SPE-190086-MS

Single Phase Microemulsions Applied to Oil Sands

P. Sharma, K. Kostarelos, and X. Xiong, University of Houston

Copyright 2018, Society of Petroleum Engineers

This paper was prepared for presentation at the SPE Western Regional Meeting held in Garden Grove, California, USA, 22-27 April 2018.

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
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Abstract
Extra–heavy oil sands deposits represent a significant part of the oil resources available all around the world.
Current recovery techniques such as open pit mining, SAG-D, etc., are not very efficient and have been
debated for their possible adverse effect on environment. We propose a method of oil recovery that has the
potential of being a "game changer" for such resources: using cyclic injection of surfactant solutions forming
single–phase microemulsion (m.e.) without mobilizing the oil. This type of m.e. has several advantages: it
is less viscous than the extra heavy oil/bitumen; when the surfactant is injected, the m.e. can finger through
the tar to a production well, where it will contain a high mass of heavy oil and can be transported without
addition of diluent. This approach would use two parallel horizontal wells as an injector/producer pair so
that injected surfactant solution would create viscous fingers/flow paths through the oil sands. The m.e.
formed during the process would be produced in the second well. After transportation, the surfactant will
need to be recovered from the m.e. and recycled for re-injection.
Phase behavior experiments such as surfactant screening, salinity scans and aqueous stability were
conducted focusing on forming single phase m.e. Previous work aimed at single phase m.e. used coal tar
as a model oil for phase behavior studies and flow experiments that yielded promising results. As a result
of the previous work, new phase behavior studies were conducted using bitumen extracted from oil sands
obtained from Alberta, Canada that are presented in this paper. Three flow experiments were conducted
using a surfactant formulation selected based on the results of the phase behavior experiments to recover
bitumen from the oil sands.
For bitumen, single phase m.e. was achieved with a mixture of internal olefin sulfonate and alcoxy sulfate
(1:1) surfactants with alkali (sodium carbonate), with bitumen solubilization of the order of 300,000 ppm.
The three flow experiments were conducted to explore two different flow schemes, to compare a synthetic
oil sand (bitumen from oil sands mixed with OK-75 sand) with an actual oil sand, and to investigate the
effects of two experimental setups. The recoveries from these flow experiments were lower than expected,
only achieving a bitumen solubilization of the order of 10,000 ppm. The analyses of the results and possible
reasons for lower recovery are discussed in the paper.
Surfactant solubilization method using single phase m.e., could provide an environment-friendly
alternative to current recovery methods. It would also eliminate the need of adding solvents for
transportation. While improved surfactant formulations could yield better recovery, the economic feasibility
2 SPE-190086-MS

of the process will depend upon the final step—recovery of the surfactant from the produced m.e. Work is
currently being conducted on several potential surfactant recovery processes.

