OTC-29732-MS

Recent Updates on Smart Water EOR in Limestone

Skule Strand and Tina Puntervold, University of Stavanger, The National IOR Centre of Norway

Copyright 2019, Offshore Technology Conference

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Abstract
Experimental data confirm that the EOR-effects observed during Smart Water flooding can be explained by
wettability alteration toward more water-wet conditions. Detailed knowledge about the important crude oil
– brine – rock parameters affecting reservoir wetting, fluid flow and wettability alteration in oil reservoirs
is needed when Smart Water EOR potential for reservoirs should be predicted.
Both field observations and laboratory experiments confirm that seawater behaves as a Smart Water
in limestone reservoirs, significantly improving the oil recovery. Laboratory core experiments have been
performed to evaluate the effects of polar components present in crude oil on core wettability during core
restoration. Spontaneous imbibition and viscous flooding oil recovery tests have been performed on the
restored cores to evaluate the effect of initial core wettability on ultimate oil recoveries. The results have
been compared with oil recovery tests that include wettability alteration induced by Smart Water.
The experimental results confirmed that adsorption of polar components in crude oil dictates the core
wettability established during the core restoration, and strongly water-wet outcrop cores became mixed-
wet. The amount of oil that the core was exposed to affected the degree of water wetness, and therefore the
crude oil amount needs to be accounted for in core restoration procedures.
Oil recovery experiments showed that the ultimate oil recovery increased with increasing water wetness
in the cores, confirming that increased positive capillary forces, resulting from wettability alteration,
significantly affected fluid flow in porous media, improving oil recovery. The results are in line with the
proposed chemical Smart water EOR model valid for both carbonate and sandstone. Wettability alteration
toward more water-wet conditions induces increased capillary forces and improved microscopic sweep
efficiency. Ultimate oil recovery in was significantly influenced by the core wettability, increasing with
water wetness, confirming that capillary forces is an important recovery parameter. Only small changes
in core wetting have significant effects on ultimate recoveries, confirming that laboratory core restoration
procedures need to be optimized when recovery potentials for reservoirs should be estimated.

Introduction
Smart Water injection with optimized ionic composition is a low cost EOR technique with huge EOR
potential in both carbonate and sandstone reservoirs. Compared to traditional, chemical EOR methods,
Smart Water is easily implemented and environmentally friendly.
2 OTC-29732-MS

The Ekofisk reservoir in the North Sea consists of large layers of coccolithic limestone – or chalk. The
reservoir is highly fractured with low matrix permeability. The reservoir wettability was classified as mixed-
wet and close to neutral. The reservoir was put on primary production in 1970. Pressure drawdown and
increasing GOR with low ultimate recoveries forced the operators to change production strategy. Pilot
seawater (SW) injection started in 1985, and full SW injection implementation have since then been a
tremendous success, with expected Sor below 30 %OOIP at production end.
Drainage of oil from porous systems is controlled by gravity, capillary, and viscous forces. In classical
reservoir engineering, Darcy's law describes the mobility of water and oil by relative permeabilities as the
water saturation increases in an imbibition process. Capillary pressure curves account for the contribution of
capillary forces. Both relative permeabilities and capillary forces are wettability dependent, and wettability
needs to be properly understood when laboratory experiments are performed. In porous rocks, wettability
can be determined by spontaneous imbibition (SI) experiments. The capillary forces are dependent on the
fluid distribution of formation water (FW) and crude oil in the porous system.
In order to restore carbonate cores, and to mimic initial reservoir conditions, a detailed understanding
of the crude-oil-brine-rock (COBR) interactions is important (Masalmeh et al. 2004, Masalmeh and Jing
2007). The formation water in carbonate reservoirs usually contains high concentrations of calcium ions,
and the carbonate surface is generally positively charged at pH<9.5 (Pierre et al. 1990, Strand et al. 2006).
Acidic polar organic components (POC) in the crude oil, mostly the negatively charged carboxylates, R-
COO−, have strong affinity to the positively charged calcite surface, and is believed to be the main wetting
parameter in carbonate rocks (Thomas et al. 1993, Standnes and Austad 2000). The acid number (AN), with
the unit mgKOH/g, quantifies the amount of acidic POC in the crude oil by measuring the amount of the
basic compound, KOH, required to neutralise the acidic material present in 1 g of crude oil. Likewise, the
base number (BN) quantifies the amount of basic components in the crude oil. BN also has the unit mgKOH/
g. By increasing the AN in a crude oil, the effect of AN on Stevns Klint (SK) chalk core wettability was
previously studied, and the SI results are given in Fig.1 (Puntervold 2008).

