DC191801 DOI: 10.

2118/191801-PA Date: 21-October-19 Stage: Page: 1 Total Pages: 14

Investigation of the Interaction of

Surfactant at Variable Salinity with
Permian Basin Rock Samples: Completion
Enhancement and Application for
Enhanced Oil Recovery
Kang Han Park and David S. Schechter, Texas A&M University

Summary
Adding a surfactant to completion fluids has been widely applied to improve the initial oil production from unconventional liquid reser-
voirs (ULRs). However, very limited research has been conducted to understand the interactions between surfactants and salt in ULRs,
and to identify the effect of f-potential (ZP), interfacial tension (IFT), and contact angle (CA) on oil recovery through surfactant/
salt-assisted spontaneous imbibition (SSASI). This study investigates the interactions of surfactant and salinity in different ULR
lithologies in west Texas (WT), USA, and determines the relationship between the experimental parameters and oil recovery to provide
potential screening criteria for completion-fluid design.
With the combination of numerous chemicals at different concentrations and nine salinity levels, more than 50 variations of
aqueous-phase solution were blended. Also, heterogeneous ULR rock samples of the WT formation with two different dominant lithol-
ogies, quartz-rich (WT QR) and carbonate-rich (WT CR), were selected. All combinations of fluid were used for ZP, IFT, and CA
measurements, and some were selected for SSASI experiments with timely computed-tomography (CT) scans. Then, all experimental
results were plotted against the oil recovery factor (RF) to determine the most impactful parameter on oil recovery and to obtain knowl-
edge regarding desired conditions of salinity for surfactant-added completion fluid.
The effect of salinity on ZP, IFT, and CA had a similar trend for all fluid cases. With increasing salinity, the magnitude of ZP
decreased to nearly 0 mV, meaning either a thin electrical double layer (EDL) or none surrounding the rock particles. Surfactant and
salt reduced IFT strongly until it reached the critical salt concentration (CSC) of 30,000 ppm, and then reduction occurred gradually
and slowly. Surface wettability was different for the two rock types, and the ability to alter wettability varied by the condition of
fluids. Wettability alteration occurred with the presence of both surfactant and salt, but most effectively at salinity between 20,000 and
30,000 ppm. Also, the wettability of the quartz-rich rock type showed more water-wetting surface compared with the carbonate-rich rock
type. Out of all the experimental parameters, CA showed the strongest effect on oil recovery. Only 5 to 10% of the oil was produced when
the rock surface was oil-wet, but the oil recovery increased up to 25% when the surface became intermediate-wet. Finally, when the rock
surface became water-wet, 25 to 40% of the oil was produced from SSASI. Consequently, on the basis of this investigation of surfactant/
salt interactions, we determined the salinity of 20,000 to 33,000 ppm to be the most favorable condition for salt/surfactant-added comple-
tion fluids, which effectively reduces IFT and yields the strongest wettability alteration.
Understanding the interactions between salt and surfactant and their behaviors in different types of reservoirs is essential when ana-
lyzing the reusability or dilution of high-salinity produced water and successfully designing completion fluids for ULRs. The signifi-
cance of this study is the ability to determine the most synergetic condition of blended-salt/surfactant solutions and identify the
parameter with the greatest impact on oil recovery in ULRs to provide surfactant-screening criteria. Furthermore, we demonstrate eco-
nomic and environmental benefits by using produced water and fresh water for completion activities.

