IPTC 17656

Dilute Surfactant Flooding Studies in a Low-Permeability Oil-Wet Middle

East Carbonate
Martin V. Bennetzen, Kristian Mogensen, Søren Frank, Maersk Oil Research and Technology Centre; Kishore

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Mohanty, University of Texas at Austin

Copyright 2014, International Petroleum Technology Conference

This paper was prepared for presentation at the International Petroleum Technology Conference held in Doha, Qatar, 20–22 January 2014.

This paper was selected for presentation by an IPTC Programme Committee following review of information contained in an abstract submitted by the author(s). Contents of the paper, as
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Abstract
The majority of alkali-surfactant-polymer (ASP) applications to date have targeted medium-to-high permeability sandstone
reservoirs containing reservoir brine with moderate salinity and hardness. Surfactant flooding experiments have been reported
in carbonates, but applications targeting oil-wet, low-permeability limestone rock are still uncommon.

This paper contains results from laboratory core flood tests performed on an oil-wet limestone rock from the Al Shaheen field,
offshore Qatar. The rock samples investigated had approximately 30% porosity and 5 mD permeability, whereas the reservoir
brine had a salinity of about 120,000 ppm of which about 10,000 ppm were divalent cations.

The first screening step involved testing combinations of several commercial surfactants, co-surfactant and alkalis. Two cost-
effective surfactant systems were identified. The first system, denoted ITR, was capable of reducing the interfacial tension
below 0.001 mN/m over the required range of salinities. The second system, referred to as WA, effectively altered the
wettability from strongly oil-wet to intermediate-wet. Static adsorption was measured to be low for both systems. No polymer
was used because the permeability was very low. Both surfactant systems yielded significant incremental oil, when injected in
tertiary as well as in secondary mode. The ITR system recovered almost 95% of OIIP but required many pore volumes since
the cores remained oil-wet. The WA system, on the other hand, recovered some 85% of OIIP in secondary mode but achieved
this with much fewer pore volumes.

The WA system was subjected to extensive analysis. Relative permeability curves from unsteady-state core flooding data were
derived and experiments were simulated with UTCHEM.

The main conclusion from the extensive laboratory work is that surfactant systems can be tailored to recover a significant
amount of oil from a low-permeability carbonate reservoir. Wettability alteration may assist in unlocking significant volumes
of additional oil from this complex, offshore field.

Introduction
Surfactant flooding and its variations (surfactant-polymer flooding (Bragg et al. 1982), low tension polymer flooding
(Kalpakci et al. 1990), and alkaline-surfactant-polymer flooding (Krumrine et al. 1982, Falls et al. 1992)) were developed
more than thirty years back for sandstone reservoirs. They were technical successes, but have been implemented only in a few
fields (e.g. in Daqing field, China) due to low oil prices during 1985-2005. Surfactants can reduce interfacial tension to
ultralow values (about 0.001 dyne/cm), which increases the capillary number and mobilizes residual oil left after waterflood
2 IPTC 17656

(Pope and Nelson 1978). Polymers increase the viscosity of the injected water and increases sweep efficiency. Alkalis reduce
surfactant adsorption and generate soap if the oil is acidic and thus reduce the amount of surfactant needed in the formulation
(Krumrine et al. 1982). Often some alcohol or co-solvent is also used in the surfactant formulation to avoid liquid crystalline
phases. Residual oil saturation in a water-wet sandstone core can be reduced to a few percent by ASP flooding.

Carbonate reservoirs are different from sandstones in many respects. The zeta potential on carbonate minerals is positive
(negative on silica at normal pH), pore structure is more heterogeneous (presence of fractures, vugs and dead-end pores), and
permeability (of the matrix) can be significantly lower. The capillary desaturation curves for carbonate rocks are quite

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different from those of sandstones (Kamath et al. 2001); higher capillary numbers are needed to reduce the residual saturations
to a few percent. Wettability alteration to water-wet or intermediate-wet conditions can be an important mechanism for
reducing the residual oil saturation in carbonates. The oil relative permeability generally increases and water relative
permeability decreases as a rock becomes more water-wet. This mechanism can increase the fractional flow of oil and improve
oil recovery rate.

Wettability of originally oil-wet carbonate rocks can be changed to more water-wet conditions by low salinity brine, certain
ions and surfactants. Yousef et al. (2010 and 2012) have demonstrated improvement of oil recovery up to 18% in carbonate
rocks by using different dilutions of seawater. Gupta et al. (2011) have shown up to 20% OOIP incremental recovery using
seawater with added borate (BO33-) and phosphate (PO43-) ions. Ion exchange and surface dissolutions can release adsorbed
organic carboxylates from the surface of the rock, thus making it more water-wet. These techniques typically need a high
temperature (>80 °C) to be effective.

Surfactants can be used to change the wettability at low as well as high temperatures. Austad and coworkers have conducted a
series of studies on imbibition from oil-wet chalk cores by use of surfactant solutions (Austad and Milter 1997, Standnes and
Austad 2003). They have shown that cationic surfactants, such as dodecyl trimethyl ammonium bromide (DTAB), are quite
effective (recovery ~70% OOIP) in imbibing water into originally oil-wet cores at concentrations higher than their CMC (~1
wt%). The imbibition mechanism is proposed as

(i) formation of ion-pairs by interaction between surfactant monomers and adsorbed organic carboxylates from
crude oil
(ii) water-wetness of the solid surface due to dissolution of ion-pairs in the oil phase and micelles. The imbibition
rate increases with temperature and decreases with connate water saturation. The interfacial tension between the
surfactant solution and oil remained high (> 0.1 mN/m).

