Th B07

Alkali and Surfactant Consumption in Sandstone

Outcrop Rocks
E. van den Pol* (Shell Global Solutions International B.V.), C.H.T. van Rijn
(Shell Global Solutions International B.V.) & J.G. Southwick (Shell Global
Solutions International B.V.)

SUMMARY
In developing a chemical EOR formulation, core floods are carried out to test the performance of the
formulation. Outcrop rocks are often used, but their properties are very different from reservoir rocks. The
mineralogy and the amount and types of clay present can be substantially different. Clays increase the
surface area of the rock and the cation exchange capacity (CEC). It is generally assumed that reservoirs
with more clay require increasing volumes of chemicals. Therefore, it is important to use an outcrop rock
that behaves similar to the reservoir rock to obtain an accurate assessment of project economics.
In this paper different outcrop sandstone rocks were studied and compared to a reservoir rock. Alkali
surfactant consumption tests were performed in these rocks. The alkali consumption increased with
increasing CEC as expected, but surfactant adsorption was constant for the different rocks in the presence
of alkali. Without alkali, the surfactant adsorption increased significantly and was found to be dependent
on CEC. Bandera Brown outcrop rock was discovered to be a relatively close mimic to a reservoir rock of
interest and it gives a more realistic estimate of oil recovery and the amount of chemical required for a
field project

IOR 2015 – 18th European Symposium on Improved Oil Recovery

Dresden, Germany, 14-16 April 2015
Introduction

To test the performance of an enhanced oil recovery (EOR) formulation, core floods are being
performed in the laboratory. Because reservoir rock material is often only available in a limited
amount, outcrop rocks are typically used for most of the experiments. Also, the state of reservoir core
material is often an uncertainty. However, the properties of outcrop rocks can be very different from
the reservoir rock and different results are often obtained. In this paper several sandstone outcrop
rocks were studied to identify an outcrop rock that better matches the reservoir rock experiments.

One of the important differences between rocks is the mineralogy and specifically the amount and
type of clays. Clays increase the surface area of the rock and the cation exchange capacity (CEC). Ion
exchange will occur if the injection brine is different in ionic composition from the reservoir brine
(Hill et al. (1977), Appelo and Postma (2007)). When relatively fresh brine is injected in EOR
processes, ion exchange will determine the concentration of divalent cations present in solution.
Divalent cations can have a negative impact on surfactants, will lower solution viscosity for most
EOR polymers, and can precipitate with alkali (Glover et al. (1979), Nelson (1981)).

Chemical consumption is an important factor in the economics of alkaline surfactant polymer (ASP)
and surfactant polymer (SP) flooding (Solairaj (2012)). Alkali is often added to reduce the adsorption
of anionic surfactants on the rock surface by making the surface more negatively charged (Nelson et
al. (1984), Bae and Petrick (1977)). It is generally assumed that reservoirs with an increased rock
surface area and CEC require increasing volumes of chemicals (Somerton (1983), Sheng (2011)).
Therefore, it is important to use an outcrop rock that has similar behaviour to the reservoir rock during
core floods.

In this study, the mineralogy of the rocks was studied by X-Ray Diffraction (XRD). To get
information on the ion exchange capacity, CEC measurements were done. Dynamic alkali surfactant
(AS) consumption tests were performed to look at the effect the mineralogy has on the chemical
consumption. Oil displacement core floods were run to confirm differences and similarities between
some outcrop rocks and a reservoir rock.

Experimental

Rock analysis
The mineralogy was determined by X-ray diffraction (XRD) which was carried out by JM Huggett
Petroclays. To determine the ion exchange properties, CEC measurements were performed in our
laboratory. Since clays have quite different surface areas, also BET (Brunauer Emmett Teller) surface
area measurements using Krypton were carried out in-house. These samples were pre-treated at 150
°C in vacuum for 4 hours.