Introduction
ULRs have been the main contributor to the energy independence of the US, despite ultratight and heterogeneous formations. In 2017,
the US Energy Information Administration predicted tight oil production to increase by more than 6 million B/D by 2040, which will
comprise approximately 60% of total crude production domestically (EIA 2017). Among various major shale plays, the southwest
region, with the help of the Permian Basin, is forecast to contribute the most production of tight oil.
Undoubtedly, the combination of horizontal drilling and hydraulic fracturing led to the significant increase in production from ULRs
during recent years. With the advanced technology of drilling and hydraulic fracturing, a larger contact area throughout the pay zone
can be accessed and developed, generating permeable fractures and leading to more-economical and -commercial production rate of
hydrocarbons (Pankaj and Kumar 2010; Moniz et al. 2011; Mohamed et al. 2015). Developing effective completion strategies for an
increasing number of horizontal wells in ULRs has been one of the most important, and most challenging, factors.
The presence of surfactant in the aqueous-phase stimulation fluids is believed to have the ability to enhance the initial peak produc-
tion rate in ULRs. Surfactants are effective in reducing the IFT between crude-oil and aqueous-phase solutions and altering wettability.
Spontaneous imbibition, which is driven by the two main mechanisms of buoyancy and capillarity, is heavily dependent on IFT and sur-
face wettability. Primarily using ZP, IFT, CA, and surfactant-assisted spontaneous imbibition (SASI), numerous active experimental
and modeling studies have been conducted to determine the effect of surfactant on improving the estimated ultimate recovery of major
US shale plays such as Bakken, Eagle Ford, Barnett, and Wolfcamp. Authors were able to observe significant increases in oil production
with surfactant-mixed solutions (Alvarez et al. 2014, 2017a, 2017b, 2017c; Alvarez and Schechter 2016a, 2016b, 2017; Neog and
Schechter 2016; Saputra and Schechter 2018; Zhang et al. 2018a, 2018b, 2018c). IFT reduction occurred with the presence of surfactant

Copyright V
C 2019 Society of Petroleum Engineers

This paper (SPE 191801) was accepted for presentation at the SPE Liquids-Rich Basins Conference—North America, Midland, Texas, USA, 5–6 September 2018, and revised for publication.
Original manuscript received for review 28 March 2019. Revised manuscript received for review 29 July 2019. Paper peer approved 31 July 2019.

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until the latter reaches the critical micelle concentration regardless of the ionic charges, and wettability alteration was observed to be
effective with increasing surfactant concentration. Although the interactions between surfactants and rocks were determined to be dif-
ferent for various shale plays with different petrophysical and reservoir properties, all ULRs showed higher estimated ultimate recovery
with surfactant-added aqueous-phase solutions compared with regular water without additives. However, despite the increasing interests
of investigation and field application for SASI in ULRs, most studies were conducted using distilled water or brines with negligible or
no salinity, which does not provide understanding regarding the interactions of surfactant, salt, and rock; as a result, insufficient studies
are available on the prolific shale plays of WT.
In addition, increasing hydraulic-fracturing activities throughout the US has ignited concerns for rising water demand and the high
volume of produced water. Between 2012 and 2014, 17.5 billion gal/yr of water was used throughout the major onshore shale plays,
whereas nearly double the amount of flowback-produced water (FPW) was observed (Kondash and Vengosh 2015). FPW is an inevita-
ble mixture of both formation water and injected water from waterflooding or hydraulic fracturing, and contains high salinity and other
naturally occurring minerals. It requires costly treatment or disposal using saltwater-disposal wells and has been one of the most prob-
lematic issues for Permian and Bakken operators during exploration and production (Whitfield 2017). Many researchers analyzed the
possible reusability of treated FPW for waterflooding or spontaneous imbibition and determined that low salinity yields more final oil
recovery and more-water-wet surface from conventional sandstone and nonreservoir rocks (Morrow and Mason 2001; Khanamiri et al.
2015; Li et al. 2016; Valluri et al. 2016; Wilson 2016). Valluri et al. (2016) analyzed the individual effects of monovalent and divalent
brines on enhanced oil recovery (EOR) from a ULR in southeast Texas and concluded that the performance of brines differs with types
and concentration of salt, whereas lower salt concentration for each salt leads to more-water-wet surface and higher oil recovery.
Although these studies showed the effect of salinity in brine for various operation and completion strategies, there have been only very
limited studies to understand the effect of salinity on unconventional rocks, especially the interactions between salt and surfactant in
aqueous-phase completion fluids when applied during hydraulic fracturing in ULRs.
This study attempts to intensively analyze the interactions of surfactant, salt, and two dominant rock types of a WT ULR to deter-
mine the most favorable salinity condition for the surfactant-added aqueous-phase stimulation fluids. Surfactants with various properties
(i.e., ionic charges, components, or fluid properties) are selected for ZP, IFT, CA, and SSASI experiments to observe the behavior and
trend of each surfactant at different salt concentration, along with regular water with no chemical or salt additives. In addition, by
analyzing the experimental parameters of more than 50 variations of aqueous-phase solution and correlating them to the final oil recov-
ery, this study provides empirical evidence of the highest contributing parameter for improving the performance of completion fluid
and enhancing oil recovery from a ULR. Ultimately, this study aims to present potential guidance to use a large volume of treated high-
salinity FPW with fresh water as the fracturing fluid, generating both economic and environmental benefits for the oil and gas industry.