Introduction
Oil sands deposits are present in vast proportions in various parts of the world, mainly in Canada and
Venezuela. According to World Energy Council survey published in 2010, there are total 598 deposits of
natural bitumen reported in 23 countries all around the world.[1] The International Energy Agency reported
in 2013 that the estimated recoverable resources for unconventional oil are equivalent to the conventional
oil,[2] hence the recovery of these resources are critical for future energy demands.
There are both ex-situ and in-situ methods available for heavy oil recovery. The open pit mining is the
most important ex-situ process. It relies on hot-water extraction process, which has a large environmental
footprint. It requires large amount of fresh water (1:4 water to oil sands ratio[3]) and also results in creation of
tailing ponds containing toxic oil components. The most important in-situ methods of recovery of heavy oil
are either thermal, such as steam assisted gravity drainage (SAG-D), cyclic steam stimulation (CSS), vapor
extraction (VAPEX), or non-thermal such as cold heavy oil production with sand (CHOPS) and chemical
enhanced oil recovery. SAG-D consumes large quantity of water and is energy inefficient due to the loss
of energy to the sub-surface.[4] CSS is criticized for low hydrocarbon recovery and less energy efficiency.[5]
VAPEX process is regarded as more energy efficient than SAG-D[6] but it can lead to flow problems as a
result of de-asphalting of the oil. CHOPS is a non-thermal, in-situ recovery technique where sand production
is encouraged with oil. It increases the porosity and permeability by creating wormholes, dilated zones, and
cavities. This method is useful in the presence of the solution gas. Handling and disposal of the produced
sand is a challenge with this process.[5]
Other potential non-thermal method is the chemical enhanced oil recovery. It is attractive due to minimal
effect on the environment and energy efficiency. Kumar and Mohanty applied the traditional alkali-
surfactant-polymer (ASP) flooding, but for a medium-heavy oil (330 cP) not bitumen.[7] Sim et al. also
proposed the alkali-surfactant-polymer (ASP) flooding for bitumen and reported improved oil recovery as
compared to polymer flooding but the pressure differential for the process was very high.[8] Fortenberry et
al. compared polymer and ASP floods for heavy oils of varying viscosities. ASP improved the performance
in every case but both polymer and ASP process performed poorly for higher viscosities.[9] The other
application of chemical EOR is the use of alkali to increase the sweep efficiency of the flood. Alkali reacts
with the naphthenic acid present in the oil and generates in-situ surfactants, which in turn create water-
in-oil emulsion. The emulsion blocks the high permeable areas of the reservoir resulting in better sweep.
The use of alkali only or in combination of surfactant was discussed in several studies.[10–14] The recovery
mechanism is disputed for alkali injection and also the improvements are not very significant.
The cyclic surfactant solubilization using single phase microemulsion can be a green and energy efficient
alternative for heavy oil recovery. This approach proposes injection of surfactant formulation into the
subsurface to achieve single phase m.e. with high oil solubilization. The produced m.e. has a lower viscosity
than bitumen, hence eliminating the need for solvent addition for transportation. After transportation the
m.e. would need to be separated to recover surfactant solution for re-injection.[15]
The work presented in this paper is a follow-up of previous work performed using coal tar as a model
oil for heavy oil. The phase behavior experiments exhibited that a surfactant formulation with a mixture of
sulfate and sulfonate (1:1) surfactants, triethylene glycol mono-butyl ether and sodium carbonate (alkali)
can achieve single phase m.e. The flow experiment conducted using synthetic tar sand (coal tar mixed with
OK-75 sand) with this surfactant formulation resulted in recovery of 77% of OOIP. Only low visocity single
phase m.e. was produced and the maximum viscosity of the produced m.e. was 80 cP.[15]
This paper presents results of phase behavior experiments to find a suitable surfactant formulation for
bitumen from oil sands to achieve single phase m.e. The surfactant formulation was utilized for dynamic
SPE-190086-MS 3

(flow) experiments. The results of these flow experiments are discussed in this paper. This paper also
presents results of some of the batch experiments performed on oil sands and synthetic sands samples mixed
with surfactant formulations.

Materials
Two types of Oil sands were acquired from Alberta Innovates Technology Futures, Alberta, Canada, high
grade and low grade in quality. High grade sand was used for oil extraction and one of the flow experiments.
Based on the soxhlet extraction, high grade sand has 12.7 wt.% bitumen. API gravity of the bitumen was
measured to be 6.8. Total acid number (TAN) was calculated to be 2.94 mg/g of KOH. The high grade sand
bitumen was analysed for saturates, aromatics, resins and asphaltenes (SARA) and results are listed in Table
1. The viscosity of the bitumen was measured using Anton Paar MCR 302 with standard CC27 Single Gap
Measuring System. The viscosity at 20 C was 6043 cP. The sand utilized in preparing synthetic oil sand
was provided by US Silica, OK-75 grade.

Table 1—SARA analysis for bitumen reported as wt.%

Surfactants utilized in the experiments were provided by different vendors. Surfactants used and their
vendors are listed in Table 2. Phase behavior tests were performed using anionic surfactants mainly. In
addition to surfactants, other chemicals used are listed with the specific vendors in Table 3.

Table 2—Details of surfactants

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Table 3—Chemicals

Experimental methods
Bitumen Extraction
Bitumen in oil sand was extracted using solvent extraction to be used in phase behavior studies.
Dichloromethane (DCM) was used as a solvent because of its low boiling point. High grade oil sand was
washed with DCM and the extract was transferred to a round bottom flask. The solvent was evaporated at
40 C from the extract and collected for re-use; remaining bitumen in the flask was transferred to a collection
vessel. Collected solvent was analyzed using GC-MS to ensure no bitumen component was evaporated.
This process was repeated to collect 1liter of bitumen for the experiments.