Core flooding
The brine contained 5822 ppm Na+, 11.7ppm Ca2+ and 8.7 ppm Mg2+. The AS composition was
0.48% alkyl propoxy (7 PO) sulfate (APS), 0.12% internal olefin sulfonate C15-18 (IOS), 2% Na2CO3
and 1.8% NaCl. The surfactants are Shell Chemicals ENORDETTM H771/J771 and O332 respectively
(Barnes et al. (2008), Barnes et al. (2010)). This is a system that develops low interfacial tension with
the oil. In the oil displacement corefloods also Flopaam 3330 polymer from SNF was added.
Reservoir crude oil with a low TAN was used in all experiments. The experiments were performed at
52 °C using an injection rate of 3 ft/day. The outcrop cores were 5 × 30 cm and the reservoir core
consisted of 3 stacked cores with total dimensions of 3.7 × 17 cm. The cores were mounted vertically
and injection occurred from the bottom.

For the AS consumption tests, 10 pore volumes (PV) of brine injection was followed by 3 PV AS
injection and finished with 3 PV brine injection. A tracer (potassium hexacyanocobaltate (III), 10 ppm
Co) was added to the AS slug which is assumed to have no interaction with the rock. This tracer was

IOR 2015 – 18th European Symposium on Improved Oil Recovery

Dresden, Germany, 14-16 April 2015
used to detect the front of the AS slug and to determine the delay in breakthrough of the surfactant
and alkali.

During the experiment, the pressure drop was measured and the pH and redox potential were
measured inline. The effluent was collected using a fraction collector. The effluent was later analyzed
for the Co-tracer and ion concentrations using Inductively Coupled Plasma (ICP). Titration using a
Metrohm Titrando 836 equipped with a Metrohm 815 robotic USB sample processor was performed
to determine surfactant and alkali concentrations. Surfactant was titrated with Tegotrant A100 and
alkali was titrated with 0.1N sulfuric acid. Sodium carbonate (alkali) titration gives two end points,
one at a pH around 8.5 when carbonate is converted to bicarbonate and one around pH 4.5 when
bicarbonate is converted to carbonic acid. This will then give values for ‘Total alkalinity’ (carbonate +
bicarbonate) and ‘Strong alkalinity’ (carbonate). More detailed surfactant analysis was done by liquid
chromatography-mass spectrometry (LCMS) (van der Lee et al. (2015)).

For oil displacement core floods the core was first saturated with brine, followed by oil injection and
then a waterflood. After the waterflood, the ASP flood was performed with a 0.5 PV ASP slug
followed by a polymer drive with lower salinity than the ASP slug.

Results

Rock analysis
XRD results are shown in Table 1 (total) and 2 (clay fraction). For the reservoir rock ranges are
shown because of the heterogeneity found across different samples.

Table 1 XRD results of the different rocks (mass fraction, tr=trace).

Illite-smectite
Illite & mica

Fe dolomite
Plagioclase
K feldspar
illite-rich

Kaolinite

Ankerite

Gypsum
Chlorite

Siderite
Calcite
Quartz
Rock

Berea 2 1 6 tr 86 3 1 1 0 0 0 0
Boise 4 1 0 0 76 9 9 1 0 1 0 0
Sister Grey 2 0 5 1 89 2 1 0 0 0 0 tr
Bandera Brown 2 1 3 1 87 0 4 tr 0 1 tr 0
Reservoir 1-4 tr-3 tr 0 86-96 0-2 0-2 0-1 0-5 0 0 0-1

Table 2 XRD of the clay fraction.

Total clay (%)

Illite-smectite

Illite-smectite
smectite rich

Vermiculite
illite-rich

Kaolinite
Chlorite
Rock

Illite

Berea 9 47 8 0 0 15 30
Boise 5 6 0 91 0 1 1
Sister Grey 8 56 11 0 0 6 27
Bandera Brown 7 38 3 0 36 2 21
Reservoir 1-7 58-75 18-22 0 0 1-7 3-15

IOR 2015 – 18th European Symposium on Improved Oil Recovery

Dresden, Germany, 14-16 April 2015
The different mineralogies lead to different properties such as the CEC. The measured CEC values are
shown in Table 3, together with the surface area.

Table 3 CEC and surface area.