Materials
ULR Rock. Sidewall cores that were approximately 1 in. in diameter and 2 to 2.5 in. long were extracted from a WT ULR, with the reser-
voir temperature of 155 F (68.2 C). These rock samples were classified into two main rock types according to their distinct physical dif-
ferences: WT CR and WT QR. WT CR contained small white calcite blocks within the core, showing extreme heterogeneous properties
with higher rock density, whereas WT QR displayed a more homogeneous condition, with a darker color. Further descriptions of each
lithology are provided in Table 1. In addition, original samples were trimmed into cylindrical shapes for accurate volumetric calculations.
Using the debris and chips from the trimming process, rock particles and rock chips were also generated for ZP and CA experiments.

Rock Types
Mineral (wt%) WT CR WT QR
Quartz 37.6 48.8
Calcite 14.9 1.9
Mica 19.9 22.2
Plagio 7.5 7.9
Dolomite 7.6 3.7
Smectite 3.9 4.4

Table 1—Average lithological compositions of the two rock types.

A temperature-driven aging process with crude oil was applied to both rock chips and core samples to restore the initial reservoir
condition. Rock chips were stored under the reservoir temperature of 155 F for more than 2 weeks, and core samples for more than
2 months, to restore any hydrocarbon lost during the coring or storing process. To minimize the variables, these core samples were
assumed to be 100% saturated with oil (So ¼ 100% or unity).

Crude Oil. Crude oil used for this investigation was extracted from the same formation, as the core samples, with the reservoir temper-
ature of 155 F; the crude samples were brown to dark brown in color at room conditions. The density of oil was measured to be 0.77 g/cm3
at reservoir temperature and the oil gravity was 41.6  API; thus, it is classified as black oil. This same oil was used throughout this investiga-
tion for all experiments and for both rock types.

Surfactant. Five chemical additives were selected for this study that contained various ionic charges, components, and physical fluid
properties. All chemicals were compared with each other and with water without chemical additives (as a control) to analyze the per-
formance improvements of each solution. Most surfactants were composed of nonionic, anionic, or both charged compounds. More-
detailed information with nomenclature is shown in Table 2. For this study, all five chemical additives were blended at a constant con-
centration of 1 gal/1,000 gal, but with various salinity levels to analyze the salinity effect on surfactant-added aqueous-phase solutions.

Brine/Salt. On the basis of the water reports from the WT field, we synthesized the laboratory brine to accurately represent the water
injected or produced in the field. The average total dissolved solids of injected water and produced water were 26,800 and 94,000 ppm,

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respectively. Both types of water contained the same primary ionic compounds, which are calcium, magnesium, sodium (Na), chloride
(Cl), sulfate, and bicarbonate. Among all, Cl– occupied nearly 60% of total compounds, followed by Naþ with nearly 37%. On the
basis of the types of cations and anions, we selected and used five salts to formulate the synthetic brine: sodium chloride, calcium chlo-
ride, magnesium chloride, sodium sulfate, and sodium bicarbonate. The composition of each salt was calculated using the injected-
water analysis, as displayed in Table 3. Using this salinity of 26,800 ppm as a standard, nine multipliers were applied to generate nine
variations of salinity for brines used in this investigation, as shown in Table 4. With six surfactants listed and nine salinity levels, a
total of 54 cases was tested to analyze the interaction between surfactant and salt on two types of rock.

