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SPE-Not Apply-MS

Rock/water Interaction of Low-Salinity: Impact on the Properties of the

Porous Medium focusing on dissolution for carbonate reservoirs
C. C. Angarita, S. A. R. Soler, State University of Campinas.

Copyright 2017, Society of Petroleum Engineers

This paper was prepared for presentation as part of the course PP302 - Reservoir Engineering II held at State University of Campinas, Brazil, 7 December 2017.

This paper was selected for presentation by an SPE program committee following review of information contained in an abstract submitted by the author(s). Contents
of the paper have not been reviewed by the Society of Petroleum Engineers and are subject to correction by the author(s). The material does not necessarily reflect any
position of the Society of Petroleum Engineers, its officers, or members. Electronic reproduction, distribution, or storage of any part of this paper without the written
consent of the Society of Petroleum Engineers is prohibited. Permission to reproduce in print is restricted to an abstract of not more than 300 words; illustrations may
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Abstract
The potential of low salinity water injection to improve oil recovery has recently generated interest
both from petroleum science and industry. During this process, multiple interactions between injected
fluid and the reservoir rock occur, including the one generated by the presence of water with salinity lower
than the water in equilibrium with the rock, which cause the dissolution. In carbonates (CB), which
comprise more than half of the world’s hydrocarbon reservoirs, several experimental studies have
highlighted the importance of carbonate solubility in the recovery process. The predominant process
indeed involves the dissolution of carbonates and possibly silicates, depending on the kinetics of
individual chemical components.

The main objective of this paper is present a literature review of the rock/water interactions of low
salinity focusing on dissolution for carbonate reservoirs, and its impact on the properties of the porous
medium. Once presented the recapitulation, there are exposed two case studies, both emphasizing on the
dynamic of chemical reactions between low salinity water and porous media mainly focusing in carbonate
rock dissolution. The first study (Case A), developed by Omekeh et al. (2014), was found that the recovery
is very dependent on the individual brine composition and that dissolution of calcite tends to reduce
desorption of calcium ions from the rock surface and hence the possibility to improve recovery by the
multicomponent ion exchange mechanism. The study also shows the calcite dissolution can change the
brine composition of the injected brine deep in the reservoir and hence alter the intended chemistry of the
brine-rock interaction. Similarly, the second study presented (Case B) was carried out by Austad et al.
(2015) and confirmed that it is possible to obtain low salinity EOR (Enhanced oil recovery) effects also in
carbonates, and not only in sandstones. It was verified, that the core material contained significant amounts
of anhydrite (CaSO4), which appeared to be the key factor for observing the low salinity EOR effect.
2 SPE-Not Apply-MS

Introduction
Seawater injection has been applied for secondary recovery of oil for decades in offshore fields. The
technique combines the proved practice for pressure support and the vast and immediate source of water,
reducing at the same time facility requirements and environmental impacts. The efficiency of seawater as
an Improved Oil Recovery (IOR) fluid, however, depends on the thermodynamic conditions and
heterogeneity/structure of the reservoir. Because of this, in recent years, controlling the salinity and
composition of the injected water has become an emerging EOR technique, often described as low-salinity
(LS) water flooding. The low salinity water injection technique, essentially means that more oil may be
produced by flooding with a brine with a low concentration of ions.

Many researchers have reported, from both field and laboratory tests, an increase in oil recovery by LS
floodings. The understanding of the LS mechanism is however debatable, and many theories have been
proposed. The complexity and number of parameters behind oil/brine/rock interactions are the main
reason. Different mechanism(s) may act together or in sequence. Various processes have been proposed
for the last few years, with the most popular processes being double-layer effects, an increase in pH,
migration of fines, multi-component ionic exchange (MIE), mineral dissolution, and microscopically
diverted flow. Bernard et al. (1967) concluded that cores containing clays will produce more oil with
fresh water waterflooding that with brine. Zhang et al. (2006) reported wettability alteration towards more
water-wet conditions for low salinity water in high presence of SO−2 2+
4 and divalent cations (Mg and Ca )
2+

in order to improve oil recovery. Al Harrasi et al. (2012) carried out spontaneous imbibition tests with low
salinity brine, and the results showed an enhance oil recovery until 21% of the original oil in place, using
formation brine diluted 100 times.