Figure 1—SI experiments performed on SK cores at 90°C using FW as imbibing brine.

The cores were restored with Swi=10% FW, and exposed to 5 PV of model crude oil
with increasing AN; 0.1, 0.5, 0.73, or 1.6 mgKOH/g oil before aging (Puntervold 2008).

The cores were spontaneously imbibed with FW as imbibing brine to avoid any chemically induced
wettability alteration during the experiments. The results confirmed that restored core wettability was
significantly affected by the amount of acidic POC present in the crude oil. The amount of acids controls
both the rate of imbibition and ultimate recoveries, in line with the wettability evaluation by Anderson
(1986, 1987). The adsorption of acidic material present in the crude oil onto chalk is fast during a dynamic
crude oil flooding process at 50 °C (Hopkins et al. 2015), and aging of the core in crude oil is actually not
OTC-29732-MS 3

required to observe a mixed core wettability, but a slightly lower water wetness was observed after aging
(Hopkins et al. 2016b). However, while carboxylic acid is the main parameter responsible for the wetting
in carbonates, the polar organic bases appeared to have only a minor effect (Puntervold et al. 2007b). At
constant AN, and by increasing BN in the crude oil the water wetness slightly increased. It was suggested
that the basic POC interacted with the acidic POC and reduced the adsorption of acids onto calcite surfaces.
SW has been reported to behave as Smart Water, significantly improving oil recoveries from mixed-wet
chalk cores, both in SI and FI processes, exemplified in Fig. 2 (Strand et al. 2008b).

Figure 2—Oil recovery tests performed on SK chalk cores at (left) 110 °C, and (right) 120 °C (Strand et al. 2008b). The
cores were restored with Swi = 10% FW, and exposed to 5 PV crude oil with AN = 1.9 mgKOH/g, and finally aged. The cores
were initially spontaneously imbibed with FW, before viscous flooding of first FW then SW was performed at injection
rates, which varied from 0.06 – 0.10 PV/D at reducing ΔP in the range of 410–70 mbar as water saturation increased.

Very low oil recoveries were observed during SI with FW in both cores, because of the high AN crude
oil, which promoted initial mixed-wet behaviour of the cores. Both cores were then viscously flooded at
a significant pressure drop (410-70 mbar) over the 7 cm cores. The oil recovery steadily increased during
FW injection, with ultimate oil recovery plateaus reaching 27 %OOIP at both tested temperatures. When
the injection brine was changed to SW, a significant increase in the oil recovery was observed, reaching
new ultimate recovery plateaus of 47 %OOIP at both temperatures. These results confirm that SW is a more
efficient injection fluid and that it behaves as a Smart Water in this chalk system.
SW as a Smart Water could be further improved by modifying the salinity and/or the ion composition,
especially Ca2+ and SO42−, which are the ions needed for the wettability alteration process (Strand et al. 2006,
Zhang et al. 2007). Smart Water EOR effects have been reported in chalks, limestone, dolomitic limestones
at temperatures ranging from 65–130 °C (Strand et al. 2008a, Austad et al. 2012, Romanuka et al. 2012,
Austad et al. 2015, Puntervold et al. 2018).
The Smart Water EOR effect cannot be explained by a viscous process controlled by mobility ratio (M),
expressed in Eq. 1.:

Eq. (1)