Surfactant Name Code Type

Nanotechnology fluid NF Nanofluid
Surfactant 01 S01 Nonionic/anionic
Surfactant 02 S02 Nonionic/anionic
Surfactant 03 S03 Nonionic/anionic
Surfactant 04 S04 Nonionic/anionic

Table 2—Key characteristics of chemical additives.

Synthetic Brine
TDS (ppm) %
NaCl 24,350 90.84
CaCl2 1,330 4.97
NaHCO3 530 2.00
MgCl2 380 1.42
Na2SO4 210 0.77
TDS 26,800 100.00

Table 3—Salt composition of the synthetic brine. NaCl 5 sodium

chloride; CaCl2 5 calcium chloride; NaHCO3 5 sodium bicarbonate;
MgCl2 5 magnesium chloride; Na2SO4 5 sodium sulfate; TDS 5 total
dissolved solids.

Case Multiplier TDS (ppm)

1 0 0
2 0.25 6,700
3 0.5 13,400
4 0.75 20,100
5 1 26,800
6 1.25 33,500
7 1.5 40,200
8 2 53,600
9 3 80,400

Table 4—Variations of salinity for brine used in the investigation.

TDS 5 total dissolved solids.

In addition to the salts listed, potassium iodide (KI) was used in this investigation as a doping agent for the SSASI experiment to
enhance the contrast of aqueous-phase solutions during CT scans. Throughout years of experiments, 4 wt% of KI was determined to be
the optimal concentration for enhancing image contrast while not affecting any property of aqueous-phase solutions. This concentration
was used for all SSASI experiments, and more-detailed procedures are explained in later sections.

Experimental Procedures
ZP. ZP determines the stability of the liquid film surrounding the rock particles, which is also known as an EDL. Using a commercial
zeta potential and particle size analyzer, the electrophoretic mobility of particles in solution was measured with the phase-analysis
light-scattering technique. Rock samples, both CR and QR, from WT were crushed and sieved through ASTM E-11 #325 mesh.
Aqueous-phase solutions with various surfactants and salinity levels were formulated and triple filtered through a 0.2-mm polytetra-
fluoroethylene syringe filter to minimize possible contamination of the fluid. Then, a small amount of rock particles (less than 1 mg)
was added to the solution and sonicated for 1 minute at 40 Hz. After letting the sonicated solution sit at room conditions so that any
heavy particles in the system could settle, this sonicated fluid was placed in the device to measure ZP. The standard deviation of results
was kept to less than 3.00 mV, and all measurements were conducted at 70 F.

IFT. IFT experiments were conducted to analyze the effect of both surfactants and salt on reducing IFT between crude-oil and
aqueous-phase solutions, using a commercial optical contact-angle-measuring system with pendant-drop bottom-up method. The

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primary components of this device include drop-shape-analyzer (DSA) software, a heating plate, an image-capturing optical camera, a
temperature-controlling box, a temperature sensor, a dispensing unit, and a lighting source. The DSA software detects the shape and
volume of injected oil and manages the temperature-control and lighting unit. Fig. 1 shows a detailed schematic of the experimental
setup and an example screenshot of the DSA software when measuring IFT. The J-shaped capillary needle was used to dispense the oil
droplet upward because of lower density. All experiments were conducted under the reservoir temperature of 155 F, and the standard
deviation was maintained at less than 0.1 mN/m with at least 10 measurements for the accuracy of the average IFT for each fluid.

Aqueous-phase
solution

Crude oil Syringe

Oil drop
Capillary needle

Aqueous-
phase Oil droplet
solution
Capillary
needle

Fig. 1—(Left) Schematic of IFT measurements and (right) a sample screenshot of DSA software for IFT measurements.