Phase behavior studies

Traditional phase behavior methods are extremely difficult to use for bitumen due to its high viscosity at
room temperature. Thus, phase behavior studies were conducted using 10 ml glass test tubes. Surfactant
stock solutions were prepared at a range of concentrations. The studies were performed at a water oil ratio
(WOR) of 1:1 and 4:1 at 20 C temperature. Surfactant solution and bitumen were mixed in the test tube
based on the desired WOR. Test tubes were sealed with aluminium foil and plastic caps to avoid any losses
due to evaporation. Tubes were inspected visually and after equilibration analyzed using GC MS.
The GC method is detailed in Table 4.
SPE-190086-MS 5

Table 4—GC method for bitumen

Flow experiments
Three flow experiments were performed: one using field obtained oil sands and two using synthetic oil nd,
which was prepared by mixing extracted bitumen and OK-75 sand.
Oil sand flow experiment. Oil sand flow experiment was performed in Kimble-Kontes Chromaflex glass
column, 15 cm long and 2.5 cm in diameter. The glass column was packed with approximately 130g of tar
sand. The experiment was conducted at various flow rates using a HPLC pump Jasco PU-2086. A water bath
(Fisher scientific ISOTEMP 6200 R28) was used to circulate water within the column jacket to maintain
temperature at 20 C during the experiment. The pressure drop during the experiment was measured with
an Omega PX-26 series pressure transducer. Produced fluid was collected in test tubes using fractional
collector and the bitumen concentration was analyzed using GC to calculate the concentration of bitumen.
The flow experiment setup is shown in Figure 1.

Figure 1—Glass column setup for oil sand flow experiment and first synthetic oil sand experiment.
6 SPE-190086-MS

Synthetic oil sand flow experiments. Two synthetic oil sand flow experiment was performed. The first
experiment was conducted using the same glass column that was used for the oil sand flow experiment
as described above. Synthetic oil sand was prepared with 13 wt.% bitumen content. Surfactant solution
was injected from bottom to top. The second experiment was performed to investigate the possibility of
channeling along the walls of the glass column, so it was conducted in a high pressure core holder with a
confining pressure of 500 psi. It was a 6-inch in length and 1.5-inch in diameter sandpack. A total 330 g of
synthetic tar sand was used to make the sand pack. Produced liquid from both experiments was collected
in glass test tubes and analyzed using GC-MS for bitumen concentration. The same pump and pressure
transducers were used as for the oil sand experiment described above. The flow diagram of the setup is
shown in Figure 2.

Figure 2—High Pressure core holder setup for the second synthetic oil
sand flow experiment. The confining pressure was maintained at 500 psig.

Batch tests
The results from several flow experiments (reported later) showed a significantly lower degree of bitumen
solubilization compared with the phase behavior experiments. A series of batch tests were designed to
investigate the possible effect that the sand may have on the degree of solubilization. The selected surfactant
formulation (10 ml) were mixed in a 20 ml glass test tubes with 10 g of oil sand sample. The mixtures
were allowed to settle and the concentration of bitumen in the supernatant (microemulsion) was analyzed
using GC-MS.
Additional batch tests were designed to study the possible effect of the sand properties on the surfactant
solubilization of bitumen. Synthetic oil sand was prepared by mixing bitumen with clean sand at mass
fractions of 9.1, 16.6, 13 and 23 wt. % of oil. These sands samples were added to glass test tubes so that
the mass of bitumen in each was maintained constant, i.e. the amount of bitumen was 2g in each test tube.
Next, 10 ml of the surfactant solution was added to each test tube and thus the amount of surfactant and
bitumen in each test tube was the same in each and only the mass of sand varied. After the test tubes were
mixed and allowed to equilibrate, the concentration of bitumen within the microemulsion (supernatant) in
each was measured by GC/MS.
SPE-190086-MS 7

Results and discussion

Phase behavior studies
Surfactant screening was performed for WOR of 1:1 and 4:1 for a total of 30 surfactant formulations. Figure
3 depicts the phase behavior for a blend of two surfactants, 0.50 wt.% C20-24 IOS and 0.50 wt.% C13
13 PO alcoxy sulfate, with 1 wt. % 2-butanol, and 0.5 wt.% sodium carbonate. Additional studies showed
that lower surfactant and co-surfactant could also be used, and the final formulation based on a WOR 1:1
was 0.25 wt% C20-24 IOS, 0.25 wt% C13 13 PO alcoxy sulfate, 0.25 wt % 2-butanol and 0.5 wt% sodium
carbonate.

Figure 3—Phase behavior tubes for 0.5% C20-24 IOS, 0.5% C13 13 PO sulfate, 1% 2-butanol and 0.5%
sodium carbonate. Surfactant formulation showed good interaction with bitumen. The two lower salinities
exhibit type I (Winsor) behavior, while the two highest salinities exhibit type II (Winsor) behavior.