Where λD is mobility of the displacing phase (water), λd is the mobility of the displaced phase (oil), μw
is the viscosity of water, μo is the viscosity of oil, krw is the relative permeability to water and kro is the
relative permeability to oil, Sor is residual oil saturation and Swi is the initial water saturation. A small and
unfavourable change in the mobility ratio due to brine viscosity (μw) cannot explain the huge EOR response
of 75 % extra oil, as observed in Fig. 2. The EOR response is also not in line with the generally accepted
understanding of highest oil recovery (lowest Sor) observed at slightly water-wet conditions, due to lower
capillary entrapment of oil (Anderson 1987, Jadhunandan and Morrow 1995).
4 OTC-29732-MS

Porous rocks are by definition capillary systems, and a generalized expression describing capillary
pressure (Pc) resulting from interfacial forces in a capillary tube is given in Eq. 2:
Eq. (2)
Where σow is the interfacial tension between oil and water, θ is wettability and r is tube radius. In the
oil recovery experiments presented in Fig. 2, the interfacial tension between oil and brine (σow) should
not significantly change by a small change in salinity from 68 000 ppm for FW to 33 000 ppm for SW.
The average pore radius should also be the same in each individual core. The main parameter that could
affect[SS1] capillary forces is the wettability (θ). Wettability alteration toward more water-wet conditions
could significantly increase capillary forces, and promote increased recovery by SI during oil recovery
experiments.
SI experiments comparing oil recoveries between FW and SW were also performed on SK chalk cores
restored in the same way, Fig 3 (Strand et al. 2008b):

Figure 3—SI tests performed on SK chalk cores at (left) 110 °C, and (right) 120 °C
(Strand et al. 2008b). The cores were restored with Swi = 10% FW, and exposed to 5 PV
crude oil with AN = 1.9 mgKOH/g, and then aged. The imbibing fluids were FW and SW.

The SI results confirmed that SW was able to change the core wettability toward more water-wet
conditions. Both the imbibition rate and ultimate recovery increased with increasing temperature for this
system, and increased capillary forces promoting SI was suggested also as the reason for the EOR effect
observed during SW injection in Fig. 2. A significant increase in the rate of imbibition was observed when
temperature was increased by only 10°C, Fig. 3, thus kinetics involved in the wettability alteration process
is important and need to be accounted for in modelling of the process.
In this paper, very water-wet outcrop chalk – coccolithic limestone - cores were restored to different
initial core wettabilities in the laboratory. Spontaneous imbibition (SI) and viscous flooding (FI) oil recovery
experiments were performed to evaluate the effect of initial wettability on ultimate oil recoveries. The results
were discussed in relation to wettability alteration processes by Smart Water.

Experimental
Core material
Outcrop coccolithic chalk from Stevns Klint (SK) in Denmark was used in this study as a representative
of CaCO3, limestone. The rock consists of 98% pure biogenic CaCO3, and has a relative low degree of
pore heterogeneity (Frykman 2001). SK cores can be used as fair representative for the North Sea chalk
reservoirs (Frykman 2001), and in wettability studies this material has shown reproducible results. The
outcrop material has a specific surface area of around 2 m2/g, a porosity between 40-50%, and permeability
in the range of 1-5 mD (Frykman 2001, Røgen and Fabricius 2002).
OTC-29732-MS 5

The core samples were drilled from the same block in the same direction and prepared according to the
procedure developed by Puntervold et al. (2007a. All cores used were first flooded with 5 pore volumes
(PV) of de-ionized water (DI) to remove easily dissolvable salts, especially sulphates, which can potentially
influence the initial wetting (Puntervold et al. 2007a, Shariatpanahi et al. 2011). Afterwards, the cores were
dried to constant weight at 90 °C. The pore volume was calculated based on weight difference between
water saturated and dry core. Core properties are given in Table 1.

Table 1—Properties of the Stevns Klint outcrop cores

Core name P3 P4 P8

Length, cm 6.06 6.23 5.91

Diameter, cm 3.70 3.79 3.75
Bulk Volume, cm3 65.16 70.28 65.05
Dry weight, g 95.10 97.60 89.58
Sat. weight, g 125.15 128.52 117.00
Pore Volume, ml 29.96 30.83 27.33
Porosity % 46 44 42

Brines
The formation water (FW) used in all oil recovery experiments had a chemical composition similar to an
offshore chalk field in the North Sea. The same FW was also used as imbibing fluid in the spontaneous
and forced imbibition experiments. Thus, no wettability alteration or severe calcite dissolution took place
during the experiments. All brine compositions are reported in Table 2.