CA. CA measurements were conducted to observe the wettability-alteration ability of surfactants and salinity. The same device used in
the IFT measurements was used with the captive-bubble method; an additional component, a rock-chip stand, was required. Rock sam-
ples, both CR and QR, were cut into small chips (approximately 1  1 cm) and polished well to have smooth surfaces for accurate mea-
surement of the static CA of crude-oil droplets on the rock surface. Because of extreme heterogeneity, rock chips were generated from
5 to 10 different depths for both rock types. As mentioned previously, rock chips were aged in crude oil under reservoir temperature for
more than 2 weeks to restore their original state. Aged rock chips were placed on top of the stand, and the entire system was submerged
in aqueous-phase solutions. A crude-oil drop was dispensed through the J-shaped capillary needle and placed carefully on the bottom
surface of the rock chip. Using the DSA software, the drop shape and the CA were measured, as shown in the detailed schematic and
sample screenshot of CA measurement in Fig. 2. All CA measurements were conducted at reservoir temperature, more than 10 mea-
surements were collected, and the standard deviation of the average static CA for all cases was kept at less than 5 .

Rock chip
Crude oil Syringe

Capillary
needle
Oil drop
Rock chip
Aqueous-
phase
solution
Oil droplet
Core-chip stand Aqueous-phase solution

Fig. 2—(Left) Schematic of CA measurements and (right) a sample screenshot of DSA software for CA measurements.

Spontaneous Imbibition with CT Scan. SSASI experiments were conducted after analyzing the results of ZP, IFT, and CA. The ULR
core samples were trimmed into cylindrical shapes and aged in crude oil under reservoir temperature for more than 2 months to restore
their initial conditions. All cores used in this experiment were assumed with 8% porosity and 100% oil saturation for mitigating varia-
bles. Modified Amott cells were used for SSASI, which are designed to hold a core immersed in an aqueous-phase solution throughout
the process and to measure the produced oil with the graduated tube at the top. The setup of SSASI was stored in an oven under reser-
voir temperature for at least 240 hours, or until the oil production stops if oil was still producing after 240 hours. In addition, cells were
scanned periodically using a multislice CT scanner throughout the experiment to observe the penetration of aqueous-phase solutions by
density change within the core. 4 wt% KI was added to the solutions as a doping agent to enhance the contrast during the image analyses.
Penetration magnitude (PM), established by Alvarez et al. (2014), was calculated to quantitatively observe the change of density. For the
volumetric, RF, and PM calculations, we used

Vcore ¼ ðp=4Þ  D2  L; . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . ð1Þ

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Vpore ¼ Vcore  porosity  So ; . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . ð2Þ

RFð%Þ ¼ Voil produced =Vpore  100; . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . ð3Þ

PM ¼ CTfinal  CTinitial ; . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . ð4Þ

where Vcore (in.3) is the volume of a whole core calculated with diameter D (in.) and length L (in.). The resultant volume (in.3) was con-
verted to cm3 for further calculations. Vpore (cm3) is pore volume; So (%) is oil saturation, which was assumed to be 100%; Voil_produced
(cm3) is the volume of the produced oil measured from SSASI; CTfinal (HU) is the average CT number of the core at the end of the
experiment; and CTinitial (HU) is the average CT number of the core at the beginning of the experiment.