In carbonates, which comprise more than half of the world’s hydrocarbon reservoirs, the main process
involves the dissolution of carbonates and possibly silicates, depending on the kinetics of individual
chemical components. Near the injection well, where the unbalance is greater, the dissolution processes
may irreversibly affect the mechanical properties and fluid dynamic parameters of the rock. Specifically,
the dissolution leads to increase in porosity and permeability, as well as changes in the reactive surface
area of the mineral. By its turn, increased cation concentrations produced by carbonate dissolution can
supersaturate the fluid ahead in the flow. In this case, precipitation may conduct to decreases in porosity
and permeability. Also, the insoluble material (calcite) can block the porous media after the deposition in
narrow pore throats. Changes in the solid matrix can alter the pore structure, inducing changes in fluid
flow properties across the porous media affecting ultimately oil recovery from the reservoir. The possible
reduction of porosity and permeability in the regions near the production well will decrease oil production
and affect field development. Several studies and a few field tests have reported positive effects for oil
recovery of the injection of low salinity water (LSW). Studies on the dissolution phenomena with the
injection of LSW in carbonates are particularly important in the case the technique of LSW is considered
for the enhancement of oil production.

Statement of Theory
Chemical reactions occur in geological reservoirs and can induce mineral dissolution. Depending on
composition of the injected fluid, the geochemical equilibrium between rock and fluids can be altered,
inducing mineral dissolution. In static conditions, the presence of water with salinity lower than the water
in equilibrium with the rock should cause the dissolution of the rock, in order to achieve the previous
equilibrium. Dissolution causes a decrease in the mass of the rock associated with an increase in
permeability and porosity while precipitation cause an increase in the mass of the rock associated with
decrease in permeability and porosity (Grigg et al, 2005).
SPE-Not Apply-MS 3

In sandstone reservoirs, EOR effects by low-salinity water flooding have been well-documented both
in the laboratory and by field tests. Even though it is in general agreement that the increased oil recovery
by low-saline water flooding is related to wettability modification toward a more water-wet system, the
detailed mechanism is still under debate. Recent studies have indicated that organic material adsorbed
onto clay minerals is desorbed because an increase in pH as active ions, especially Ca2+ , is desorbed from
the clay as the low-saline water invades the porous medium.

In carbonates, the main process involves the dissolution of carbonates and possibly silicates, depending
on the kinetics of individual chemical components. Changes in the solid matrix can alter the pore structure,
inducing changes in fluid flow properties across the porous media affecting ultimately oil recovery from
the reservoir. In accordance with Grigg et al. (2013), carbonate dissolution caused changes in core
permeability and porosity. So, the possible reduction of porosity and permeability in the regions near the
production well will decrease oil production and affect field development.

The dissolution of carbonate rocks was studied by many authors using different approaches. A rotating
disk apparatus was used to investigate the dissolution rate of carbonate rocks (Fredd and Floger, 1998;
Liu et al, 2005; Taylor et al, 2006). Percolation experiments (core flooding experiments), on the other
hand, were used to better mimic the natural reservoir conditions and evaluate changes in rock flow
properties (permeability, porosity and others) (Bacci et al, 2010; Grigg et al, 2005; Izgec et al, 2005;
Luquot and Gouze, 2009; Noiriel et al, 2009; Zekri et al, 2009).