Table 2—Brine properties and compositions

BrinesIons FW mM SW mM

Na+ 997 450

K+ 5 10
Li+ 0 12
Ca2+ 29 13
Mg 2+ 8 45
Cl− 1066 525
HCO3 −
9 2
SO4 2−
0 24

Ionic strength 1.112 0.657

pH 7.3 7.8
TDS g/l 62.83 33.39

Crude oil
A stabilized crude oil containing similar amounts of acids and bases, that is having similar AN and BN, was
used in the tests. No precipitation of asphaltenes was observed during storage prior to analyses and core
saturation. The crude oil properties are given in Table 3. AN and BN of the crude oil samples were analysed
by potentiometric titration according to methods developed by Fan and Buckley, and which are modified
versions of ASTM 665 and ASTM 2898 (Fan and Buckley 2007).
6 OTC-29732-MS

Table 3—Crude oil properties

Viscosity Density (g/

Crude oil AN (mgKOH/g) BN (mgKOH/g)
(cP) 25°C cm3) 25°C

Oil A 0.34 0.24 3.25 0.808

Adsorption of polar organic material by core flooding

The cores had an initial water saturation of Swi=0.10 established by using the desiccator technique (Springer
et al. 2003). The core was 100% saturated with 10 times diluted FW, d10FW, before vaporization in desiccator
to 10 % water saturation, controlled by weight. At the end the core was equilibrated in a sealed container
for 4 days to establish an even ion distribution.
The core with Swi = 10% was mounted in a Hassler core holder, with a confining and back pressure of
25 and 10 bar, respectively. Core P4 was flooded in one direction at 50 °C with 15 PV of oil A, at a rate of
0.1 ml/min (4 PV/D). Core P3 was first saturated then flooded with 4 PV of oil A; 2 PV in both directions,
meaning that the core had seen a total of 5 PV of oil A. Effluent oil samples were collected and AN analysed.
After oil A flooding, the cores were wrapped in Teflon tape, and placed on marble balls in a sealed aging
cell surrounded by oil A. The Teflon tape was used to avoid unrepresentative adsorption of active polar
components on the outer core surface, which could prevent spontaneous imbibition (Standnes and Austad
2000). The cores were aged at 50 °C for 2 weeks.

Oil recovery by spontaneous imbibition (SI) and forced imbibition (FI)

The restored core was transferred from the aging cell to the Amott imbibition cell and was surrounded
by FW. The SI test was performed at 50 °C, and the cumulative amount of capillary driven oil produced
was monitored by time and until recovery plateau was reached. When oil recovery plateau was reached by
spontaneous imbibition, the core was mounted into a Hassler core holder with confining and back pressure
of 25 and 10 bar. FW was injected into the core in a forced imbibition process at 50 °C, until recovery
plateau was reached. The injection rate was 1 PV/D.

Results and discussion

Several publications have highlighted the presence of POC in crude oil as a main wetting parameter for
controlling reservoir wettability both in sandstone and carbonate reservoirs (Standnes and Austad 2000,
Puntervold et al. 2007b, Hopkins et al. 2016a, Mamonov et al. 2019)
The results in Fig.1 confirm the importance of acidic POC regarding core wetting in coccolithic limestone
- chalk, and the same effect has previously also been confirmed using different types of reservoir crude oils
(Standnes and Austad 2000). Keeping all core restoration procedures the same, including the volumes of
crude oil exposure, the established core wettability is controlled by the amount of acidic POC present in the
crude oil. SI experiments confirmed reduced water wetness with increased AN of the crude oil (Standnes
and Austad 2000).
To verify the importance of crude oil exposure to the established core wettability, two SK chalk cores
were exposed to different amounts of crude oil during the core restoration process. Core P4 was flooded
with 15 PV of oil A and core P3 was flooded with only 5 PV. Produced effluent oil samples were collected,
and AN was analysed and is plotted in Fig. 4.
OTC-29732-MS 7

Figure 4—AN in effluent oil samples during crude oil flooding of core P4 and P3 at 50°C. Both
cores was restored with Swi=10% FW. (left) Core P4 was flooded with 15 PV of oil A in one direction.
(right) Core P3 was flooded with 2.5 PV of oil A in both directions. Flooding rate was 4 PV/D.