Rock CEC Surface area CEC
(meq/100g) (m2/g) (meq/m2, ×10-3)
Berea 0.24 1.54 1.55
Boise 0.39 N/A N/A
Sister Grey 0.21 1.39 1.52
Bandera Brown 1.08 8.3 1.3
Reservoir 1.25 8 1.6

Table 4 CEC and surface area of clays (Appelo and Postma (2007) and Farrell).
Clay CEC (meq/100 g) Surface area (m2/g)
Smectite 80-120 650-800
Vermiculite 100-200 600-800
Kaolinite 3-15 10-30
Illite 20-50 70-175
Chlorite 10-40 70-100

The CEC per unit weight of rock is mainly determined by the surface area; as can be seen the CEC in
meq/m2 is fairly constant. Bandera Brown contains a significant amount of vermiculite which is a
large surface area clay with a high CEC (Table 4), explaining the large values found for that rock.
Berea and Sister Grey have mainly illite and kaolinite which have a smaller CEC and surface area and
indeed smaller values are found for these rocks. Boise rock is an intermediate case: the total clay
content is lower but it is smectite rich.

For the reservoir rock it is not clear from the mineralogy why the surface area and CEC are so large.
In reservoir rock, more parameters might play a role, like oil components or contamination. Also,
surface mineralogy can be very different from bulk mineralogy (Suijkerbuijk et al. (2013)).

Chemical consumption, Alkali Surfactant

The results of the chemical consumption experiments in Berea and Bandera Brown outcrop rock are
shown in Figures 1 and 2. On the x-axis the injected PV’s are shown, on the left y-axis the
concentration of chemicals compared to the injected concentration and on the right y-axis the pH.
After about 1 PV the front of the AS slug breaks through as seen by the tracer signal going from 0 to
100%. The 3 PV AS slug can be recognized in the produced tracer profile as it is 3 PV wide.

It can be seen that the total alkalinity front is delayed in the Bandera Brown experiment but not in
Berea. Also, the strong alkalinity consumption clearly is higher in Bandera Brown compared to Berea.
Interestingly, the surfactant retention was found to be about the same for both experiments.

These experiments were also performed with the other rocks. The retention was calculated from the
difference between the tracer front (at 50% breakthrough) and the front of the chemical (at 50%
breakthrough). From the delay in PV the retention in mg/100g rock was then calculated. The results of
the experiments with the different rocks are shown in Table 5 and plotted in Figure 3.

IOR 2015 – 18th European Symposium on Improved Oil Recovery

Dresden, Germany, 14-16 April 2015
 Adsorption in Berea
120 12

100 10

80 Surfactant, Alkali, Tracer (C/C0, %) 8

60 Surfactant 6

pH
Strong Alkalinity

40 Tracer 4
Total Alkalinity

20 pH 2

0 0
0 1 2 3 PV 4 5 6

Figure 1 Chemical consumption in Berea outcrop rock, low CEC (brine permeability 90 mD).

Adsorption in Bandera Brown 
120 12

100 10
Surfactant, Alkali, Tracer (C/C0, %)

80 8

60 6
Surfactant

Strong Alkalinity pH
40 Tracer
4

Total Alkalinity

20 pH 2

0 0
0 1 2 3 PV 4 5 6

Figure 2 Chemical consumption in Bandera Brown outcrop rock, high CEC (brine permeability 20
mD).

Table 5 Chemical retention in different rocks.

Rock Surfactant retention Strong alkali consumption
Δ PV mg/100g rock Δ PV mg/100g rock
Berea 0.29 16 0.10 19
Boise 0.22 13 0.21 63
Sister Grey 0.20 12 0.14 28
Bandera Brown 0.26 16 0.64 130
Reservoir 0.19 17 0.34 101

IOR 2015 – 18th European Symposium on Improved Oil Recovery

Dresden, Germany, 14-16 April 2015
 Chemical loss vs. CEC of rock
140

120 Surfactant
Chemical loss (mg/100 g rock)

Bandera Brown
100
Alkali
Reservoir
80

60
Boise
40

20 Berea
Sister Grey

0
0 0.2 0.4 0.6 0.8 1 1.2 1.4
CEC (meq/100 g rock)

Figure 3 Chemical retention versus CEC, AS consumption tests.