Anionic (Seethepalli et al. 2004; Adibhatla and Mohanty 2008; Hirasaki and Zhang, 2004) and non-ionic (Xie et al. 2004; Wu
et al. 2006) surfactants have also been identified which alter wettability of originally oil-wet carbonate rocks by micellar
solubilization of adsorbed hydrophobic components. More than 60% of the original oil can be recovered from initially oil-wet
cores by dilute (0.05 wt%) alkaline surfactant imbibition at room temperature (Seethepalli et al. 2004). The anionic surfactant
imbibition process has been modeled and the simulator results match the experimental results at the laboratory-scale
(Adibhatla and Mohanty 2008). The simulations show that increase in water-wetness increases oil relative permeability, which
enhances the rate of oil drainage by gravity. Anionic surfactants imbibe from the sides (and the bottom) and oil is recovered
from the top in imbibition experiments. Gupta and Mohanty (2010) have studied the effect of temperature on wettability
alteration with anionic and non-ionic surfactants at low brine salinity and hardness. Sharma and Mohanty (2011) have studied
wettability alteration with surfactant formulations for carbonate reservoirs at higher temperatures (>90 °C) and higher salinity
(>50,000 ppm with hardness).

Surfactant flooding is currently not an established enhanced oil recovery technique for low-permeability carbonate reservoirs.
Potential loss of surfactant due to adsorption on to the calcite surface can lead to inefficient oil recovery and a high chemical
consumption. The present study has been conducted with the aim to develop cost-effective surfactant flooding strategies for
the Kharaib B formation of the Al Shaheen field offshore Qatar, which is a low-permeability predominantly oil-wet carbonate
IPTC 17656 3

reservoir. Currently the reservoir is successfully being waterflooded; however, chemical flooding may help unlock further
potential from the field.

This paper describes results from an extensive surfactant study involving phase behavior, interfacial tension, wettability and
reservoir core flooding experiments as well as computational modeling and simulation.

Aqueous Phase Behavior Studies

Phase behavior studies were conducted to identify regions of low interfacial tension that would lead to oil solubilisation and

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presence of a third phase (a Winsor Type III micro-emulsion). Different types of surfactants (Table 1) were studied (0.2-0.5
wt%) and for each surfactant the compatibility with the reservoir and sea brine was investigated. The brines were prepared
according to Table 2. Moreover, compatibility of sea and reservoir brine with various alkalis (sodium bicarbonate, sodium
hydroxide and sodium metaborate) and the dependency of brine concentration and pH were investigated.

Adsorption by anionic surfactants to the positively charged carbonate surface can be significantly reduced if the pH of the
injected brine solution is increased above the point of zero charge, which is around 8.3 for calcite (Zhang et al. 2006), by
addition of alkali to the brine; hence various alkalis were tested for brine compatibility. Both sea brine and reservoir brine gave
rise to precipitation with 0.125 wt% sodium carbonate. Potassium hydroxide was also expected to give precipitate as well, but
was not tested. 0.5 wt% of sodium metaborate was used in the subsequent experiments.

The results for brine-alkali-surfactant phase behavior are summarized in Table 1 that indicates that alkyl ether sulfate
(‘Surfactant A’ or ‘B-110’), alkyl propoxy sulfate (‘Surfactant B’ or ‘AL’), alkyl propoxy ethoxy sulfate (‘Surfactant C’ or
‘3PO-4EO’), alkyl ethoxy sulfonates (‘Surfactant D’ or ‘S150’), and secondary alcohol ethoxylate (‘Surfactant E’ or ’15-S’)
showed compatibility with the injection brine.

The ability of the brine-compatible surfactants to form micro-emulsions when mixed with oil was subsequently investigated. A
total surfactant concentration of 0.2 wt% was required to safely exceed the critical micelle concentration (CMC), which is to a
large extent dictated by water salinity and temperature (Noll, 1991). Results showed that surfactant combination A/C (0.11
wt% B110 + 0.09 wt% 3PO4EO + 2% iso-butanol + 0.5% sodium metaborate) and B/D (0.125 wt% AL + 0.075 wt% S150 +
1% iso-butanol + 0.5% sodium metaborate) led to significant micro-emulsion formation when mixed with oil – see Figure 1.
The combinations were designed to have an optimal salinity of 36,000 ppm. Surfactant E did not cause micro-emulsion
formation.

At reservoir temperature (52 °C), the surfactant formulations also formed macro-emulsions when contacting the crude oil.
Since such viscous macro-emulsions generally cause high pressure drops during core floods, they were suppressed by addition
of iso-butanol (1-2 wt%). Salinity scans (34,000 to 45,000 ppm) were subsequently conducted for the A/C(1:1)-surfactant
formulation along with 0.5 wt% sodium metaborate and 1-2% iso-butanol. The optimum salinity was found to be approx.
36,000 ppm. The phase behaviour shifted from Winsor Type II- (oil-in-water emulsion) to Type III to Type II+ (water-in-oil
emulsion) as salinity increased. Figure 1B shows the phase behaviour results of the A/C- combination at 36,000 ppm with
1.5% iso-butanol. The total surfactant concentration was kept constant at 0.2 wt%. A desirable low-viscosity third phase with
no macro-emulsion was observed (a Type III micro emulsion), indicating ultra-low interfacial tension. Figure 1C shows the
corresponding interfacial tension values for both 1.5 wt% and 2 wt% alcohol systems. Similar phase behavior was observed
for the surfactant B/D combination. Figure 1D shows the interfacial tension for the B/D surfactant combination at different
concentration ratios. Similar to the A/C-combination low interfacial tension and high oil solubilisation were observed at
36,000 ppm salinity. Based on these initial experiments the following surfactant combinations were chosen for the core flood
analysis:

 0.09 wt% A + 0.11 wt% C (2 wt% iso-butanol) + 0.5 wt% sodium metaborate
 0.11 wt% B + 0.09 wt% D (1 wt% iso-butanol) + 0.5 wt% sodium metaborate
4 IPTC 17656

Surfactant-Induced Wettability Alteration

Mineral crystals representative of the reservoir were aged with reservoir brine and oil and subsequently treated with brine-
compatible surfactants identified in the previous sections. The contact angle was measured and spontaneous imbibition
experiments using a reservoir core plug were conducted to verify wettability alteration.