The horizontal line at AN = 0.34 mgKOH/g oil indicates the amount of acidic POC in the influent oil
A. As seen in Fig. 4, the first effluent samples were completely depleted in acidic POC, meaning that the
acids had been retained inside the core. With an increasing amount of injected oil, the effluent AN gradually
increased. Negatively charged carboxylates (R-COO−) adsorbed onto the easily available adsorption sites
at the positively charged chalk surface. By time, the sites filled up, and the adsorption gradually reduced
until the equilibrium between adsorbed carboxylates on the surface and in the free oil phase was reached at
8-9 PV injected, Fig. 4 (left). In Fig. 4 (right) it can be seen that the adsorption equilibrium had not been
reached in core P3 after only flooding a total of 5 PV oil A. To secure a more even distribution of polar
components, 2.5 PV of oil A was injected in each direction, meaning that after 2.5 PV injected, the flooding
direction was reversed.
Having completed the crude oil flooding, both P4 and P3 cores were aged for 14 days at 50 °C, and the
established initial wettability in the cores were evaluated by SI tests at 50 °C using FW as imbibing brine.
The experimental results are presented in Fig. 5.

Figure 5—SI experiments performed on core P4 and P3 at 50 °C. The cores were both restored with Swi = 10% FW, but core
P4 (left) was exposed to 15 PV of oil A, while core P3 (left) was exposed to only 5 PV of oil A. FW was used as imbibing fluid.

In core P4, exposed to 15 PV of oil A, FW steadily imbibed, resulting in a recovery plateau of 13 %OOIP
after 9 days. The shape of the spontaneous imbibition curve and the level of ultimate recovery reveal the
core wettability (Ma et al. 1999), and they both indicated that core P4 behaved slightly water-wet. Core P3
which had only seen 5 PV of oil A, behaved significantly more water-wet, reaching its recovery plateau
of 26 %OOIP after 7 days. This effect on wettability of crude oil exposure was observed previously, and a
similar conclusion was drawn; a chalk core became less water-wet in a second core restoration due to the
fact that it had seen twice the amount of oil (Hopkins et al. 2016b).
8 OTC-29732-MS

A SI experiment was performed on a virgin outcrop SK core, P8, which had not been exposed to any
crude oil containing POC. The core with Swi=10%, was saturated with heptane and spontaneously imbibed
at 23 °C with FW as imbibing brine, Fig. 6. Ultimate recovery plateau of 75 %OOIP was reached after only
30 minutes, confirming very strong positive capillary forces, and very water-wet core behaviour.

Figure 6—Oil recovery by SI at 23 °C in a virgin outcrop SK core P8. The core was restored with
Swi= 10 % FW and saturated with heptane. The imbibing brine was FW (Hopkins et al. 2016b).

The experimental results confirmed that acidic POC in crude oil is a key wetting parameter for chalk, a
coccolithic limestone. Both the amount of acidic POC present in the crude oil (Standnes and Austad 2000),
and the volumes of crude oil the core is exposed to during core restoration will influence the wettability of
the restored core. This should be borne in mind when preserved reservoir cores are restored prior to SCAL
analyses in laboratories, especially when wettability dependent analyses are performed, like oil recovery
tests, or when relative permeability and capillary pressure curves are measured. It should be pointed out
that most reservoirs are charged with less than 1 PV (1-Swi) reservoir fluid during the accumulation. The
amount of POC present in the crude oil during reservoir filling, and the ability of the reservoir fluid to wet
reservoir mineral surfaces is unknown.
After the SI experiments on core P3 and P4, both cores were exposed to viscous flooding/forced
imbibition (FI) using FW as injection brine. The injection rate was 1 PV/D. When viscous forces were
applied, increased oil recovery was observed, Fig. 7.

