correspondence Caprock corrosion a Argon 1st cycle CO2 flow test CO2 1st cycle CO2 flow test CO2 2nd cycle CO2 flow test CO2 3rd cycle 10–19 H2O flow test H2O 1st cycle H2O flow test H2O 2nd cycle Argon (postCO2 saturated water flow) b BEFORE Quartz Pore Chlorite Siderite 50 mm c Permeability (m2) To the Editor — The storage of naturally and industrially produced carbon dioxide in depleted hydrocarbon reservoirs and aquifers is viewed as an essential component of the strategy to combat the build-up of greenhouses gases in the atmosphere1. The success of these projects relies on the long-term integrity of low-permeability caprocks that must seal the CO2 within the reservoir 2,3. However, we find that the integrity of caprock can be altered by flowing CO2saturated aqueous fluid. Specifically, fluid flow under laboratory conditions through siltstone caprock sampled at one of the world’s largest carbon storage projects, In Salah in Algeria4, increases the permeability of the caprock by one order of magnitude under simulated reservoir conditions. The increase in permeability is caused by chemical reactions between the CO2-rich fluid and minerals commonly found in caprocks. We therefore argue that such geochemical interactions must be considered in geological carbon sequestration projects. The geological sequestration of CO2 is currently under investigation in field trials at sites including Weyburn in Canada5, Sleipner in the North Sea6 and In Salah in Algeria4. For carbon capture and storage to succeed, the integrity of the reservoir must be preserved over thousands of years. The injection of CO2 into saline aquifers and depleted hydrocarbon reservoirs inevitably alters the geochemical conditions of the reservoir (see Supplementary Information), but little is known about the effect of CO2 injection on the physical properties of the reservoir and caprocks. Pure CO2 is considered to be relatively inert in the rock matrix. However, contact with water leads to solution of the CO2, the creation of carbonic acid and partial dissociation leading to reduced fluid pH (ref. 7). When CO2 has been injected into oil fields for the purpose of enhancing oil recovery, the acidic CO2-rich aqueous fluids created in the subsurface reservoir is known to interact geochemically with rockforming minerals7. To test the influence of CO2-saturated fluid flow on caprock integrity, we selected a typical sample from the base of the caprock sequence of the Krechba gas field at In Salah. Here, about 0.5 megatons of CO2 are being injected into the subsurface each Chlorite AFTER Permeability increase Pore 10–20 Siderite Quartz 10 20 30 40 50 Effective pressure (MPa) 60 70 Figure 1 | Changes in permeability and microstructure of a sample of caprock from In Salah, Algeria, caused by various pore fluids. a, Permeability measured using various single-phase pore fluids over a range of effective pressures shows no change. Measurements made after CO2-saturated water flow show permeability has increased by approximately 8-fold. b,c, Scanning electron microscope images before (b) and after (c) the flow of CO2-saturated water. Dissolution of the minerals chlorite and siderite increases pore throat radii and hence porosity. year (see Supplementary Information). The Lower Carboniferous caprock at In Salah is a 950-m-thick mudstone, of which the lower part is a thinly bedded estuarine siltstone that contains no organic material or swelling clays8,9. Mineralogical analyses of the lower part of the caprock show the presence of the dominant silicate minerals quartz, illite and potassium feldspar, with subordinate quantities of chlorite and kaolinite, and small quantities of siderite and pyrite8. Extensive characterization of the lower caprock3,8 confirmed that our sample was representative of the lower caprock as a whole. In the laboratory, we investigated experimentally whether any changes in caprock permeability could be attributed to pore-fluid–rock interactions (Fig. 1). We used a high-pressure permeameter 9 and replicated in situ reservoir-stress conditions at room temperature (see Supplementary Information). We first measured the initial permeability of the sample of caprock using argon — an inert pore fluid — over a range of effective pressures. Subsequently, we used dry CO2 and then distilled water NATURE GEOSCIENCE | VOL 6 | FEBRUARY 2013 | www.nature.com/naturegeoscience © 2013 Macmillan Publishers Limited. All rights reserved to again measure permeability over the same pressure range. Experiments using each of these single-phase fluids gave the same values for permeability (within experimental uncertainty) over the same pressure range. We also varied the method for permeability measurement, using both the pulse transient and constant flow methods. The method of permeability measurement had no effect on the result. We then flowed CO2-saturated water through the sample at approximate reservoir pressure conditions (45 MPa confining pressure, 20 MPa pore pressure and 25 MPa effective pressure) for 72 hours (Supplementary Fig. S3). The flux of fluid through the sample during the experiment was 0.015 cm3 hr–1, which equates to a volume of fluid that is about 4.07-times that of the pore volume of the sample. We found that the permeability of the caprock sample increased by approximately a factor of 8 during the experiment (Fig. 1). The pressure difference across the sample decreased throughout the experiment as the permeability increased (Supplementary Fig. S3). 