Wettability was evaluated by measuring water-oil contact angles on polished calcite plates using a Kruss goniometer. Polished
plates were aged first in reservoir brine and then in crude oil for 7 days at 90 °C. These plates were immersed in the reservoir
brine at a reservoir temperature of 52 °C and the contact angle was measured. Hereafter the plates were immersed in surfactant

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solutions (solutions of individual surfactants A-D and the two surfactant combinations A/C and B/D) at 52 °C and the change
in contact angle was monitored for 48 hours.

A spontaneous imbibition experiment was conducted on a reservoir core plug to investigate wettability alteration. The oil-wet
core was placed in an imbibition cell at 52 °C containing 0.2 wt% surfactant at 36,000 ppm salinity. The contact angle of an oil
droplet on calcite plates was about 170-180° after aging the calcite plate with reservoir oil (oil gravity of 33 °API). When an
oil-aged calcite plate was immersed in the surfactant solutions A/C and B/D at 36,000 ppm brine salinity, small amounts of oil
were mobilised and rose to the top of the plate. Figure 2A shows oil drops on an oil-aged calcite plate in the presence of B/D
surfactant formulation in 36,000 ppm salinity brine. The contact angle was approximately 144°, indicating oil-wet conditions
in the presence of this surfactant system. Similar wettability behaviour was observed with A/C surfactant formulation and the
individual surfactant components A-D.

Figure 2B shows oil drops on an oil-aged calcite plate in the presence of 0.2 wt% surfactant E in 36,000 ppm salinity brine. No
alcohol or sodium metaborate was used in this formulation. The contact angle was about 65-85° indicating that surfactant E
can change wettability to intermediate to water-wet conditions. A subsequent imbibition experiment validated the wettability-
altering potential of surfactant E. About 20% of oil-initially-in-place (OOIP) was recovered from the imbibition experiment in
7 days. Expulsion of oil during spontaneous imbibition is shown in Figure 2C. The interfacial tension of the oil-surfactant-
water system was about 5 mN/m.

Coreflood Experiments and UTCHEM Simulations

Tertiary Flooding with ITR Surfactant

The cores used in the experiments were evacuated using a vacuum pump for 2 days and then saturated with reservoir brine.
Dead oil was injected until no more brine was produced. Initial oil saturations were 0.88-0.89. The cores were then placed in
an oven and aged for 45 days at 90 °C. Hereafter they were flooded with synthetic sea brine to residual oil saturation. Tertiary
surfactant floods for the surfactant combinations A/C and B/D were initiated after water flooding at a flow rate of 8 ml/h.
Changes in pressure drop during the tertiary surfactant flood were monitored (Figure 3) and the salinity of the effluent was
measured using a conductivity meter (Figure 4).

Combinations of A/C (0.11 wt% B110 + 0.09 wt% 3PO4EO +2 wt% iso-butanol) and B/D (0.125 wt% AL + 0.075 wt% S150
+ 1 wt% butanol) were subjected to core flood experiments after analyzing the phase behavior data. In both cases, 0.5 wt%
sodium metaborate was added. Two secondary waterfloods were performed to establish residual oil saturation. Continuous
injection of the surfactant formulation A/C and B/D, respectively, were then carried out in tertiary mode with a negative
salinity gradient.

The results of two tertiary surfactant core floods (referred to as ‘Core flood 1’ and ‘Core flood 2’ in two different cores are
given in Table 3 and Figure 3. The cores were oil-wet and consequently water did not spontaneously imbibe into the core.

In Core flood 1, sea brine was injected for 4.6 PV and the remaining oil saturation was 0.28. In Core flood 2, the sea brine
throughput was 16 PV and remaining oil saturation reduced to 0.194. Sea brine was injected in both floods at 8 ml/h for
several PV until no more oil was recovered. This suggests that the capillary number was too low to mobilize any oil. For Core
IPTC 17656 5

flood 1, 4.6 PV injected sea brine led to a recovery of 67.5 % OOIP, see Figure 3, while 16 PV led to a recovery of 79.6 %
OOIP for Core flood 2. The total recovery after each surfactant flood was approx. 95%. Despite the excellent oil recovery,
many pore volumes were required to reach this value, which is typical of oil-wet reservoirs.

The flow rates during the surfactant floods were 8 ml/h. Similar corefloods were conducted at lower flow rates (2 and 4 ml/h;
data not shown) with very little tertiary oil recovery; rather than a gradual lowering of residual oil saturation with increasing
capillary number, there appeared to be a critical displacement rate of 8 ml/min required to mobilize the residual oil. This is to
our knowledge an unusual observation.

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The pressure drop during the tertiary surfactant flood of core flood 1 is shown in Figure 3. The pressure increased considerably
to about 52 psi as oil was mobilized and then decreased to about 17 psi as oil was displaced from the core. The initial pressure
drop suggests that the implementation of a tertiary surfactant flood in the field might be difficult in low permeable carbonate
rock unless the rate is reduced.

To improve the surfactant flood design and in particular to reduce the injection volumes required a low molecular weight
polymer (SNF FLOPAAM 3230S) was tested to provide mobility control but was unfortunately found to cause plugging of the
pore throats. Use of foam as mobility controlling agent was also tested; surfactant combination A/C (1:3) was used to generate
foam by mixing it with air. The generated foam was able to penetrate the rock but gave rise to large pressure drops.