This selected formulation was also mixed at different WOR to observe the solubilization performance at
higher WOR ratios, namely WOR 2, 3 and 4. The surfactant formulation resulted in single phase m.e. for
all the WOR ratios as shown in Figure 4. The degree of solubilization was 300,000 ppm, and preferential
solubilization was not observed.
8 SPE-190086-MS

Figure 4—Phase behavior tubes for 0.5% C20-24 IOS, 0.5% C13 13 PO sulfate, 1% 2-
butanol and 0.5% sodium carbonate. Salinity 0.2% and WOR from left to right 2,3 and 4.

Flow experiments
Oil sand flow experiment. Surfactant solution was initially injected with flow rate of 0.032 mL/min into
the vertically–oriented column from top to bottom. Since the bitumen is heavier than water, any bitumen
that was recoverable by means of viscous and gravity forces would be noted. No gel formation was observed
and only m.e. was produced. The surfactant broke through at about 0.73 PV and pressure became steady.
On visual examination, the produced m.e. appeared to contain a low amount of bitumen in comparison with
the phase behavior results. The samples were analyzed by means of GC-MS and the analysis confirmed
that the concentration of bitumen in produced fluid was approximately 12,000 ppm at the time of surfactant
breakthrough and reduced to 3500 ppm, in contrary to the phase behavior where concentration of up to
300,000 ppm was observed.
Based on these observations the experiment was shut-in at approximately 2 PV for approximately 8 hrs.
Upon commencing surfactant injection, the flow direction was changed to be upwards, from bottom to top.
The bitumen concentration in the produced samples increased to 7500 ppm immediately after the shut–in
period, but decreased to 1500 ppm after 2 PV of injection. The shut–in process was employed periodically,
after every 1 PV injection, to understand whether rate–limited processes were affecting the results. Total
bitumen recovery after 10 PV injected was 4.52%.
As a result of this, the flow rate was reduced to increase the contact time of the surfactant more time
to react with the bitumen. Injection was started at a lower flow rate 0.017 ml/min. A total of 7 PV of
surfactant solution was injected; performance in terms of bitumen recovery continued to be low. To rule
out the possibility of channeling with the sandpack or along the column walls, the next 3PV of surfactant
solution included a viscosifer namely 400 ppm polymer (xanthan gum). Polymer addition increased the
pressure drop of the system as expected, but the bitumen concentration in the produced m.e. remained
the same indicating that channeling was not likely the cause of the low bitumen solubilization. Overall
incremental bitumen recovery for the second 10 PV injection was 2.97%. Cumulative recovery and pressure
drop for the experiment is shown in Figure 5.
SPE-190086-MS 9

Figure 5—Pressure drop and cumulative recovery with respect to pore volume of
surfactant solution injected for the oil sand flow experiment initial 10 PV injection.

Synthetic oil sand flow experiment. Two flow experiments were conducted using synthetic oil sand,
i.e., bitumen combined with clean sand (pure quartz sand) at the same mass fraction found in the actual
high grade oil sand. The first synthetic oil sand flow experiment utilized the same setup as actual oil sand
experiment. The purpose of the experiment was to understand whether some element within the actual oil
sand (e.g., clay minerals, silts, or other materials) were adversely affecting the recovery process. The flow
rate was maintained at 0.017 ml/min and temperature at 20C. A total of 8 PV solution was injected, and
the bitumen concentration in effluent was measured to be 10000 ppm initially and dropped to 2000 ppm
—again, significantly lower than the expected values from phase behavior that were upwards of 300,000
ppm. The total recovery was 8.34% better than the oil sand case, but is still low without explanation.
All the previous flow experiments were done in the glass columns, where there was no confining stress
applied to the sandpack. The confining stress helps keep the shape of the sandpack uniform and it will
eliminate any possibility of channeling along the sides of the column (between sandpack and column wall).
Hence, a second flow experiment with synthetic oil sand was designed using a high pressure core holder
with 500 psi confining stress. The flow properties of the sandpack was measured using; brine solution, at
the same salinity as the surfactant solution, was injected to saturate the pack with brine first and make these
measurements. The flow properties of the sand pack are listed in Table 5. It should be noted that these
properties correspond to the sand pack that is contains 13 wt.% bitumen.