Fred and Floger (1998) studied the dissolution rate of calcite in various pHs using a rotating disk. The
reactants used in the experiments were white Italian marble and HC1. The authors demonstrated that the
rate of calcite dissolution in acetic acid solution is influenced by the rate of transport of reactants to the
surface, the kinetics of the surface reaction, and the rate of transport of products away from the surface.
Liu et al (2005) used a rotating disk apparatus to investigate the dissolution rate of dolomite and limestone
samples. They found that the dissolution rate of dolomite was far lower than that of limestone, and also
that dolomite dissolution is mainly homogeneous and determined by surface reaction. Taylor et al (2006),
also using a rotating, found that the dissolution rate of carbonate reservoir rocks in HC1 acid will generally
increase as the concentration of calcite increases. This trend is varied if significant amounts of clay are
present in the rock. It was also observed that the anhydrite contained in the carbonate disks appears to
have formed, after experiments, fine needles that might cause formation damage in tight carbonate
reservoirs.

The authors of Pu et al. (2008) in their study of Tensleep, Minnelusa sandstone and Phosphoria
dolomite formation concluded that the improved recovery seen during the low salinity flood may be as a
result of increased dissolution of oil wet carbonate and/or sulphate surfaces in the core.
It has been experimentally observed that ion exchange alone is not sufficient to explain Ca concentrations
during rock brine interaction, and carbonate dissolution cannot be neglected (Omekeh et al., 2011).

In carbonate reservoirs, the concentration of Ca2+ in the formation water (FW) is usually high.
Therefore, sulfate is often present as anhydrite, CaSO4 (s), and because of a decrease in the solubility of
anhydrite at high temperatures, the concentration of sulfate dissolved in the FW, SO2−
4 (aq), is usually low.
To discuss the chemical mechanism for the observed low-salinity effect in carbonates, the impact of the
temperature and brine composition on the following equilibrium must be understood:

CaSO4 (s) ↔ Ca2+ (aq) + SO2−

4 (aq)
4 SPE-Not Apply-MS

↔ Ca2+ (ad) + SO2−

4 (ad) ………………… (1)

Ca2+ (aq) and SO2− 2+ 2−

4 (aq) are ions dissolved in the pore water, and Ca and SO4 (ad) are ions adsorbed
onto the carbonate surface. Dissolution of anhydrite, CaSO4 (s), which is the source for SO2− 4 (ad), is
dependent upon the salinity/composition of the brine and the temperature in the following way,
(1) The solubility increases as the concentration of Ca2+ in the FW decreases (common ion effect).
(2) The solubility decreases as the concentration of NaCl decreases.
(3) The solubility normally decreases as the temperature increases.
(4) The concentration of SO2− 4 (aq) may also decrease as the temperature is increased because of the
increased adsorption onto the carbonate surface; i.e., the concentration of SO2−
4 (ad) increases.

Wettability
Carbonate dissolution is one of the mechanisms suggested by many authors that attributed the
wettability changes in carbonates reservoirs. They have concluded the contribution of softening injected
brine in dissolution part and of modified ions in changing surface charge for wettability alteration
mechanism in carbonate rocks (Zahid et al., 2012; Mohanty and Chandraekar, 2013). In general, CB
reservoirs have bothmixed-wet and oil-wet conditions. Several techniques have been proposed to enhance
the recovery of these reservoirs. One of these techniques is wettability alteration toward water-wet by
adjusting the salinity and ionic composition, which will lead to RF (Recovery factor) enhancement.
Wettability alteration has been described as the interaction between potential determining ions; such as
Mg 2+ , Ca2+ , and SO2−
4 and organic materials adsorbed in the rock surface (Strand et al., 2006; Zhang et
al., 2007).

Wettability alteration is one of the key parameters in the distribution of fluids in porous media, which
depends on the composition of the oil, the aqueous phase, and the type of rock. Accordingly, for better
understanding of the LSW injection process, another goal of upcoming studies is to investigate the effect
of salinity on wettability alteration and its effect on the oil RF. Berg et al. (2010) showed that wettability
alteration could be achieved by LSW. Nasralla et al. (2013) reported that LSW injection can alter the
system wettability; however, they did not mention it as a main mechanism affecting the process. Fathi et
al. (2011) showed that modified seawater has the ability to alter the wettability of CB systems in the water-
based EOR process. By studying the effect of LSW injection on the CB samples, Al-Harrasi et al. (2012)
reported oil recovery enhancement of 3% – 5% in waterflooding tests and considered this issue in
association with wettability alteration.