The simulator UTCHEM was used to simulate the two water floods, termed WF1 and WF2 as well as the tertiary flood for the
A/C surfactant combination. The interfacial tension was modelled as a function of surfactant concentration in this model.
Capillary numbers which affect the relative permeability of the fluid phases were calculated using UTCHEM. Porosity,
permeability, and water saturation before the tertiary surfactant flood were assumed to be uniform throughout the core.
Resident brine salinity prior to surfactant flood was modelled as 41,840 ppm NaCl. The injected brine salinity for the
surfactant flood was modelled as 34,033 ppm NaCl. The optimal salinity was modelled as 36,792 ppm NaCl. The
solubilisation ratio corresponded to an interfacial tension of 10-3 mN/m. The relative permeability parameters at the low
capillary number end were obtained by matching the water flood data using the JBN method (Johnson et al. 1959). The end
point relative permeability and exponents (of oil, water and emulsion phases) were assumed to be 1. The roles of alcohol and
sodium metaborate are implicitly included. Brine viscosity was 0.6 cP and oil viscosity 4 cP at 52 °C. The Corey function
parameters are shown in Figure 5.

All other data for the simulation is included in Table 3. The salinity gradient design for the simulation was the same as for the
laboratory experiment. The simulated data for the two core floods were similar and the match between the experimental and
simulated data was very good, see Figure 6.

UTCHEM was also used to simulate the tertiary surfactant flood for Core flood 1. The phase behavior of the surfactant,
wettability of the rock and relative permeability were incorporated into the UTCHEM simulator. The residual oil saturation
after water flood 1 was about 0.284. In Figure 7A the simulated and measured cumulative oil recovery after injection of
surfactant solution for core flood 1 are shown. As observed, oil is recovered by the surfactant flood at a low rate with first oil
arriving at the outlet after 2 PV. Effluent salinity and surfactant concentration profiles are shown in Figure 7B. While the
injected salinity breakthrough occurs at 1 PV, the surfactant breakthrough occurs after 2 PV. The slow mobilization of oil and
the out-of-phase correlation with salinity can be explained by the nature of the oil-wet rock, surfactant adsorption and
retention, lack of mobility control and maybe trapping of the surfactant in the micro emulsion phase. Figure 7C shows that the
high-capillary number propagates slowly into the core during the surfactant flood. Figure 7D shows that the oil saturation is
reduced where the trapping number is high. The trailing end of the oil bank does not propagate as fast as the front of the oil
bank, possibly due to surfactant dispersion.

To summarize, the low recovery rate, the need for large injection volumes and the lack of mobility control excluded the
interfacial tension-reducing surfactants from further analysis. The surfactants A-D gave very good recoveries due to significant
6 IPTC 17656

interfacial tension reduction, but required a large number of pore volumes to reach the low oil saturation.

Secondary Flooding with WA Surfactant

Surfactant E at 0.2 wt% was tested in a secondary core flood experiment. Fluids were evacuated using a vacuum pump for 2
days and the core was then saturated with reservoir brine. Dead oil was injected until no more brine was produced. The core
was aged in an oven for 45 days at 90 °C. Hereafter it was flooded with sea brine to residual oil saturation. The secondary
surfactant flood was conducted at a flow rate of 0.05 ml/min and at a temperature of 52 °C. No alkali, co-surfactant or polymer
was added to the surfactant solution.

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The secondary core flood showed that the ultimate oil recovery increased from 60 to 78% after 3 PV of surfactant and 82.4%
after 4 PV as a result of wettability alteration (Figure 8). The pressure drop was comparable to the pressure drop for water
flooding and there was no need for a mobility-controlling agent. Furthermore, the non-ionic surfactant E was much more
salinity-tolerant than the anionic surfactants A-D.

Tertiary Flood with WA Surfactant

A tertiary surfactant flooding experiment was conducted with surfactant E. To ensure reproducibility, two core plugs (termed
‘core A’ and ‘core B’) were used in this study. The two cores were treated identically and hence the description below will
only focus on core A. Core, oil and brine properties are listed in Table 5 and Table 6. The core was initially saturated with
formation brine followed by flooding with the reservoir oil and aged at 80 °C for 1 month. A short oil flood was done after
aging to estimate the relative oil permeability at initial oil saturation at 52 °C. The core was then flushed by water flood, a
surfactant flood and an additional chase-brine flood. All floods were conducted at the injection rate of 0.05 ml/min. Figure 9
shows the contact angle measurements.

After the chase-brine injection the core was cleaned and re-saturated with oil and subjected to another round of water flood
(called a ‘post-surfactant water flood’) to establish whether relative permeabilities have changed permanently as a result of the
presence of surfactant E. Finally, a high-rate water flood (2 ml/min) was performed after the post-surfactant water flood.

Simulations of the following floods were conducted using the chemical simulator UTCHEM:

 Initial water flood of core A and B before addition of surfactant E

 Water flood of cleaned and subsequently re-aged core A after addition of surfactant (the post-surfactant flood)
 The full surfactant flood design (water floodsurfactant floodchase-brine injection) for core A

Parameters from Table 5 and relative permeability parameters obtained from the JBN method were used for the UTCHEM
simulations. Wettability alteration was modeled using the ‘Tracer option’ in UTCHEM where altered capillary pressure
parameters (endpoint and exponent) were determined from history matching. Relative permeability parameters were used only
to a minor extent as fitting parameters.

A secondary water flood (4.5 PV) and a subsequent tertiary surfactant flood (3 PV) followed by chase brine injection (5.3 PV)
were conducted on core A, see Figure 10. The secondary brine flood breakthrough occurred after approx. 0.3 PV and the oil
recovery after 4.5 PV brine was approx. 35%. The pressure drop decreased steeply at the beginning before breakthrough and
later dropped slowly. After the surfactant solution was injected the oil recovery curve initially continued as an extension of the
water flood curve. After approx. 1.5 PV of surfactant injection the oil recovery rate started to increase. The out-of-phase oil
recovery and surfactant injection profiles can be due to three effects:

i. it may take 1.5 PV for the surfactant to invade the pore space and to cause alteration of rock wettability;
ii. wettability alteration happens fast but the macroscopic mobilization of trapped oil takes place slowly;
iii. a combination of (i) and (ii).
IPTC 17656 7

Oil recovery at the end of the surfactant flood was about 40%. The pressure drop across the core decreased as more oil was
pushed out of the core. After the tertiary surfactant flood chase brine was injected resulting in a final oil recovery of approx.
45%, due to the flow of surfactant still present inside the core and due to permanent wettability alteration. Similar recovery
profiles were obtained for core B.