Results and Discussion

ZP. For all fluid and rock cases, the magnitude of ZP showed a decreasing trend with increasing salinity. All solutions, including water
without additives, started at negative ZP lower than –30 mV, meaning the negatively charged stable EDL. However, as salinity
increased, the magnitude of ZP decreased to a value close to zero, and even resulted in a shift of sign convention in the highest salinity
of 80,400 ppm, as shown in Figs. 3 and 4. The decreasing trend of ZP indicates that the repulsive energy between rock particles
strongly reduces with increasing salinity, causing the thinning of the EDL. Because of this extreme thinness of the EDL on both rock
types, rock surfaces become more hydrophobic in higher-salinity fluid, leading to less-effective adsorption of surfactant or salt mole-
cules. In general, rocks with a higher magnitude of ZP are believed to have more-water-wet surface because of EDL expansion. How-
ever, wettability alteration does occur even with the low magnitude of ZP, as presented later. This suggests that the ion exchange or
transfer between the charged surface and surfactant/salt system works as a more impactful factor for wettability alteration. Therefore, it
is difficult to draw a conclusion on the basis of ZP alone for the performance of aqueous-phase solutions. In addition, ZP measured with
WT CR resulted in a slightly higher negative value compared with WT QR because of the higher calcite content within the WT CR
matrix. These results are related to the natural surface charge of each rock type: carbonate with a positively charged surface and quartz
with a negatively charged surface in the neutral condition.

ZP Change by Salinity per Fluid, WT CR

10

–10

–20
ZP (mV)

Unstable
–30
Stable
Water, WT CR
–40
NF, WT CR
S01, WT CR
–50
S02, WT CR

–60 S03, WT CR
S04, WT CR
–70
0 10,000 20,000 30,000 40,000 50,000 60,000 70,000 80,000
Salinity (ppm)

Fig. 3—Results of ZP measurements for WT CR.

IFT. Similar to ZP, the average IFT between the aqueous-phase solutions and crude oil decreased with increasing salinity level and the
addition of surfactant. As expected, surfactants reduced the IFT, but the presence of salinity made the surfactant much more effective
and stimulated the IFT reduction further, as shown in Fig. 5, with a standard deviation of less than 1.00 mN/m represented in the error
bar. The highest IFT observed in this investigation was 24.66 mN/m, which was between distilled water and crude oil. However, when
13,400 ppm of salt was added to distilled water, the IFT was reduced to 12.05 mN/m, nearly one-half of the initial measurement. All
solutions resulted in a similar trend of nearly 50% decrease in the lower salinity level. This level of salinity could be concluded as the
CSC, which was observed at approximately 30,000 ppm for all solutions. At this salinity, IFT reached a fairly stable condition, although
the reduction still slowly occurred further after reaching the CSC.
Among all, Surfactant 01 (S01) showed the lowest initial IFT of 1.65 mN/m, which can be explained by its sodium chloride compo-
nent within the surfactant itself. Surfactants 02 and 03 (S02 and S03) showed the highest interaction and reaction to salinity, starting at
approximately 15-mN/m IFT to as low as 2 mN/m with only 13,400 ppm of salt. The nanotechnology fluid (NF) and S01 resulted in the
most stable IFT throughout all salinity levels, whereas distilled water and other surfactants showed high reactivity and a less-stable con-
dition with the presence of salinity. This confirms that the interaction between surfactant and salt can vary by types of surfactants, and
thus it is important and necessary to analyze the interactions properly before selecting chemicals to be applied in the field.

CA. Different interactions and levels of wettability alteration occurred, but similar trends of wettability shifts were observed for all
cases throughout the CA measurements. Because of its extreme heterogeneity throughout the formation, qualitative analysis and com-
parison to understand the interactions of surfactant, salt, and rock are more important than the quantitative results of each average CA.

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The original condition of the WT formation was oil-wet, with WT CR showing a strongly oil-wet surface with a contact angle of 132 ,
whereas WT QR showed a close to intermediate-wet surface and had a contact angle of 119 . Throughout the CA measurements with
all aqueous-phase solutions, WT CR showed relatively more oil-wet surface than WT QR, which agrees with the natural surface proper-
ties of conventional carbonate and quartz, verified by Kumar and Mandal (2016) in their studies on conventional quartz rock.

ZP Change by Salinity per Fluid, WT QR

10

–10

–20
ZP (mV)

Unstable
–30
Stable

–40 Water, WT QR
NF, WT QR
–50 S01, WT QR
S02, WT QR
–60 S03, WT QR
S04, WT QR
–70
0 10,000 20,000 30,000 40,000 50,000 60,000 70,000 80,000
Salinity (ppm)

Fig. 4—Results of ZP measurements for WT QR.