The chemical induced wettability alteration process is sensitive to temperature, and the efficiency
increases with increasing temperature. The surface reactivity of SO2− 4 and Ca
2+
at the carbonate surface
also increases as the temperature increases, and desorption of carboxylic material becomes more efficient.
Regarding oil recovery, it has also been shown that a decrease in temperature can be compensated for by
an increase in the SO2−4 concentration of the imbibing fluid. Provided that reasonable amounts of Ca
2+

and/or Mg 2+ are present, both the concentration of NaCl and SO2− 4 (aq) in the injected brine will have
significant effects on the wettability alteration process at a given temperature. If SO2−
4 is not present in the
injection fluid, dissolution of anhydrite, CaSO4 (s), can act as an in situ source of SO4 , if present in the
formation.

One of the methods for measuring the wettability alteration in core samples is the Amott–Harvey
method (Amott, 1959). In general, testing consists of spontaneous and forced displacement. By measuring
the volume of oil displaced by brine and the volume of water displaced by oil by a spontaneous and force
displacement process, the wetting index of oil and water is calculated.
SPE-Not Apply-MS 5

pH
A new chemical understanding of the increased oil recovery process has recently been published, which
involves desorption of active cations from the clay surface promoting an increase in pH at the clay−water
interface. A local increase in pH desorbs basic and/or acidic polar organic crude oil components from the
clay surface by an ordinary acid−base reaction. A sensitivity study of the pH indicated that, at the
mineral/brine interface, the pH may be higher, where a better agreement when the pH of the LS brines
was increased (Hamouda et al., 2014).

The rise in pH during laboratory experiments has shown two concomitant reactions: carbonate
dissolution and cation exchange. The dissolution of carbonate (i.e. calcite and/or dolomite) results in an
excess of OH − and cation exchange occurs between clay minerals and the invading water. The dissolution
reactions are relatively slow and dependent on the amount of carbonate material present in the rock

CaCO3 ↔ Ca2+ + CO2−

3 ………………… (2)

CO2− −
3 + H2 O ↔ HCO3 + OH
−
………………… (3)

However, cation exchange occurring on the clay minerals, and to a much lesser extent quartz, is faster.
The mineral surface will exchange H + present in the liquid phase with cations previously adsorbed. This
will lead to a decrease in H + concentration inside the liquid phase resulting in a pH increase.

Case Studies
In reservoir characterization, it is important to study and understand key properties in oil production.
A number of mechanisms have been proposed in the literature by researchers evaluating these properties
under various conditions for both sandstone and carbonate reservoirs and varying the method of recovery
applied between carbonated water or low salinity water injection. The scope of this literature review is on
the dynamic of chemical reactions between low salinity water and porous media mainly focusing in
carbonate rock dissolution. To study the interactions between the brine and reservoir rock, two case studies
were analyzed focusing in dissolution.

Case A
Omekeh et al. (2014) presented a one-dimensional mathematical model and also showed how the
dissolution can change the brine composition of the injected brine deep in the reservoir and hence alter
the intended chemistry of the brine-rock interaction. They proposed the following brine composition
(Table 1) used for their example 2 of the four concluded in that study.