After the waterflood-surfactant flood-chase brine flood design, the core plug was cleaned and re-aged. Then the sea brine was
injected for about 4 PV during a post-surfactant waterflood. The recovery and pressure profiles for the initial waterflood and
the post-surfactant waterflood are shown in Figure 11. The oil recovery for the initial waterflood is 34.3% whereas the

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recovery was 51% for the post surfactant flood. This significantly higher oil recovery can be ascribed to a more water-wet rock
system when surfactant E has entered the rock. The pressure drop during the post-surfactant flood decreases after the brine
breakthrough and reaches a final value of 10 psi. Final pressure drop is lower than that of the initial water flood indicating
higher water end-point relative permeability. In summary, the comparison shows that the wettability of the rock after the
surfactant flood, and after thorough cleaning, is significantly different from that of the original oil-aged core. It is clear that
care must be taken when cleaning and re-aging core plugs if these have already been subjected to surfactant flooding.
Surfactants might (which is the case here) change the wettability of the rock permanently. Based on the oil recovery and
pressure profiles relative permeabilities were calculated using the JBN method (Figure 12).

After the completion of post-surfactant water flood at a rate of 0.05 ml/min, about 10 PV of injection brine was pumped into
the core plug (at 52 °C) at a very high flow rate (2 ml/min) to assess the capillary end effect on the residual oil saturation of the
core; a reduction in residual oil saturation from 0.39 to 0.33 was observed.

UTCHEM was used to simulate some of the core floods. Parameters for the simulation of the floods for core A and core B are
included in Table 5 and Table 6.
A very good match between the experimental and simulated data for the initial water flood and the post-surfactant water flood
was obtained for core A, see Figure 13; pressure drops and oil recoveries matched very well. A good match was also found for
the water flood for core B, see Figure 14; the pressure profile is matched well, whereas the recovery profile is matched less
well. The reason for the difference between the simulated and experimental recovery data can to some extent be ascribed to the
small number of data points. The very good match for the experimental and simulated pressure profiles indeed suggests that
the UTCHEM model captures the essential physical mechanisms affecting the flood.

A simulation of the whole surfactant flood design (for core flood A) was more complicated because a number of parameters
for the UTCHEM simulation were not available from laboratory data, such as parameters for the Langmuir adsorption
function, the ion exchange function, the viscosity function, and capillary pressure. We speculate that incorporation of a
relevant capillary pressure profile might have led to a better match. Also, Figure 12 shows that the water permeability for the
waterflood exhibits a curvature which cannot be fitted with a Corey power function. However, the curve representing the chase
brine injection is matched well and ultimately the simulated and experimental data converge at the end of the flood. A
simulation was not performed for the surfactant flood design applied to core B.

Secondary and Tertiary Slug Floods with Wettability-Altering Surfactant

To reduce chemical consumption, surfactant E was tested with a 0.5 PV slug in secondary and tertiary flooding modes in two
similar cores. First a conventional water flood recovery with formation brine in an oil-aged core plug (core 1) was conducted.
Hereafter the core was washed, cleaned and re-aged to restore oil saturation and subsequently subjected to a short secondary
surfactant flood. This two-step scheme was conducted to eliminate the effect of variation in core plugs for the assessment of
incremental oil recovery specifically induced by the surfactant. A second core (core 2) was used in another experiment where
the surfactant injection was conducted in tertiary mode after 0.5 PV injection of brine. Core properties are listed in Table 7.
8 IPTC 17656

Core 1
After an initial water flood (4.9 PV) in core 1 was conducted at 52 °C the dead crude oil was again injected into the core to
displace all the mobile water. The secondary surfactant flood consisted of injecting a 0.5 PV surfactant solution followed by
injection brine (3.8 PV) at a rate of 0.05 ml/min.

The pressure drop and oil recovery profiles for the initial water flood and the subsequent secondary surfactant flood are shown
in Figure 16. The breakthrough during the water flood occurred at 0.35 PV and the final oil recovery was 54% OOIP. For the
ultra-short surfactant flood the water breakthrough occurred at around 0.4 PV and the final oil recovery at the end of 4.3 PV

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(0.5 PV surfactant flood + 3.8 PV chase brine) was 69% OOIP. As observed the pressure drop during the secondary surfactant
flood (including the chase brine injection) was similar to that of the water flood indicating similar injectivity. The surfactant
flood (followed by 3.8 PV chase brine injection) recovered 15% OIIP more than the initial water flood which is significant for
such a small surfactant volume. The additional recovery during the chase brine injection after the surfactant flood is about 16%
OOIP after 1 PV, 24% OIIP after 2 PV and 25% after 3.8 PV chase brine. If the chase brine injection had been terminated after
1 PV the additional recovery would be approx. 6% OIIP when compared to the recovery after 4.9 PV of water flooding. This
improvement is significant. Furthermore additional recovery would be 15% OIIP if the brine injection was terminated after 2
PV. To summarize, a 0.5 PV surfactant slug pumped in secondary flooding mode yielded significant oil recovery without the
need for alkali, co-solvents or polymers.