Figure 7—Oil recovery tests by FI at 50 °C were performed on the previous SI cores P4 and P3. The
FW injection rate was 1PV/D. (left) the slightly water wet core, and (right) the more water wet core.

For the slightly water-wet core P4, the oil recovery increased from 13 %OOIP after SI, to a new ultimate
recovery plateau of 28 %OOIP during FW flooding. But, for the more water-wet core P3, significantly
OTC-29732-MS 9

higher ultimate recovery plateaus were reached: 26 %OOIP after SI, and 48 %OOIP after FW injection,
corresponding to an extra 71% oil produced compared to that from the slightly water-wet core P4. This
increased recovery happened even though the average water saturation in the core after SI was significantly
higher when the FW injection started in P3.
By using both spontaneous and forced imbibition data, the Amott water index, Iw, can be calculated
according to Eq. (3) (Amott 1959):

(3)

Where δSWS signifies increase in water saturation after spontaneous imbibition of water, and δSWF
signifies increase in water saturation after forced imbibition of water.
The Amott water index incorporates the change in water saturation from spontaneous imbibition to the
total change in water saturation from both spontaneous and forced imbibition, hence it reflects the relative
importance of capillary forces in the oil recovery process. The scale goes from 0 to 1, where 0 is equal to
an oil-wet system, where no spontaneous imbibition of water takes place, and 1 is equal to a very water-
wet system where all oil is recovered by spontaneous imbibition. The Amott indices and the experimental
results from all three cores are summarized in Tbl. 4.

Table 4—Summary of oil recovery results and Amott water indices

Core P4 P3 P8

Oil A injected, PV 15 5 0
SI recovery, %, OOIP 13 26 75
FI recovery 1PV/D, %OOIP 28 48 -
FI – SI, %OOIP 15 22 -
Iw 0.31 0.35 -

The significantly increased oil recovery from the more water-wet core P3 could be explained by positive
capillary forces contributing to the mobilization of oil from smaller pores, increasing the microscopic
displacement efficiency. During FW injection, no change in physical properties of the brine phase takes
place, and FW will not induce any chemical wettability alteration during oil recovery. The oil recovery
results are in line with the Smart Water EOR observation in Fig. 2. The extra mobilized oil is a result
of increased water wetness by Smart Water flooding, promoting increased positive capillary forces, and
increased microscopic sweep efficiency. However, these experimental results are also contradicting the
general acceptance of the highest oil recovery (lowest Sor) observed at slightly water-wet conditions due to
lower capillary entrapment of oil (Anderson 1987, Jadhunandan and Morrow 1995).

Conclusions
By performing spontaneous and forced imbibition tests, the core wettabilities of two cores exposed to
unequal amounts of crude oil, 5 and 15 PV, were evaluated. Based on the results from this study the following
conclusions were drawn:
1. The amount of crude oil flooded through the core during core restoration affected the initial core
wettability. Increased volumes of oil reduced the water wetness of initially very water-wet cores.
2. Spontaneous imbibition showed that the core exposed to 15 PV of crude oil behaved slightly water-
wet. The core exposed to 5 PV crude oil behaved significantly more water-wet, confirmed by both
imbibition rates and ultimate recoveries
3. The increase in oil recovery by forced imbibition was significantly higher for the more water-wet core.
10 OTC-29732-MS

Acknowledgements
The authors acknowledge Paul A. Hopkins for the experimental work performed.
The authors also acknowledge the Research Council of Norway and the industry partners, ConocoPhillips
Skandinavia AS, Aker BP ASA, Vår Energi AS, Equinor ASA, Neptune Energy Norge AS, Lundin Norway
AS, Halliburton AS, Schlumberger Norge AS, Wintershall Norge AS, and DEA Norge AS, of The National
IOR Centre of Norway for support.

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