The strong alkali consumption increased with increasing CEC. This was expected since rocks with
higher CEC have a larger surface that consumes alkali by ion exchange and other surface mineral
reactions. Also, the calcium ions that are exchanged with sodium ions will be precipitated as calcium
carbonate, thereby consuming alkali.

Surprisingly, the surfactant adsorption was found to be fairly constant for all the rocks, even the
reservoir rock (after extensive flush cleaning to remove oil contaminants). Apparently, with the 2%
sodium carbonate added, the surfactant retention was reduced to a fixed baseline level. All divalent
cations were precipitated (as confirmed by ICP measurements) and the pH was sufficiently high to
ionize the rock surface.

Although the total surfactant retention was comparable for all rocks, more chromatographic separation
between individual components of the APS surfactant was observed with Bandera Brown rock
compared to Berea and Sister Grey rock, see Figure 4 (for more details: van der Lee et al. (2015)). For
the Bandera Brown rock it was observed that surfactant components with increasing number of PO
groups (more hydrophobic) were more retained in the core. For the IOS surfactant components no
chromatographic separation was observed. For Bandera Brown a slight difference in APS retention
compared to IOS retention was observed (Figure 5), although the signal above 100% is a bit
suspicious. Sister Grey does not show any difference between APS and IOS.

A change in the surfactant composition can potentially cause a formulation to go from optimum to
over- or under-optimum. However, in this case the components lagging behind are only a small
fraction of the total composition and no severe impact is expected. Highly performing core floods
with this formulation in Bandera Brown core confirm that the differential adsorption of APS
components did not negatively affect oil recovery (Southwick et al. (2014)). It is also possible that
this differential adsorption does not occur when oil is present, which is a subject for further study.

Chemical consumption, surfactant only

To verify the expected trend of surfactant retention with CEC, two chemical consumption tests were
performed without alkali. The tests were done in Berea and Bandera Brown outcrop rock. The results
are plotted in Figure 6 (blue squares).

IOR 2015 – 18th European Symposium on Improved Oil Recovery

Dresden, Germany, 14-16 April 2015
 Sister Grey, H771 Bandera Brown, H771
120 120

100 100

80 80
C12‐3PO‐SO4 C13‐2PO‐SO4

% of AS injected
% of AS injected

C12‐4PO‐SO4 C13‐3PO‐SO4 C12‐3PO‐SO4 C13‐2PO‐SO4

C13‐4PO‐SO4 C14‐3PO‐SO4 C12‐4PO‐SO4 C13‐3PO‐SO4
C12‐5PO‐SO4 C13‐5PO‐SO4 C13‐4PO‐SO4 C14‐3PO‐SO4
60 C14‐4PO‐SO4 C12‐6PO‐SO4 60 C12‐5PO‐SO4 C13‐5PO‐SO4
C12‐7PO‐SO4 C13‐6PO‐SO4 C14‐4PO‐SO4 C12‐6PO‐SO4
C14‐5PO‐SO4 C12‐8PO‐SO4 C12‐7PO‐SO4 C13‐6PO‐SO4
C13‐7PO‐SO4 C14‐6PO‐SO4 C14‐5PO‐SO4 C12‐8PO‐SO4
40 C12‐9PO‐SO4 C13‐8PO‐SO4 40 C13‐7PO‐SO4 C14‐6PO‐SO4
C14‐7PO‐SO4 C12‐10PO‐SO4 C12‐9PO‐SO4 C13‐8PO‐SO4
C13‐9PO‐SO4 C14‐8PO‐SO4 C14‐7PO‐SO4 C12‐10PO‐SO4
C12‐11PO‐SO4 C13‐10PO‐SO4 C13‐9PO‐SO4 C14‐8PO‐SO4
C14‐9PO‐SO4 C12‐12PO‐SO4 C12‐11PO‐SO4 C13‐10PO‐SO4
20 C13‐11PO‐SO4 C14‐10PO‐SO4 20 C14‐9PO‐SO4 C12‐12PO‐SO4
C12‐13PO‐SO4 C13‐12PO‐SO4
C12‐14PO‐SO4 C13‐13PO‐SO4 C13‐11PO‐SO4 C14‐10PO‐SO4
C13‐14PO‐SO4 C12‐13PO‐SO4 C13‐12PO‐SO4
C12‐14PO‐SO4 C13‐13PO‐SO4
0 0
0 1 2 PV 3 4 5 0 1 2 PV 3 4 5

