, France (2011)Google Scholar
  33. Megawati, M., Madland, M.V., Hiorth, A.: Mechanical and physical behavior of high-porosity chalks exposed to chemical perturbation. J. Petrol. Sci. Eng. 133, 313–327 (2015). CrossRefGoogle Scholar
  34. Molenaar, N., Zijlstra, J.J.P.: Differential early diagenetic low-Mg calcite cementation and rhythmic hardground development in Campanian–Maastrichtian chalk. Sediment. Geol. 109, 261–281 (1997). CrossRefGoogle Scholar
  35. Nagel, N.B.: Compaction and subsidence issues within the petroleum industry: from Wilmington to Ekofisk and beyond. Phys. Chem. Earth. Part A 26, 3–14 (2001). CrossRefGoogle Scholar
  36. Nermoen, A., Korsnes, R.I., Hiorth, A., Madland, M.V.: Porosity and permeability development in compacting chalks during flooding of nonequilibrium brines: insights from long-term experiment. J. Geophys. Res. Solid Earth 120, 2935–2960 (2015). CrossRefGoogle Scholar
  37. Nermoen, A., Korsnes, R.I., Aursjø, O., Madland, M.V., Kjørslevik, T.A.C., Østensen, G.: How stress and temperature conditions affect rock-fluid chemistry and mechanical deformation. Front. Phys. 4, 1–19 (2016). CrossRefGoogle Scholar
  38. Neveux, L., Grgic, D., Carpentier, C., Pironon, J., Truche, L., Girard, J.P.: Experimental simulation of chemomechanical processes during deep burial diagenesis of carbonate rocks. J. Geophys. Res. Solid Earth 119, 984–1007 (2014). CrossRefGoogle Scholar
  39. Newman, G.H.: The effect of water chemistry on the laboratory compression and permeability characteristics of some North Sea chalks. J. Petrol. Technol. 35, 976–980 (1983). CrossRefGoogle Scholar
  40. Palandri, J.L., Kharaka, Y.K.: A Compilation of Rate Parameters of Water–Mineral Interaction Kinetics for Application to Geochemical Modeling. U. S. Geological Survey, Menlo Park (2004)Google Scholar
  41. Parkhurst, D.L., Appelo, C.A.J.: Description of input and examples for PHREEQC version 3—a computer program for speciation, batch-reaction, one-dimensional transport, and inverse geochemical calculations. U.S. Geological Survey Techniques and Methods, Chap. A43 (2013)Google Scholar
  42. Paterson, M.S.: Nonhydrostatic thermodynamics and its geologic applications. Rev. Geophys. Space Phys. 11, 355–389 (1973). CrossRefGoogle Scholar
  43. Putnis, A.: Mineral replacement reactions: from macroscopic observations to microscopic mechanisms. Miner. Mag. 66, 689–708 (2002). CrossRefGoogle Scholar
  44. Risnes, R., Flaageng, O.: Mechanical properties of chalk with emphasis on chalk-fluid interactions and micromechanical aspects. Oil Gas Sci. Technol. 54, 751–758 (1999). CrossRefGoogle Scholar
  45. Risnes, R., Madland, M.V., Hole, M., Kwabiah, N.K.: Water weakening of chalk—mechanical effects of water-glycol mixtures. J. Petrol. Sci. Eng. 48, 21–36 (2005). CrossRefGoogle Scholar
  46. Ruiz-Agudo, E., Putnis, C.V., Putnis, A.: Coupled dissolution and precipitation at mineral-fluid interfaces. Chem. Geol. 383, 132–146 (2014). CrossRefGoogle Scholar
  47. Rutter, E.H.: The kinetics of rock deformation by pressure solution. Philos. Trans. R. Soc. Lond. 283, 203–219 (1976)CrossRefGoogle Scholar
  48. Schroeder, C., Gaviglio, P., Bergerat, F., Vandycke, S., Coulon, M.: Faults and matrix deformations in chalk: contribution of porosity and sonic wave velocity measurements. Bull. Acad. Vet. Fr. 177, 203–213 (2006). Google Scholar
  49. Strand, S., Standnes, D.C., Austad, T.: Spontaneous imbibition of aqueous surfactant solutions into neutral to oil-wet carbonate cores? Effects of brine salinity and composition. Energy Fuels 17, 1133–1144 (2003). CrossRefGoogle Scholar
  50. Strand, S., Hjuler, M.L., Torsvik, R., Pedersen, J., Madland, M.V., Austad, T.: Wettability of chalk: impact of silica, clay content and mechanical properties. Petrol. Geosci. 13, 69–80 (2007). CrossRefGoogle Scholar
  51. Tang, G.Q., Firoozabadi, A.: Effect of pressure gradient and initial water saturation on water injection in water-wet and mixed-wet fractured porous media. SPE Res. Eval. Eng. 4, 516–524 (2001). Google Scholar
  52. Van den Bark, E., Thomas, O.D.: Ekofisk-1st of the giant oil-fields in Western Europe. AAPG Bull. 65, 2341–2363 (1981)Google Scholar
  53. Wang, W., Madland, M.V., Zimmermann, U., Nermoen, A., Korsnes, R.I., Bertolino, S.A.R., Hildebrand-Habel, T.: Evaluation of porosity change during chemo–mechanical compaction in flooding experiments on Liège outcrop chalk. In: Armitage, P.J., Butcher, A.R., Churchill, J.M., Csoma, A.E., Hollis, C., Lander, R.H., Omma, J.E. Worden, R.H. (eds.) Reservoir Quality of Clastic and Carbonate Rocks: Analysis, Modelling and Prediction. Journal of the Geological Society London. Special Publications, vol. 435 (2016).
  54. Zhang, X., Spiers, C.J., Peach, C.J.: Compaction creep of wet granular calcite by pressure solution at 28 \(^{\circ }\text{ C }\) to 150 \(^{\circ }\text{ C }\). J. Geophys. Res. 115, 1–18 (2010). CrossRefGoogle Scholar
  55. Zhang, X., Spiers, C.J., Peach, C.J.: Effects of pore fluid flow and chemistry on compaction creep of calcite by pressure solution at 150 \(^{\circ }\text{ C }\). Geofluids 11, 108–122 (2011). CrossRefGoogle Scholar
  56. Zimmermann, U., Madland, M.V., Bertolino, S.A.R., Hildebrand-Habel, T.: Tracing fluid flow in flooded chalk under long term test conditions. In: 75th EAGE Conference & Exhibition Incorporating SPE. London (2013)Google Scholar
  57. Zimmermann, U., Madland, M.V., Nermoen, A., Hildebrand-Habel, T., Bertolino, S.A.R., Hiorth, A., Korsnes, R.I., Audinot, J.N., Grysan, P.: Evaluation of the compositional changes during flooding of reactive fluids using scanning electron microscopy, nano-secondary ion mass spectrometry, X-ray diffraction and whole rock geochemistry. AAPG Bull. 99, 791–805 (2015). CrossRefGoogle Scholar

Copyright information

© Springer Science+Business Media B.V. 2017

Authors and Affiliations

  1. 1.Department of Petroleum TechnologyUniversity of StavangerStavangerNorway
  2. 2.The National IOR Centre of NorwayUniversity of StavangerUllandhaug, StavangerNorway
  3. 3.FaMAFUniversidad Nacional de CórdobaCórdobaArgentina
  4. 4.IRIS AS, International Research Institute of StavangerUllandhaug, StavangerNorway
  5. 5.Department of Economic Geology and PetrologyTU Bergakademie FreibergFreibergGermany

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