SPE 133005

Design and Application of a New Acid-Alkali-Surfactant Flooding

Formulation for Malaysian Reservoirs
Khaled A. Elraies, SPE, Isa M. Tan, Universiti Teknologi PETRONAS, Malaysia

Copyright 2010, Society of Petroleum Engineers

This paper was prepared for presentation at the SPE Asia Pacific Oil & Gas Conference and Exhibition held in Brisbane, Queensland, Australia, 18–20 October 2010.

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 not be copied. The abstract must contain conspicuous acknowledgment of SPE copyright.

Abstract
A new Acid-Alkali-Polymeric Surfactant (AAPS) flooding formulation has been developed to overcome the precipitation
problems caused by the divalent metal cations prevalent with conventional ASP flooding. The acid was evaluated in an acid-
alkali-surfactant formulation using sodium carbonate and introducing a new polymeric surfactant derived from Jatropha oil.
The effect of the new formula on IFT, viscosity, and oil recovery was studied using natural seawater having a large quantity of
divalent metal cations. The tolerance of the AAPS towards natural untreated sea water was monitored for 90 days at 90 oC. No
precipitations were formed with the acid additive, while precipitations were always generated without the acid. A combination
of the new system was found to significantly reduce the IFT between Angsi crude oil and AAPS solution. The most
outstanding feature of the AAPS formulation lies in its viscosity insensivity towards an increasing alkali concentration up to
1.2%. Core flood tests with alkali and acid concentrations of 0.6% and 1% respectively confirmed an optimum surfactant
concentration of 0.6%. Using the optimum AAPS concentrations, another series of core flood were conducted by changing the
injection volume. Only a small incremental recovery was obtained with AAPS slugs higher than 0.5 PV. Injection of 0.5 PV of
the formulated AAPS slug followed by chase water produced an additional 18.8% OOIP over water flooding. The benefit of
the new system is the use of seawater rather than softened water while maintaining the desired slug properties.

Introduction
In Malaysia and many other countries, most mature reservoirs are already waterflooded, or are presently being subjected to
secondary and tertiary recovery processes. In Malaysian oil reservoirs, only about 36.8% of original oil in place (OOIP) is
produced through the entire life of mature reservoirs that have been developed under conventional methods (Hamdan et al.,
2005). A significant amount of the hydrocarbon would not be recovered utilizing the current production strategies, and that has
motivated Malaysia to attempt Enhanced Oil recovery (EOR).

Recognizing the potential of EOR in the fields, the national oil company (PETRONAS) endorsed a comprehensive EOR
screening in year. The screening study on seventy two reservoirs has identified almost a billion barrels of additional reserves
can be achieved through EOR (Samsudin et al., 2005). The Chemical Enhanced Oil Recovery (CEOR) was identified as one of
the key EOR processes that have good potential for field implementation to increase ultimate recovery in Malaysian oil fields
(Othman et al., 2007).

Chemical EOR processes are being considered for large field applications with recent high price of crude oil (Ibrahim et al,
2006). These include surfactant (S), surfactant-polymer (SP), and alkali-surfactant-polymer (ASP). ASP flooding has been
used widely in a field application with great success (Pitts et al., 2006; Pratap and Gauma, 2004; Clara et al., 2001; Wang, et
al., 1997; Hong-Fu, et al., 2008). It uses the benefits of the three flooding methods simultaneously and oil recovery is
sufficiently improved by decreasing the interfacial tension (IFT), increasing the capillary number, and improving the mobility
ratio (Pingping et al., 2009). Despite the potential of ASP flooding, the approach towards ASP in Malaysia has taken a
conservative route. This could be attributed mostly to the fact that all of the producing fields are located offshore. Offshore
environment poses a number of challenges (Hamdan et al., 2005).

One of the primary considerations for chemical flooding application in Malaysia is the use of seawater rather than softened
water as injection water (Hamdan et al., 2005). However, using seawater adds other problems to the process. Adding alkaline
agents such as sodium carbonate or sodium hydroxide will result in precipitation of the anions with divalent metal cations
(calcium, magnesium, potassium. etc) in the seawater. The alkali has also a detrimental effect on polymer performance and in
2 SPE 133005

many cases additional polymer is required to achieve the desired viscosity (Wang et al., 2006). Nasr-El-Din et al., (1992)
documented that there was an exponential decrease in viscosity of the combined ASP solution with an increase in alkali
concentration. A process that eliminates some of the existing problems is required and this paper is proposing a new system for
ASP flooding that will mitigate viscosity reduction.