FW SW LSW
Ions
[mmol/L] [mmol/L] [mmol/L]
Na+ 1326,22 450,11 13,26
Cl− 1677,73 525,13 16,61
Ca2+ 147,94 12,99 1,48
Mg 2+ 17,46 44,51 0,18
SO2−
4 0,89 24,01 0,01
K+ 5,62 10,06 0,06
HCO−3 0,00 2,02 0,00
Table 1. Brine compositions used for coreflood experiments FW, SW, and LSW.
6 SPE-Not Apply-MS

The flooding experiment was implement with sequential injection with FW, SW and LSW in
succession using an injection rate of 6,323 [cm/d]. For each of the brines, approximately 10 pore volumes.
Effluent samples were taken out for determination of ionic composition and pH of the water phase.

Comparing the simulation results produced by the model presented in their paper, taking in account
three models: for dissolution and cation exchange, ion-exchange only, and tracer (without interaction
fluid-rock) with the experimental data of injected and effluent, including compositions and pH obtained
from the core flood experiment.

The results are presents in the Figure 1 with the calcium compositions of the floods and shows that in
the first injection stage (FW injection) the effluent calcium concentration from the experiment during the
early stages was higher than the injected concentration. This effect is likely due to dissolution since the
simulated values with dissolution are higher than those without dissolution.

While during the SW stage, the Ca2+ effluent from the experiments is more than the injected. This
difference suggests that there is a net release of Ca2+ ions during sea water injection. The simulations with
dissolution and ion-exchange fit the experimental data best, suggesting that more of the Ca ions are
released from the rock surface are from dissolution than from cation exchange.

The effluent concentration during LSW flood shows that there is some retention of the Ca2+ ions since
the effluent does not get up to the quantity injected after about 10 pore volumes. The simulation data for
this stage suggests that the retention is mostly due to ion exchange but that dissolution can reduce such
retention.

Figure 1. Ca effluent concentrations from experiment and simulations during FW, SW and LSW flooding.

As we have said before, another important parameter in the dissolution analysis is the pH. Comparing
the simulations results for dissolution and cation exchange with the experimental data, the pH results are
shown in Figure 2. For the first stage (FW), the pH rises from about 6 in the injected FW to about 7 in the
effluent FW and the same trend is seen in the simulation data. The SW shows pH within the same range
of the injected SW pH which is also seen in the simulation.

The LSW injection shows a high increase in pH when compared with the pH of the injected LSW.
Despite this increased pH, the LSW did not result in increased recovery. It seems that the pH increase
seen in the experiment can be explained by a combination dissolution of carbonate and ion exchange.
SPE-Not Apply-MS 7

Since according to the results obtained by Larger et al. (2006) prove that despite previous evidence, high
pH is not responsible for the increase in oil recovery due to the injection of low salinity water.

Figure 2. Effluent pH from experiment and simulation.

Case B
Another of the representative studies in carbonates was carried out by Austad et al. (2015) which
objective was discussing a chemical mechanism for low salinity EOR effects in carbonates, by using
preserved core material containing dissolvable anhydrite (CaSO4) with a special focus on the relationship
between the concentration of SO42- and NaCl present in the low saline brine.

With the purpose of achieving with the study objectives, they prepared synthetic samples as described
below and summarized in Table 2. and used preserved reservoir limestone cores from a formation in the
Middle East.

‘FW0S is sulfate-free formation water with high salinity, 213000 ppm, containing high concentrations of
Ca2+ and Mg2+. By dilution of this brine 100 times, the salinity of d100FW0S is reduced to 2130 ppm. GSW
is Persian/Arabic Gulf seawater with a total salinity of 57760 ppm. GSW was diluted 10 giving the brines
termed d10GSW with salinities of 5776 ppm’.

FW0S d100FW0S GSW d10GSW

Ions
[mM] [mM] [mM] [mM]
𝑁𝑎 + 2577,1 25,8 797,5 79,8
𝐶𝑎2+ 475,0 4,7 16 1,6
𝑀𝑔2+ 100,0 1,0 86,0 8,6
𝐶𝑙 − 3721,1 37,2 909,5 91
𝑆𝑂42− 0 0 45,0 4,5
𝐻𝐶𝑂3− 6,0 0,1 2,0 0,2
TDS [g/L] 213,0 2,13 57,76 5,78

Table 2. Brine Compositions.