Core 2
A core flood with 0.5 PV of injection brine (IB) followed by 0.5 PV of surfactant slug (SS) followed by 2 PV of injection
brine (IB) was conducted using core 2. The pressure drop and oil recovery profiles are shown in Figure 17. Water
breakthrough during the initial water flood (IB) occurred at around 0.35 PV and the oil recovery after 0.5 PV (corresponding
to the initially injected volume of brine) was approx. 42%. When the surfactant solution was injected the oil recovery
increased to approx. 50% after 0.5 PV surfactant solution (SS). Additional 2 PV injection brine improved the oil recovery to
approx. 60% confirming that the surfactant-induced wettability alteration of the rock has a significant and permanent effect on
post-surfactant water flooding. Thus, this surfactant flooding design of only 3 PV (0.5 PV surfactant solution + 2.5 PV chase
brine) led to a significant incremental oil recovery of about 18% OOIP compared to the initial water flood.

Conclusions
Five different surfactants (four anionic and one non-ionic) from a large pool of commercially available surfactants were
identified as being compatible with injection brine at relevant salinity and hardness and were subjected to thorough analysis.
The surfactants were an alkyl ether sulphate (‘B 110’, surfactant A), an alkyl propoxy sulphate (‘AL 167’, surfactant B), an
alkyl propoxy ethoxy sulphate (‘3PO4EO’, surfactant C), an alkyl ethoxy sulphonate (‘S 150’, surfactant D) and a secondary
alcohol ethoxylate (‘15-S’, surfactant E). The effect of adding alkali was tested and it was shown that sodium metaborate was
compatible with the brine-surfactant system. Sodium metaborate and small amounts of the co-solvent iso-butanol to lower the
emulsion viscosity were used for experiments involving surfactant A-D. Two surfactant systems (A/C and B/D) were tailored
to yield ultra-low oil-water interfacial tensions at an optimum salinity of 36,000 ppm. The contact angle of an oil droplet on
calcite immersed in surfactant solutions consisting of the individual surfactants A-D, A/C and B/D decreased from 170-180° to
around only 140°, indicating that surfactant A-D did not change wettability of the reservoir rock. However, surfactant E was
able to decrease the contact angle from 170-180° to 65-85°. Alteration of wettability was confirmed by a spontaneous
imbibition experiment whereas the oil-water interfacial tension of the wettability-altering surfactant E remained high (approx.
5 mN/m).

From core flood experiments it was evident that oil could be mobilized and recovered by tertiary injection of low interfacial
tension surfactant formulations such as combination A/C and B/D (+ iso-butanol + alkali). As much as 95% OIIP was
recovered from the core floods using either of the formulations. Recovery was very high but occurred at a very low rate. No
suitable mobility control agent was identified for such a low-permeability rock. UTCHEM simulations of the initial water
IPTC 17656 9

floods (leading to recoveries of 67.5% OIIP and 80.6% OIIP) were conducted showing a good match of the experiments. In-
depth interpretation of the recovery process was done based on output from the simulations.

Secondary surfactant flooding using surfactant E led to significant oil recovery of 78% OIIP after 3 PV and 82.4% OIIP after 4
PV as a result of wettability alteration. No mobility control agent, alkali or co-solvents were required which is beneficial with
respect to design and cost. The pressure profile of the surfactant flood was similar to pressure profiles of water floods in
similar cores indicating good injectivity.

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Surfactant E used in a tertiary flooding scheme involving initial water flooding followed by surfactant flooding and subsequent
chase brine injection led to an oil recovery of 40% OIIP (compared to 35% OIIP water flood). Additional chase brine injection
increased oil recovery from 40% to 45% OIIP due to a sustained wettability alteration induced by surfactant E. The core
flooding experiments involving surfactant E were modeled with UTCHEM and a good match between experimental and
simulated data was obtained.

The promising results from secondary and tertiary flooding using surfactant E encouraged us to investigate whether a flooding
design involving smaller surfactant volumes could lead to significant incremental oil recovery. It was found that addition of
surfactant E (0.2 wt%, 0.5 PV) increased the oil recovery significantly over that of the water flood in an originally oil-wet low
permeable carbonate rock. The increase was of the order of 15% and 18% OIIP for the injected surfactant solution when
operated in secondary and tertiary flooding mode, respectively. Secondary surfactant flooding led to almost the same oil
recovery as for the tertiary surfactant flood. As for the previous secondary and tertiary surfactant floods, the pressure drops
observed were similar to that of the water flood.

Technically attractive strategies have been identified for recovering significant amounts of oil using a wettability altering
agent, Tergitol 15-S-20, for secondary and tertiary dilute surfactant flooding. Even a slug size of 0.5 PV of the dilute surfactant
solution led to significant oil recovery. The surfactant was compatible with brine, exhibited low adsorption, did not require
alkali, co-solvent, or a mobility-controlling agent, and did not form any viscous macro-emulsions. An economic feasibility
evaluation has not yet been performed.

Acknowledgment
The authors wish to thank Maersk Oil Management and Qatar Petroleum for permission to publish this work.

References
Adibhatla, B., Mohanty, K.K.: “Oil Recovery from Fractured Carbonates by Surfactant-Aided Gravity Drainage: Laboratory Experiments
and Mechanistic Simulations”, SPEREE, 11, 119-130 (2008).

Austad, T., Milter, J.: “Spontaneous imbibition of water into low permeable chalk at different wettabilities using surfactants”, SPE 37236
(1997).

Bragg, J.R. et al.: “Loudon Surfactant Flood Pilot Test”, SPE 10862 (1982).

Falls, A.H., Thigpen, D.R., Nelson, R.C., Ciaston, J.W., Lawson, J.B., Good, P.A., Ueber, R.C., Shahin, G.T.: “A Field Test of Cosurfactant-
Enhanced Alkaline Flooding”, SPE 24117 (1992).

Gupta, R., Mohanty, K.K.: “Temperature Effects on Surfactant-Aided Imbibition Into Fractured Carbonates”, SPE Journal, 15 (3), 588-597
(2010).