In this study, a new chemical formulation has been developed to overcome the precipitation problems caused by the
divalent metal cations such as calcium (Ca2+) and magnesium (Mg2+). It consists of an acid, alkali, and polymeric surfactant
(AAPS). The main advantage of the new combination involves the use of seawater without the need for softening the injection
water or preflushing the reservoir before injection.

The Mechanism of the New Formula

In order to use seawater as injection water, acid-alkali-polymeric surfactant formulation has been developed. The polymeric
surfactant is the main component used in the new formulation. It is a one component system for a simultaneous IFT reduction
and viscosity control. The acrylic acid and alkali are used together with seawater to form the sodium salt of acrylic acid. The
sodium acrylate acts as a precipitation inhibitor to prevent the reaction between divalent metal cations (Ca2+ and Mg2+) and the
polymeric surfactant. The inhibitory effect of the sodium acrylate is due to the adsorption of the acrylates on the crystal surface
or at the active growth sites of the divalent metal crystals (Mohnot and Chakrabarti, 1987; Amjad, 1989).

In the AAPS system, the precipitation inhibitor (sodium acrylate) was produced in-situ with added acid and alkali before
introducing the polymeric surfactant to the system. When enough acid-alkali concentrations were used, sufficient precipitation
inhibitor will be generated to prevent the reaction between divalent metal cations and the subsequently added surfactant. When
there are no free calcium and magnesium ions in the solution, the surfactant is then introduced to the system without any
precipitation problems.

Experimental Methodology
Material Description. Crude oil collected from Angsi I-68 reservoir, offshore Trengganu, Malaysia was used in this study.
The API gravity was 40.1o and the live oil had a viscosity of 0.3cp. The kinematic viscosity of the dead oil used in this study
was 1.456 mm2/sec at test temperature of 90oC.

Three types of alkalis, namely, sodium hydroxide, sodium carbonate, and sodium bicarbonate were screened to define the
suitable candidate. The acid used in the new formula was acrylic acid. It is a weak polymer acid and used widely as a
precipitation inhibitor. Polymeric sodium methyl ester sulfonate was used for IFT reduction and viscosity control. This
polymeric surfactant was produced in our laboratory and full details on this surfactant can be found in Elraies et al, (2009).

Natural seawater was used as injection water and synthetic brine similar to the formation water was blended to saturate the
core sample prior to core flood test. The compositions of seawater and synthetic brine are given in Table 1. A series of core
flood experiments are performed to investigate the performance for the polymeric surfactant and slug size. The basic
properties of the core samples are given in Table 2.

Table 1: Seawater and synthetic brine compositions Table 2: Basic properties of core samples
Sea water Synthetic brine Core ID 1 2 3 4 7 8
Salinity, ppm 33,400 9990 Length, cm 7.5 7.1 7.4 7.5 7.4 7.1
Sodium, ppm 11,908 3810 Diameter, cm 3.8 3.8 3.8 3.8 3.8 3.8
Chloride, ppm 14,010 6070 Porosity, % 16.8 17.2 16.8 16.4 15.2 16.2
Calcium, ppm 790 30 Pore volume, cc 14.4 13.9 14.2 13.9 12.8 13.1
Magnesium, ppm 6720 25 Permeability, md 102 105 104 86 64 87
Potassium, ppm 373 55

Apparatus and Methods. The first stage of the study concerns the fluid-fluid compatibility test using natural seawater. The
fluid-fluid interactions involved were acid-alkali, and acid-alkali-polymeric surfactant. Different acid-alkali weight ratios were
used to investigate the performance of the generated in-situ inhibitor in preventing the Ca2+ and Mg2+ precipitations. The
compatibility tests were conducted at 90°C for a period of time, and observation was made by visual evaluation with the
formation of solids being indicative of incompatible fluids. The kinematic viscosity of the acid-alkali-polymeric surfactant
(AAPS) solutions was measured using Tamson viscometer model TVB44 at 90oC.

Interfacial tensions (IFT) between different AAPS solutions and Angsi crude oil were measured with spinning drop
method. Model SVT 20 spinning drop tensiometer equipped with a video camera was used to determine the IFT at ambient
temperature. Phase behavior tests were conducted over a range of acid-alkali concentrations using seawater. The test samples,
SPE 133005 3

oil and AAPS solutions at different concentrations were prepared with a fixed crude oil/AAPS solution ratio and placed in an
oven at 90oC over a period of time.