For our case of interest one of the tests made by the authors, was made for a core of 28% porosity and 51
[mD] permeability, at temperature conditions of 100°C during the injection of water of formation FW0S
8 SPE-Not Apply-MS

and d100FW0S with constant injection rate at 0,01ml/min, comparing the low salinity effect by injecting
formation water (Figure 3). This process is interesting since it compares the same type of fluid in
conditions of high (FW0S) and low salinity (d100FW0S-diluted)

Figure 1. Concentration of Ca2+ and SO42− in the effluent vs PV injected.

The dissolution of anhydrite increased from 2.8 mM in FW0S to 5.3 mM in d100FW0S, nearly by a
factor of 2. The difference in the concentrations of SO42- in FW0S and d100FW0S is of great interest,
because SO42- acts as a catalyst for the wettability alteration process and the increased concentration has
an effect on the oil recovery in a forced displacement process. Thus, by decreasing the salinity, with a 100
times decrease in the concentration of NaCl, more oil is recovered due to improved wettability alteration.
The concentration of SO42- increased due to increased solubility of anhydrite.

The Ca concentration was higher in the effluent d100FW0S, this means that d100FW0S was not in
equilibrium with the rock and it can be due to dissolution of calcite. Because in the begging the injection
water had 4,7 mM calcium concentration and increased by more than 10 mM. Then, the reduction of the
Ca (after 2 pore volume injected) the concentration was relased from the rock by ion-exchange and/or
dissolution.

Another of the brines used by the authors is the GSW (Gulf seawater), and they evaluate the low salinity
effect by injecting diluted seawater explaining that seawater itself is a smart wettability modifying brine
containing all of the active ions needed to improve the water wetness. Provided that dissolvable anhydrite
is available in the pore space, diluted seawater can act as an improved wettability modifier. They observe
the low salinity effect in relation to the concentration of SO42− and NaCl in the effluent and the results are
shown in the Figure 4.

Getting that, the dissolution of anhydrite in d10GSW is evidenced by the change of the initial
concentrations of Ca2+ and SO42− from 1.6 and 4.5 mM, respectively, increased to ∼10 mM the
concentrations of both ions in the effluent. It was suggested that the access of the active ions Ca2+, Mg2+,
and SO42− toward the calcite surface was improved if the ionic double layer close to the surface was
depleted in inactive ions such as Na+ and Cl−.
SPE-Not Apply-MS 9

Figure 2. Concentration of Ca2+ and SO42−in the injected and effluent d10GSW vs PV injected.

Conclusions
The low salinity EOR technique can have a great economical potential in carbonate reservoirs
containing a significant amount of dissolvable anhydrite distributed in the pore space (matrix).

The dissolution of anhydrite increases as the flooding fluid is switched from a high saline to a low
saline fluid, resulting in increased concentration of the active catalyst, SO42−, in the flooding fluid.
Consequently, having a positive effect on the wettability alteration process.

The chemical equilibrium is disturbed the moment low salinity water is injected; this causes interaction
between brine and rock to compensate for the loss of cations, especially Ca2+. This causes H+ ions to get
closer to compensate for the Ca2+ loss into the low saline water, which creates an increase in the pH close
to the clay surface. Local increase in pH leads to reactions between the adsorbed basic and acidic material.

Carbonates without sulfate initially present in the formation, usually as anhydrite, do not show
improved oil recovery in response to a salinity gradient in the injected fluid, instead, at a higher
concentration of dissolvable anhydrite in the rock material, equilibrium between ions and rock would be
established and the concentration of sulfate in the effluent should be constant.

Nomenclature
CB Carbonate
EOR Enhanced Oil Recovery
FW Formation Water
IOR Improved Oil Recovery
LS Low-salinity
LSW Low-salinity water
MIE Multi-component Ionic Exchange
RF Recovery Factor
SW Sea Water

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