Gupta, R., Griffin, P., Hu, L., Willingham, T.W., Cascio, M.L., Shyeh, J.J., Harries, C.R.: “Enhanced Waterflood for Middle East
Carbonates Cores – Impact of Injection Water Composition”, SPE 142668 (2011).
10 IPTC 17656

Hirasaki, G., Zhang, D.L.: “Surface Chemistry of Oil Recovery from Fractured, Oil-Wet, Carbonate Formation”, SPE Journal, 9(2), 151-162
(June 2004).

Johnson, E.F. et al.: “Calculation of relative permeability from displacement experiments”, Petroleum Transactions, AIME (1959), vol. 216.

Kalpakci, B., Arf, T.G., Barker, J.W., Krupa, A.S., Morgan, J.C., Neira, R.D.: “The Low Tension Polymer Flood Approach to Cost Effective
Chemical EOR”, SPE 20220 (1990).

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Kamath, J. Meyer, R.F., Nakagawa, F.M.: “Understanding Waterflood Residual Oil saturation of Four Carbonate Rock Types”, SPE 71505
(2001).

Krumrine, P.H., Falcone, J.S., Campbell, T.C.: “Surfactant Flooding I: The Effect of Alkaline additives on IFT, Surfactant Adsorption and
Recovery Efficiency”, SPE Journal (August 1982) 22, 503-513.

Noll, L.A.: “The Effect of Temperature, Salinity, and Alcohol on the Critical Micelle Concentration of Surfactants”, SPE 21032 (1991).

Pope, G.A., Nelson, R.C.: “A Chemical Flooding Simulator”, SPE Journal (1978), 18, 339-354.

Seethepalli, A., Adibhatla, B., Mohanty, K.K.: “Physicochemical Interactions During Surfactant Flooding of Fractured Carbonate
Reservoirs”, SPE Journal 9(4), 411-418 (December, 2004).

Sharma, G., Mohanty, K.K.: “Wettability Alteration in High Temperature and High Salinity Carbonate Reservoirs”, SPE 147306 (2011).

Standnes, D.C., Austad, T.: “Wettability alteration in carbonates: Interaction between cationic-surfactant and carboxylates as a key factor in
wettability alteration from oil-wet to water-wet conditions”, Colloids and Surfaces A: Physicochemical Engineering Aspects (2003) 216,
243-259.

Wu, Y., Shuler, P., Blanco, M., Tang, Y., Goddard, W. A.: “A Study of Wetting Behavior and Surfactant EOR in Carbonates with Model
Components”, SPE 99612 (2006).

Xie, X., Weiss, W.W., Tong, Z., Morrow, N.R.: “Improved Oil Recovery from Carbonate Reservoirs by Chemical Stimulation”, SPE 89424
(2004).

Yousef, A.A., Al-Saleh, S., Al-Kaabi, A., Al-Jawfi, M.: “Laboratory Investigation of Novel Oil Recovery Method for Carbonate
Reservoirs”, SPE 137634 (2010).

Yousef, A.A., Al-Saleh, S., Al-Jawfi, M.: “Improved/Enhanced Oil Recovery from Carbonate Reservoirs by Tuning Injection Water Salinity
and Ionic Content”, SPE 154076 (2012).

Zhang, R. et al.: “Advances in adsorption of surfactants and their mixtures at solid/solution interfaces”, Advances in Colloid and Interface
Science (2006).
IPTC 17656 11

Figures and Tables

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A
+ iso-butanol B

C D

Figure 1.
A. Surfactant formulation A/C results in micro emulsion formation. Formation of macro emulsions in the left-hand tube were removed by
adding iso-butanol in the right hand tube. B. Phase behavior studies with surfactant combination A/C indicate the existence of a wide range
of Type III system for different surfactant/co-surfactant ratios at 1.5 wt% iso-butanol. C. Interfacial tension at two different alcohol
concentrations for the A/C-surfactant system with different concentration ratios. D. Interfacial tension for B/D-surfactant system with
different concentration ratios at 1 wt% alcohol.

Figure 2. A. Oil drops on aged calcite plate in surfactant A/C with 0.5 wt% sodium metaborate and 2 wt% alcohol.
B. Oil drops on aged calcite plate in 36,000 ppm brine containing 0.2 wt% surfactant E. C Expulsion of oil using 0.2 wt% surfactant E.
12 IPTC 17656

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Figure 3 (left) Profile and recovery curves for core flood 1 for secondary water flood and tertiary surfactant (A/C) flood.
(right) Comparison between oil recoveries for water flood WF1 and WF2 (only the region from 0-5 PV is shown).

Figure 4. Salinity and oil recovery for surfactant flood on core 1 Figure 5 Relative permeability curves for Core flood 1.

Figure 6 The water floods for core 1 and 2. Experimental data and the simulation are shown.
IPTC 17656 13

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Figure 7
(top left, A) Oil recovery profile for the tertiary surfactant flood
(top right, B) The time-profile of the salinity gradient and the surfactant concentration at the outlet.
(bottom left, C) The distance-profile of the trapping number at selected time points.
(bottom right, D) The distance-profile of the residual oil saturation at selected time points.

Figure 8
A. Recovery profiles for secondary surfactant flood (blue line and points) and for two water floods as well
as pressure profile for the surfactant flood.
B. The color of two cores after secondary floods. The upper core is still oil-wet (dark color) after a water flood
whereas the lower core has changed its wettability to intermediate-wet (light color) after secondary flood with the
wettability-altering surfactant.
14 IPTC 17656

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Figure 9
(top) Contact angles of formation brine drops on brine saturated core
(bottom) oil-aged core at initial water saturation

Figure 10 Recovery and pressure drop during surfactant flood with pre- and post-flush of water.
IPTC 17656 15

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Figure 11 Oil recovery and pressure profiles for initial and post-surfactant water floods

Figure 12 Relative permeability for the WF (initial water flood) and WFPSF (water flood post surfactant flood) floods (for core A).
16 IPTC 17656

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Figure 13
(left) The initial water flood before the surfactant flood of core A.
(right) The water flood after re-aging of the core posterior to the surfactant flood.