Oil recovery was determined using linear Berea sandstone core samples. A series of coreflood tests were conducted to
define the optimum surfactant concentration. In a typical test, core sample was saturated with synthetic brine followed by oil
until an immobile water saturation condition is achieved. The core was next flooded to the residual oil saturation or the
remaining oil saturation. At residual oil saturation, the core was flooded with 0.5PV of AAPS slug using an injection rate of
0.5 ml/min. Once the entire AAPS slug has been injected, extended water flood was initiated until the oil production became
negligible. For all runs, synthetic brine similar to Angsi formation water was used to displace Angsi crude oil before and after
the AAPS flood was initiated.

Results and Discussions

Fluid-Fluid Compatibility Test

Polymeric surfactant-seawater interaction: The polymeric surfactant used in this study was incompatible with the seawater.
Precipitation was observed with solutions of either surfactant at 0.1% and 0.6%. Solutions became cloudy and as they aged
solid deposits were formed. This is attributed to the interaction between the divalent metal cations and the sulfonate groups of
the surfactant.

Acid-alkali interaction: All alkalis employed in this study were incompatible with the seawater. They were immediately
consumed by Ca2+ and Mg2+ ions to form their insoluble compounds as precipitations. To eliminate the precipitations, different
acrylic acid to alkali weight ratios were used to evaluate the performance of the in-situ precipitation inhibitor in preventing
Ca2+ and Mg2+ precipitations. Fig. 1 shows the performance of the in-situ inhibitor in combating Ca2+ and Mg2+ precipitations
over time.

Table 3: Summary of the acid-alkali

compatibility test after 90 days at 90 oC
0:1 0.3:1 1:1 1.6:1 2.3:1
Sodium hydroxide
Days (Sodium hydroxide)
0:1 0.3:1 1:1 1.66:1 2.33:1
pH
0 10.9 11.1 11.06 11 5.73
0 ppt ppt ppt Cloud -
4 ppt ppt ppt ppt -
12 ppt ppt ppt ppt -
90 ppt ppt ppt ppt -
Sodium carbonate 0:1 0.3:1 1:1 1.6:1 2.3:1
pH
0 10.64 10.4 10.22 5.7 5.02 (Sodium carbonate)
0 ppt Cloud - - -
4 ppt ppt - - -
26 ppt ppt ppt - -
40 ppt ppt ppt - -
90 ppt ppt ppt - -
Sodium bicarbonate
pH
0 9.63 9.31 5.63 4.86 4.33
0 - - - - - 0:1 0.3:1 1:1 1.6:1 2.3:1
7 ppt - - - -
(Sodium bicarbonate)
19 ppt ppt - - -
40 ppt ppt - - -
60 ppt ppt - - -
90 ppt ppt - - -
ppt denotes precipitation, - denotes clear solution
2+ 2+
Fig. 1. Performance of the in-situ inhibitor in preventing Ca and Mg
o
precipitations after 90 days at 90 C

Based on the summary of results presented in Table 3, the generated in-situ inhibitor was very effective in preventing Ca2+
and Mg2+ precipitations over 90 days at 90oC. In the case of sodium hydroxide, a high acid to alkali ratio was required to
provide adequate inhibitor (sodium acrylate) as compared to the other alkalis. With an acid to alkali ratio of 1.66:1, the acid
was fully consumed by the alkali and the generated inhibitor was inadequate to prevent the Ca2+ and Mg2+ precipitations. As
the acid to alkali ratio was increased to 2.33:1, Ca2+ and Mg2+ ions became more soluble due to the presence of inhibitor and
excess acrylic acid. The inhibitor adsorbs on the active growth sites of the Ca2+ and Mg2+ surfaces to prevent the latter from
precipitating. The presence of the acid makes the solution more acidic which increases the solubilities of these ions.
4 SPE 133005

From the foregoing, sodium hydroxide was not considered for selection because of its detrimental reaction with the acrylic
acid and Ca2+ and Mg2+ ions. On the other hand, the weak pH alkali (sodium bicarbonate) showed the lowest acid to alkali
ratio required to maintain the solution free from precipitation. However, because the high pH is also needed in this system, so
sodium carbonate with the optimum ratio of 1.66:1 was selected as the best candidate for this study.

The effect of temperature on the inhibitor performance: The effect of various temperatures on the precipitation inhibitor
performance was investigated for 54 days using different acid to sodium carbonate weight ratios. As a result, the temperature
has no effect on the inhibitor performance if the optimum acid to alkali ratio was used. However, when the acid to alkali ratio
was less than optimum, the inhibitor was ineffective when the temperature exceeded 60oC. Beyond 60oC, temperature has little
effect on the inhibitor performance.