79 correspondence The sample was then placed in a vacuum oven to remove any remaining pore fluid. Using inert argon, we performed a series of pulse transient permeability measurements across the range of effective pressures previously used for the other pore fluids. This final experiment confirmed that permanent change in the permeability of the caprock had occurred as a result of the passage of CO2-saturated water through the sample (Fig. 1). Mechanical effects can be discounted as the cause of the change because the permeability of the caprock was unaffected by the flow of either dry CO2 or distilled water. The increase in permeability during the flow of CO2-saturated water has most probably been caused by geochemical processes. Petrophysical analyses before and after the CO2-saturated water flow test showed that the sample porosity increased from 7 to 10%, its weight decreased from 6.83 to 6.39 g and the internal surface area decreased from 0.901to 0.423 m2 g–1. We used X-ray diffraction to compare the mineral content of an unaffected caprock sample to that of our experimental sample. The caprock that had been subject to CO2-saturated fluid flow showed significant loss of the mineral cements siderite (iron carbonate) and chlorite (iron-rich aluminosilicate clay) (Supplementary Fig. S2). Scanning-electron microscope examination of polished thin sections of the experimental sample revealed a substantial change to the typical pore network and confirmed the dissolution of siderite and chlorite from the sample, both in pores and in pore throats (Fig. 1). These changes were 80 fairly uniform throughout the sample, and did not seem focussed along preferential pathways. The loss of chlorite and siderite caused a net increase in porosity and opened up pore throats, leading to a corresponding increase in permeability. This finding is consistent with previous results based on crushed bulk rock samples3,10. Typical reservoir temperatures are about 95 °C — much higher than our room temperature experiments. A higher in situ temperature would probably increase reaction rates, so the permeability increase could occur on shorter timescales than in our experiments. Higher temperatures may also result in a marginally different pH of the fluid. Although the experimental temperature used is below the critical temperature for CO2, the fluid pressure used is much greater than the critical pressure. Consequently, the CO2 should not experience any phase changes owing to higher temperature at reservoir conditions: the liquid will only become less dense. The overall integrity of the caprock seal as a whole may not necessarily be compromised. Reaction between the pore fluid and caprock is likely to occur only in the immediate vicinity of the caprock–fluid interface, close to the injector wells in a reservoir. Furthermore, minerals dissolved at one location may precipitate elsewhere, in parts of the caprock with lower chemical potential, some distance along the flow path in the reservoir. Thus, caprock integrity might actually be enhanced in these regions and may ameliorate the local permeability increase. The balance between dissolution and precipitation within caprock horizons requires further investigation. Our results show that the chemistry of fluids injected into carbon sequestration systems can significantly alter the physical properties of the overlying caprock. Our study was performed on rock from the In Salah project, but may be applicable to other existing, or future, carbon storage sites: the minerals lost during the reaction are common constituents of a variety of caprock types. Our results do not imply that carbon storage sites will necessarily leak over time, but they illustrate that reactive fluid flow at carbon storage sites should be a fundamental consideration before routine large-scale injection of CO2 commences. ❐ References 1. IPCC Working Group III Special Report on Carbon Dioxide Capture and Storage (Cambridge Univ. Press, 2005). 2. Wollenweber, J. et al. Int. J. Greenh. Gas Con. 4, 231–241 (2010). 3. Carroll, S. A., McNab, W. W. & Torres, S. C. Geochem. Trans. 12, 9 (2011). 4. Riddiford, F. A., Tourqui, A., Bishop, C. D., Taylor, B. & Smith, M. in Greenhouse Gas Control Technologies Vol. 1 (eds Gale, J. & Kaya, Y.) 595–600 (2003). 5. Riding, J. B. et al. in Greenhouse Gas Control Technologies Vol. 2 (eds Gale, J. & Kaya, Y.) 1629–1632 (2003). 6. Torp, T. A. & Gale, J. in Greenhouse Gas Control Technologies Vol. 1 (eds Gale, J. & Kaya, Y.) 311–316 (2003). 7. Worden, R. H. & Smith, L. K. in Geological Storage of Carbon Dioxide Vol. 233 (eds Baines, S. & Worden, R. H.) 211–224 (Geological Society Special Publication, 2004). 8. Armitage, P. J. et al. Mar. Petrol. Geol. 27, 1395–1410 (2010). 9. Armitage, P. J. et al. J. Geophys. Res. 116, B12208 (2011). 10. Czernichowski-Lauriol, I. et al. in Final Report of JOULE II Project CT92–0031: The Underground Disposal of Carbon Dioxide (ed Holloway, S.) 183–276 (British Geological Survey, 1996). P. J. Armitage, D. R. Faulkner* and R. H. Worden Department of Geology and Geophysics, School of Environmental Sciences, University of Liverpool, Liverpool, L69 3GP, UK. *e-mail: faulkner@liv.ac.uk NATURE GEOSCIENCE | VOL 6 | FEBRUARY 2013 | www.nature.com/naturegeoscience © 2013 Macmillan Publishers Limited. All rights reserved