Figure 14 Experimental and simulated pressure Figure 15 The full surfactant flood design.
drop and oil recovery for initial water flood of core B.
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17

Figure 17 The tertiary flood design applied to core 2; pressure and recovery profiles
Figure 16 The secondary flood design applied to core 1.
IPTC 17656
18 IPTC 17656

Surfactant Type Company Result

Code
B-110 Alkyl Ether Sulfate Stepan Significant precipitation with RB. Very
slight precipitation with SB, co-
surfactant or salinity <40,000 ppm.
Alf-38 Propoxy Sulfate Alcohol Sasol Significant precipitation with RB. Very
slight precipitation with SB, co-
surfactant or salinity <40,000 ppm.
Alf-68 Propoxy Sulfate Alcohol Sasol Significant precipitation.
AL Propoxy Sulfate Alcohol (7 PO) Sasol Very slight precipitation with SB, co-

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surfactant or salinity <40,000 ppm.
CS230 Sodium Lauryl Ether Sulfate-2EO Stepan Clear solution.
3PO-4EO Propoxy Ethoxy Sulfate Alcohol Stepan Clear solution.
4PE-2EO Propoxy Ethoxy Sulfate Alcohol Stepan Murky.
1518 Internal Olefin Sulfonate Shell Significant precipitation.
Chemical
2024 Internal Olefin Sulfonate Shell Significant precipitation.
Chemical
S70 Ethoxylated Sulfonate (7 EO) BASF Clear solution.
S150 Ethoxylated Sulfonate (15 EO) BASF Clear solution.
DF Alkyldiphenyloxide Disulfonate Dow Clear solution.
Chemical
T-8323 Nonionic Alkoxylate Stepan Significant precipitation.
Makon 12 Mono(nonyl phenyl) Ether Stepan Significant precipitation.
15-S Secondary Alcohol Ethoxylates Dow Clear solution. Precipitation with RB.
Chemical
NP Nonyl Phenol Ethoxylate Dow Clear solution. Precipitation with RB.
Chemical
Table 1 List of surfactants tested.

Reservoir Brine (RB)     Sea Brine (SB)  

Salt MW gm/L   Salt MW gm/L
NaCl 58.4 60.3   NaCl 58.4 32.3
MgCl26H20 203.3 13.6   MgCl2 6H20 203.3 12.6
CaCl22H20 147.0 16.8   CaCl2 2H20 147.0 1.7

Table 2 Salt composition of reservoir and sea brines

IPTC 17656 19

Initialization Core 1 Core 2

Diameter, inches 1.5 1.5

Length, inches 3.5 4.1

Porosity, % 31.5 30.6

Brine permeability, md 4.34 3.67

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OOIP, ml 28 32

Oil permeability at initial water 2.5 2.9

saturation, md
Initial oil saturation 0.875 0.89

Water flood WF1 WF2

Sea brine injected, PV 4.6 16

Brine permeability at residual oil 0.35 0.25

saturation, md
Residual oil saturation 0.28 0.20

Oil recovery, ml 18.9 25.5

Oil recovery, % 67.5 80.6

Tertiary Flood Surfactant A/C Surfactant B/D

Surfactant solution injected, PV 11 15

Tertiary oil recovery, % 28 14.7

Residual oil saturation 0.03 0.05

End-point brine permeability, md 1.8 1.4

Ultimate oil recovery, % 95.5 95

Table 3 Properties and results for the core floods experiments conducted.

Parameter Core flood 1 Core flood 2

o
krw 0.08 0.07

kroo 0.57 0.79

nw 1.60 1.40

no 3.60 3.10

Swi 0.13 0.11

Sor 0.28 0.17

Table 4 Parameters for Corey functions.

20 IPTC 17656

Core Properties Fluid Properties

Viscosity Surface
Length, Density IFT with oil
3.3 (cP) at tension
inches (g/ml) (dynes/cm)
52°C (dynes/cm)

Diameter,
1.5 Crude Oil 0.86 6.9 27.5 - 28.5
inches  
Pore Formation

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29.9 1.054 0.9 45.15
Volume, ml brine  
Total Injection
93.0 1.023 0.81 23
Volume, ml brine

0.2 wt%
Porosity, % 32 15-S-20 1.023 0.81 5
in brine

Brine
permeability, 4.80
md

Initial oil
0.87
saturation
  plug (core A) and the fluid systems.
Table 5 Properties of the core

Core Properties Fluid Properties

Viscosity Surface
Length, Density IFT with oil
3 (cP) at tension
inches (g/ml) (dynes/cm)
52°C (dynes/cm)

Diameter,
1.5 Crude Oil 0.86 6.9 27.5 - 28.5
inches  
Pore Formation
28.0 1.054 0.9 45.15
Volume, ml brine  
Total Injection
84.6 1.023 0.81 23
Volume, ml brine

0.2 wt%
Porosity, % 33 15-S-20 1.023 0.81 5
in brine

Brine
permeability, 5.3
md

Initial oil
0.88
saturation
Table 6 Properties of the core plug (core B) and the fluid systems.
IPTC 17656 21

Corey function parameter WF WFPSF

Initial water saturation 0.13 0.1

Residual oil saturation 0.57 0.45

Relative oil permeability at initial water 0.42 0.42

saturation
Relative water permeability at residual oil 0.1 0.14
saturation
Corey exponent, water 3.2 3

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Corey exponent, oil 1.9 1.3

Table 7 Relative permeability parameters for initial water flood (WF) and
water flood post-surfactant flood (WFPSF) (for core A).

Core 1 Core 2
Length, inches 3 3.2
Diameter, inches 1.5 1.5
Porosity, % 33 31.3
Initial oil saturation 0.88 0.87
Permeability at initial oil saturation, md 5 7
Table 8 Parameters associated with core 1 and 2.