Acid-alkali-polymeric surfactant interaction: The compatibility of the acid-alkali-polymeric surfactant (AAPS) with seawater
was investigated at different temperatures for 63 days. Different sodium carbonate concentrations were used to define the
optimum alkali concentration in the presence of surfactant. The surfactant concentration was maintained at 0.6% and the acid
concentration was set proportional to the alkali concentration using the ratio of 1.66:1.

As shown in Table 4, all the AAPS solutions remained clear for 63 days when these solutions were kept at room
temperature. However, precipitations were formed when AAPS solutions were maintained at 90oC. As can be seen from Table
4, precipitations were generated when the alkali concentration was 0.6% or less, while clear solutions were obtained when the
alkali concentration exceeded 0.6%. An explanation is that when the alkali concentration was 0.6% or less, the acid
concentration was not sufficient to generate the required amount of in-situ inhibitor in the presence of surfactant. However,
when the alkali concentration exceeded 0.6%, the generated in-situ inhibitor was capable of preventing any precipitations.

Table 4: Effect of different alkali-acid concentrations 3.5

in the inhibitor performance
o
Alkali concentration @ 90 C 3
0.2% 0.4% 0.6% 0.8% 1% 1.2%
Viscosity, mm2/second

Acid concentration 2.5

days
0.33% 0.66% 0.99% 1.32% 1.66% 1.99%
2
pH
9.54 9.36 9.17 9.09 9.05 8.74
1.5
1 - - - - - -
26 - - - - - - 1
36 ppt - - - - -
40 ppt - - - - - 0.5
49 ppt ppt ppt - - -
63 ppt ppt ppt - - - 0
o 0 0.2 0.4 0.6 0.8 1 1.2 1.4 1.6 1.8
@ 26 C
Alkali concentration, %
1 - - - - - -
63 - - - - - - 0 0.33 0.66 0.99 1.32 1.66 1.99 2.32 2.65 2.98
Acid concentration, %
ppt denotes precipitation, - denotes clear solution
Fig. 2. The effect of different alkali-acid concentrations on the
o
viscosity performance (0.6% surfactant - 90 C)

The effect of the inhibitor on viscosity performance was investigated using different alkali and acid concentrations and
0.6% surfactant concentration. The most interesting and important finding shown in Fig. 2 is the large increment in the
viscosity of acid-alkali-polymeric surfactant (AAPS) as compared to the polymeric surfactant without acid and alkali additive.
This is due to the presence of the inhibitor and the excess amount of acrylic acid in the solution. This feature makes the new
AAPS slug a superior compared to the conventional ASP where the polymer is greatly affected by the alkali.

Interfacial Tension and Phase Behavior Test.

Fig. 3 shows the IFT measurements between the crude oil and full system of acid-alkali-polymeric surfactant. The effect of
precipitation inhibitor in the IFT was investigated using different alkali-acid concentrations and 0.6% surfactant concentration.
The IFT increased drastically with the addition of alkali and acid concentrations and remained constant as the alkali and acid
concentrations were as high as 0.6% and 0.99% respectively. This is associated with the change in salinity of the system
caused by the generated in-situ inhibitor and excess amount of acrylic acid. When the acid and alkali are used together with the
polymeric surfactant, the generated inhibitor can block the active sites of the Ca2+ and Mg2+ ions resulting in a decrease in the
salinity of the system. At a critical acid and alkali concentrations, the surfactant will be able to play its role of reducing the
IFT. As shown in Fig. 3, the critical acid and alkali concentrations were seen to be 0.99% and 0.6% respectively.

The above IFT trends were also confirmed by the phase behavior tests (Fig 4). The phase behavior test was conducted for
24 days at 90oC days using same acid, alkali, and polymeric surfactant concentrations employed during IFT measurements. All
the AAPS solutions possess a middle phase microemulsion (type III). Type III microemulsion is unique and favorable because
SPE 133005 5

both interfaces have equal volumes and low IFT. As the alkali and acid concentrations increased, the middle phase
microemulsion volume decreased due to the reduction of the salinity. This decreases the surfactant concentration in the middle
phase, resulting in an increase of IFT in the middle phase microemulsion (Flaaten et al., 2008).
0.8

Alkali concentration
Interfacial tension, mN/m

0.6
0.6% 0.8% 1% 1.2% 1.4%

Acid concentration

0.4 0.99% 1.32% 1.66% 1.99% 2.33%

0.2

0
0 0.2 0.4 0.6 0.8 1 1.2
Alkali concentration, %

0 0.33 0.66 0.99 1.32 1.66 1.99

Acid concentration, %
Fig. 4. Phase behavior of acid-alkali-surfactant/crude oil
Fig. 3. IFT between crude oil and various alkali- o
system after 24 days at 90 C
acidconcentrations (surfactant 0.6%)