Change in IFT with Salinity per Fluid

30
Water
NF
25 S01
S02
S03
20
S04
IFT (mN/m)

15

Water
10
S04

5 S03
S02 NF
S01

0
0 10,000 20,000 30,000 40,000 50,000 60,000 70,000 80,000
Salinity (ppm)

Fig. 5—Results of IFT measurements.

Adding surfactants to distilled water, even at no salinity, showed effective wettability alteration. However, as observed in the IFT
measurements, the presence of salinity in the aqueous-phase solution improves the fluid’s ability to alter wettability further, but only to
a certain salinity level. The effect of salinity on CA was similar for all fluids and rock types: Stronger wettability alteration than with
surfactant alone occurred up to approximately 30,000 ppm, and then the surface wettability shifts back toward its original state, as
shown in Figs. 6 and 7, for WT CR and WT QR, respectively. For all fluids, the most effective wettability alteration seems to occur at
the optimal salinity of 26,800 ppm, as presented in Figs. 8 and 9. When considering the standard deviation of each measurement, the
range of salinity that yields the most effective wettability alteration can be determined as 20,000 to 33,000 ppm.
These wettability trends and interactions with salinity can be explained by ion exchange or transfer of monovalent and divalent cations
of salt, anionic or nonionic charges of surfactant molecules, and charged surface of each rock type. Ionic components of surfactant and
salt interact and enhance the adsorption to negatively or positively charged sites of each rock type, replacing the oil droplet on the surface
to the bulk system. However, when the salt concentration exceeds the CSC, an excessive number of cations in salts starts dominating and
interfering with the interactions of surfactant molecules and rock surface, preventing an effective adsorptive reaction of surfactant, salt,
and rock. In addition, the existence of salinity might have caused surfactant adsorption to solid surfaces to increase marginally, which
can significantly reduce the efficiency and efficacy of the surfactant molecule to change wettability (Saxena et al. 2019). Although pH is

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also known to affect ZP, surface charge, and ultimately surface wettability, the concentration at which this investigation was conducted
was 1 gal/1,000 gal or 0.1 vol%. At this low concentration, surfactant had very little to no effect on pH, which was confirmed with each
measurement during ZP analysis. Therefore, it can be concluded that the wettability alteration is much more influenced by the ionic
exchange and transfer between salt, surfactant, and natural rock surface than by the change in pH or ZP.

Change in CA for WT CR
140
Oil-wet

120
CA (degrees)

100

80
Water, WT CR
NF, WT CR
60 S01, WT CR Water-wet
S02, WT CR
S03, WT CR
S04, WT CR
40
0 10,000 20,000 30,000 40,000 50,000 60,000 70,000 80,000
Salinity (ppm)

Fig. 6—Results of CA measurements for WT CR.

Change in CA for WT QR
140
Water, WT QR NF, WT QR S01, WT QR S02, WT QR
Oil-wet
S03, WT QR S04, WT QR
120
CA (degrees)

100

80

60

Water-wet

40
0 10,000 20,000 30,000 40,000 50,000 60,000 70,000 80,000
Salinity (ppm)

Fig. 7—Results of CA measurements for WT QR.

Water NF S01 S02 S03 S04

0 ppm

26,800 ppm

80,400 ppm

Fig. 8—Salinity effect on wettability alteration for WT CR.

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Water NF S01 S02 S03 S04

0 ppm

26,800 ppm

80,400 ppm

Fig. 9—Salinity effect on wettability alteration for WT QR.

NF, S01, and S03 showed the most reduction in CA with the presence of salt in the solution, whereas the other surfactants resulted
in an insignificant shift of wettability. In addition, different surfactants interacted differently with each rock type: WT QR resulted in
the more-water-wet surface when NF and S03 were applied, whereas WT CR experienced stronger wettability alteration with S01 and
S03. This also supports the importance of prescreening of surfactants on various rock types before field applications.