Table 5—Properties of sandpack in flow experiments

10 SPE-190086-MS

The surfactant solution injection was started at 0.015 ml/min which is equivalent to 0.5 ft/day based on
initial porosity value. The injection continued for 5.44 PV and a total 1.66% OOIP was recovered. The
bitumen concentration in the produced m.e. was initially 17,000 ppm and fell to 3,000 ppm when injection
was stopped. The surfactant solution was shut–in for 24 hrs. once the outlet concentration was observed to
fall in an attempt to understand whether the contact time was negatively affecting solubilization. Injection
was started again at the same flow rate, and the bitumen concentration in the produced m.e. increased to
10,000 ppm as a result of the shut–in, but decreased to 5000 ppm after 1 PV additional surfactant injection.
Flow rate was increased to 0.03 ml/min (1 ft/day) again but no significant increase in bitumen concentration
was measured. The pressure drop and bitumen concentration for this experiment are shown in Figure 6.

Figure 6—Pressure drop and concentration with respect to pore volume of surfactant
solution injected for the synthetic oil sand flow experiment with 500 psig confining pressure.

In the previous studies that used coal tar as a model oil in lieu of bitumen, an extremely high flow rate
was used. In order to understand if the shear forces were affecting the mixing process in-situ, and thereby
affecting the degree of bitumen solubilization thus far, the flow rate was further increased to 0.15 ml/min
(5 ft/day). No significant increase in bitumen concentration was measured. Overall bitumen recovery from
the flow experiment was 5.75% OOIP.

Batch tests
Batch tests were planned after conducting the flow experiments and noting the low degree of bitumen
solubilization in produced microemulsions compared with phase behavior results, which resulted in low
bitumen recoveries. For these batch tests, 10 ml of the selected surfactant formulation (used for the flow
experiments) was mixed with 10g of oil sand. After tumbling and allowing the solids to settle, the liquid
phase (supernatant) was analyzed using GC. The theoretical maximum concentration based on complete
solubilization of the bitumen within the 10 g of oil sand was expected was 120,000 ppm. Instead, only 4,000
ppm concentration was observed in the liquid phase.
On visual examination of the test tube, it was observed that bitumen on the sand was washed–off from
the sand but it remained as a separate phase within the tubes. These separate phases can be observed in
SPE-190086-MS 11

Figure 7. Based on this observation, additional batch tests were performed with synthetic oil sand at varying
wt% oil. Table 6 lists the different combinations of surfactant solution/oil sands that were prepared, and
concentration of bitumen resulting in the aqueous phase. The amount of oil solubilized decreases as the
initial oil concentration increases. Interestingly, the phenomenon of bitumen separating from the sand and
creating a different phase was observed in the case of synthetic oil sand also, and can be observedin Figure 8.

Figure 7—Batch test result for oil sand mixed with 0.5% C20-24 IOS, 0.5% C13 13 PO sulfate,
1% 2-butanol and 0.5% sodium carbonate. Note the separated oil layer at the top of the sand.

Figure 8—Batch test tubes for 0.5% C20-24 IOS, 0.5% C13 13 PO sulfate, 1% 2-butanol and 0.5% sodium carbonate
mixed with synthetic oil sands as repoted in Table 6. Note the clean sand and separated oil layer above the sand.

Table 6—Compositions of test tubes for batch test with synthetic oil sand
12 SPE-190086-MS

Conclusions
The study investigated the feasibility of applying single phase microemulsions for recovery of bitumen
from oil sands. Previous experiments with coal tar suggested that reasonable recovery is possible using
single phase microemulsion with proper selection of surfactants. Similar studies were made for bitumen
extracted from field-obtained oil sands and suitable surfactants were selected. The surfactant formulation
selected for further study exhibited a high degree of bitumen solubilization, on the order of 300,000 ppm.
When the selected formulation was used in 1-D flow experiment with field-obtained oil sand, the bitumen
solubilization was much lower than expected. Additional flow experiments were conducted using synthetic
oil sands composed of clean quartz sand in order to limit the potential adverse effects of the sand/solids and
thereby help to understand the results of the flow experiment, yet recoveries were still very low. While the
evidence pointed to the solids, the cause for the low bitumen solubilization in these flow experiments was
not clear. Batch tests improved the understanding of the problem. They exhibited that bitumen is washed
off from the sand particles but it is not solubilized by the surfactant formulation. Preliminary investigation
of the oil aggregation in the batch tests suggested that the problem is related to the interaction between
silt particles within the sand and asphaltenes present in bitumen. Continued studies are being conducted to
better elucidate the cause and thus, guide the future design.

Acknowledgements
The authors would like to thank Division of Research, University of Houston for the financial support for the
work. The authors would also like to thank Sasol, Cytec and Shell for the surfactant samples provided for the
study. We would also like to thank Dr. Adry Bissada and his group in the Center for Petroleum Geochemistry,
Department of Earth and Natural Sciences at the University of Hosuton for the SARA analysis work.

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