Figure 4 Chromatographic separation of the APS surfactant in Sister Grey and Bandera Brown rock.
The surfactant concentration is plotted as percentage of the injected AS composition. Darker red
colour indicates fewer PO groups.

Sister Grey, APS / IOS retention Bandera Brown, APS / IOS retention
120 120

100 100

80 80
% of AS injected
% of AS injected

60 60
H771 H771
O332 O332
40 40

20 20

0 0
0 1 2 PV 3 4 5 0 1 2 PV 3 4 5

Figure 5 Chromatographic separation between (the weighted average of) the APS (H771) and the
IOS (O332) surfactant in Sister Grey and Bandera Brown rock.

Surfactant loss vs. CEC of rock
140

No alkali
120
Surfactant loss (mg/100 g rock)

No alkali, no calcium
100 With alkali

80
Bandera Brown
60

40
Berea
20

0
0 0.2 0.4 0.6 0.8 1 1.2 1.4
CEC (meq/100 g rock)

Figure 6 Surfactant retention versus CEC, S versus AS consumption tests.

IOR 2015 – 18th European Symposium on Improved Oil Recovery

Dresden, Germany, 14-16 April 2015
Without alkali, the expected trend of increasing surfactant retention with CEC was indeed observed.
The surfactant retention for Berea increased by a factor of almost 3 compared to AS, while for
Bandera Brown this was a factor of 6. This indicates that adding alkali is more important for high
CEC rocks than for low CEC rocks. It should be realized though that more alkali is needed in the case
of a high CEC rock since more of the alkali will be consumed.

In addition to the increased surfactant retention, the chromatographic separation of the APS surfactant
also increased, compare Figure 7 to Figure 4. The impact of this needs to be studied further. There
was no separation observed between the APS and IOS surfactants.

As presented in two other papers (Southwick et al. (2014), van den Pol et al. (2014)) the surfactant
retention of this surfactant system is strongly dependent on the calcium divalent ion concentration.
Without alkali present but with the calcium ions removed by a long NaCl preflush, the surfactant
retention in Bandera Brown went down from 98 to 40 mg/100 g rock (Figure 6, red diamond). This
suggests that removing divalent ions from solution is an important function of the alkali. Multivalent
ions can significantly reduce the solubility of surfactants. Furthermore, they decrease the electrostatic
repulsion between the negatively charged surfactant and the negatively charged rock surface and they
might form an ionic bridge between the surfactant and the surface.

Bandera Brown, S only, H771
120

100
C13‐2PO‐SO4 C12‐3PO‐SO4
C12‐4PO‐SO4 C13‐3PO‐SO4
C14‐3PO‐SO4 C12‐5PO‐SO4
80 C13‐4PO‐SO4 C12‐6PO‐SO4
% of AS injected

C14‐4PO‐SO4 C13‐5PO‐SO4
C12‐7PO‐SO4 C14‐5PO‐SO4
C13‐6PO‐SO4 C12‐8PO‐SO4
60 C13‐7PO‐SO4 C14‐6PO‐SO4
C12‐9PO‐SO4 C13‐8PO‐SO4
C14‐7PO‐SO4 C12‐10PO‐SO4
C13‐9PO‐SO4 C14‐8PO‐SO4
40 C12‐11PO‐SO4 C13‐10PO‐SO4
C14‐9PO‐SO4 C12‐12PO‐SO4
C13‐11PO‐SO4 C14‐10PO‐SO4
C12‐13PO‐SO4 C13‐12PO‐SO4
20 C12‐14PO‐SO4 C13‐13PO‐SO4
C13‐14PO‐SO4 C13‐15PO‐SO4
tracer

0
0 1 2 PV 3 4 5

Figure 7 Chromatographic separation of the APS surfactant in Bandera Brown rock, S only.