Core Flood Test

Based on the compatibility tests, IFT measurements and phase behavior tests, the chemical formula of 0.99% acid, 0.6% alkali,
and 0.6% polymeric surfactant was determined as the best formula. However, in order to examine the effectiveness of the new
polymeric surfactant, three core flood runs with different surfactant concentrations (0.2%, 0.6%, and 1%) were conducted to
reconfirm the optimum surfactant concentration. For each test, alkali and acid concentrations were kept constant at 0.6% and
0.99% respectively.
Fig. 5 shows the oil recovery performance as a function of different surfactant concentrations. The recovery increased
significantly as the surfactant concentration was increased from 0.2% to 0.6%. When the surfactant concentration was higher
than 0.6%, oil recovery increment was not significant. With 0.2% surfactant concentration, only 7.2% OOIP was recovered
after the injection of 0.5PV of AAPS slug followed by 4.66PV chase water. However, using 0.6% surfactant, 18.8% OOIP was
produced over water flooding when 0.5PV of AAPS slug was injected and followed by 5.38PV chase water. This indicates that
the mobility control between the AAPS slug and crude oil was necessary for the new formula. When the surfactant
concentration was increased to 1.2%, the recovery increment was not significant as compared to the recovery obtained from
0.6% surfactant. From these results, it can be concluded that 0.6% surfactant is the optimum surfactant concentration for this
study.

25 25 20%
20% 21.3% 18.8%
18.8%
20
20
Oil recovery, %OOIP
Oil recovery, %OOIP

15
15
8.66%
7.2% 10
10

5
5

0
0 0.3 P V 0.5 P V 1P V
0.2% 0.6% 1. 0% 1. 2% S lug s ize
S urf a c t a nt c o nc e nt ra t io n
Fig 6. Effect of slug size on oil recovery
Fig 5. Effect of surfactant concentration on oil recovery (Acid 0.99%, Alkali 0.6%, Surfactant 0.6%)
(Acid 0.99%, Alkali 0.6%)

Using the optimum acid, alkali and polymeric surfactant concentrations, a series of core flood experiments were performed
using different AAPS slug size. Fig. 6 shows the oil recovery performance as a function of different slug sizes of AAPS
formula. Obviously, 0.3 PV of AAPS slug was not effective in forming an oil bank for recovering waterflooded residual oil as
compared to 0.5 PV. However, only a small incremental recovery was observed when the AAPS slug size was increased from
0.5 PV to 1 PV. This indicates that the injection of 0.5PV of AAPS slug is effective and therefore more economical than other
relatively larger slug sizes.
6 SPE 133005

Conclusion
1. Alkali-water interactions showed that sodium hydroxide, sodium carbonate, and sodium bicarbonate were incompatible
with seawater where the precipitations were always generated at 90oC.
2. With the incorporation of acrylic acid, the generated in-situ inhibitor was very effective in preventing calcium and
magnesium precipitations over 90 days at 90oC. The acid to sodium carbonate ratio of 1.66:1 was found to be the optimum
ratio for generating sufficient precipitation inhibitor.
3. Acid-Alkali-Polymeric Surfactant Interaction showed that the alkali concentration should be equal or higher than the
polymeric surfactant concentration in order to prevent the precipitations.
4. The most interesting and important feature of the formula is the increment on the viscosity of AAPS solution. The
viscosity of the AAPS system increased with the increase of alkali-acid concentration. This is contrary to the popular
believe of ASP viscosity reduction associated with alkali incorporation
5. The IFT increased as the alkali-acid concentration was increased up to the critical concentration of 0.6%-0.99%. After this
concentration, the IFT was slightly decreased.
6. Using the optimum acid and alkali concentrations, the oil recovery was improved as the surfactant concentration was
increased. The optimum chemicals concentration was confirmed as 0.99% acid-0.6% alkali-0.6% surfactant. Injection of
0.5PV of this slug followed by chase water produced 18.8%OOIP over waterflood.
7. The benefit of the new system is the use of seawater rather than softened water while maintaining the desired slug
properties. This makes the new AAPS formula an attractive and cost-effective agent for CEOR particularly for offshore
field application.

Acknowledgment
The authors would like to thank Universiti Teknologi PETRONAS (UTP) for supporting this research work. Also
contributions made by Mr. M. Riduan and Mr. Shahrul Rizzal from reservoir laboratory at UTP are also appreciated.

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