Oil displacement tests

From the CEC and chemical consumption data Bandera Brown rock was identified as the best match
for the reservoir rock. To further compare Berea and Bandera Brown outcrop rock to our reservoir
rock, oil displacement core flood experiments were conducted. The Berea results are shown in Figure
8, Bandera Brown in Figure 9 and Reservoir rock in Figure 10. Oil production is shown as percentage
of remaining oil after waterflood (Sor).

Clearly, the results of the Bandera Brown experiment better match the Reservoir rock compared to the
Berea experiment. The oil cut and oil production are more similar as is the chemical consumption.
This confirms the identification of Bandera Brown outcrop rock to resemble this reservoir rock.

IOR 2015 – 18th European Symposium on Improved Oil Recovery

Dresden, Germany, 14-16 April 2015
 Berea ‐ oil displacement
120 12

Oil cut, Oil production (%Sor), Surfactant, Alkali, Polymer (C/C0,%)
100 10

80 8

pH
60 6

Oil production
Oil cut
40 Surfactant 4
Polymer
Strong alkalinity
20 Total alkalinity 2
pH

0 0
0.0 0.5 1.0 PV 1.5 2.0 2.5 3.0

Figure 8 Oil displacement test in Berea outcrop rock (brine permeability 68 mD).
Bandera Brown ‐ oil displacement
120 12
Oil cut, Oil production (%Sor), Surfactant, Alkali, Polymer (C/C0,%)

100 10

80 8

pH
60 6

Oil production
Oil cut
40 Surfactant 4
Polymer
Strong alkalinity
20 Total akalinity 2
pH

0 0
0.0 0.5 1.0 PV 1.5 2.0 2.5 3.0

Figure 9 Oil displacement test in Bandera Brown outcrop rock (brine permeability 19 mD).
Reservoir rock ‐ oil displacement
120 12
Oil cut, Oil production (%Sor), Surfactant, Alkali, Polymer (C/C0,%)

100 10

80 8
pH

60 6

Oil production
Oil cut
40 Surfactant 4
Polymer
Strong alkalinity
20 Total alkalinity 2
pH

0 0
0.0 0.5 1.0 PV 1.5 2.0 2.5 3.0

Figure 10 Oil displacement test in Reservoir rock (brine permeability 188 mD).
IOR 2015 – 18th European Symposium on Improved Oil Recovery
Dresden, Germany, 14-16 April 2015
Conclusions

Different sandstone outcrop rocks were tested and compared to a reservoir rock. Alkali surfactant
consumption tests showed that the alkali consumption increased with increasing CEC as expected.
However, the surfactant retention was found to be constant for the different rocks in the presence of
2% w/w sodium carbonate (~15 mg/100 g rock). This is thought to be because the alkali provided a
sufficiently high pH to ionize the rock and the concentration was high enough to precipitate all
divalent ions. When no alkali was used, the surfactant retention increased by a factor 3-6 and was
dependent on CEC.

The Bandera Brown rock was found to be a relatively close mimic to the reservoir rock of interest.
Experiments showed that this is a much closer match than Berea sandstone which is typically used in
chemical flood formulation development. Both Bandera Brown and the reservoir rock have a large
CEC and showed large alkali consumption. Oil displacement experiments confirmed the comparable
behaviour by having a similar amount of oil (remaining after water flood) produced by the chemical
flood. Use of Bandera Brown sandstone gives a more realistic estimate of oil recovery and the amount
of chemical required for a field project.

Acknowledgements

We thank Fons Marcelis and Ab Coorn for drilling and characterizing outcrop cores, Merit van der
Lee for LCMS measurements and Diederik van Batenburg for stimulating discussions. We also wish
to thank Shell for their permission to publish these results.

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Dresden, Germany, 14-16 April 2015