Spontaneous Imbibition with CT Scans. On the basis of the analyses of the EDL stability, IFT reduction and stability, and effective
wettability-alteration ability, we selected NF and S01 for the SSASI experiment and compared them with the water without surfactants.
Three salinity levels were also selected: 0 ppm as a control, 26,800 ppm as a representation of the most favorable condition of injection
water, and 80,400 ppm as a representation of produced/flowback water. Nine aqueous-phase solutions were applied for SSASI on both
WT CR and WT QR aged core samples. Their detailed compositions and the nomenclature used can be found in Table 5. Also, as men-
tioned previously, timely CT scans were performed throughout the SSASI and images were analyzed for PM calculation, which inspects
the fluid penetration in the core during the oil displacement. Again, the quantitative results of SSASI are less significant than the obser-
vation of overall interactions and performance improvements of fluids for EOR.

Fluid/Rock Type Compositions

DW_C, Q Distilled water (0 ppm brine) + 4 wt% KI
FW_C, Q Fracture water (26,800 ppm brine) + 4 wt% KI
PW_C, Q Produced water (80,400 ppm brine) + 4 wt% KI
D_NF_C, Q DW + 1 gal/1,000 gal of NF + 4 wt% KI
F_NF_C, Q FW + 1 gal/1,000 gal of NF + 4 wt% KI
P_NF, C, Q PW + 1 gal/1,000 gal of NF + 4 wt% KI
D_S01_C, Q DW + 1 gal/1,000 gal of S01 + 4 wt% KI
F_S01_C, Q FW + 1 gal/1,000 gal of S01 + 4 wt% KI
P_S01_C, Q PW + 1 gal/1,000 gal of S01 + 4 wt% KI

Table 5—Information about fluid tested for SSASI. D, DW 5 distilled water (0 ppm brine) 1 4 wt% Kl;
F, FW 5 fracture water (26,800 ppm brine) 1 4 wt% KI; P, PW 5 produced water (80,400 ppm brine) 1
4 wt% KI; C 5 carbonate-rich rock type; Q 5 quartz-rich rock type.

Oil recovery from WT CR ranged from 5 to 15%. For all cases, aqueous-phase solutions with a salinity of 26,800 ppm resulted in
the highest RF regardless of the presence of a surfactant. The combination of S01 and fracture water (FW) produced the most oil
volume from SSASI, followed by NF and FW, as presented in Fig. 10. This agrees directly with the CA measurement, where S01 inter-
acted more favorably with WT CR, altering wettability more effectively than NF. The lowest RF was observed with high-salinity brine
without chemical additives, which was expected because of its poor ability to shift wettability and higher IFT compared with other solu-
tions. Even when surfactants were added to produced water, not much improvement of oil recovery was obtained, producing less
volume of oil than just distilled water or FW without surfactant. CT image analyses supported that the PM of each experiment with WT
CR was not high, indicating that the ability of aqueous-phase solutions to penetrate into the matrix and displace oil from pore spaces is
limited in calcite-rich formations.
On the other hand, oil recovery from WT QR was much higher, ranging from 11 to 34%, with a faster imbibition rate, as displayed
in Fig. 11. Like WT CR, solutions with lower salinity yielded a higher RF for all cases. NF blended in FW produced the highest oil
volume with 33.5% RF, followed by S01 and FW with 30.7% recovery, which again agrees with the CA measurements given pre-
viously. However, unlike WT CR, fluids with high salinity resulted in slightly higher RF compared with no-salinity solutions at a
slower production rate. This can be explained by the much lower IFT of high-salinity brine, causing a buoyant force to slowly act as a
dominant oil-recovery mechanism within the WT QR matrix. In addition, the PM for WT QR was much higher than that for WT CR,
which means that more aqueous-phase solution is penetrating into the rock, accessing and replacing the oil in the matrix more effec-
tively, and producing more oil to the surface through imbibition.
CT images analyzed for fluid penetration at the most optimal salinity are shown in Fig. 12. Although only one cross-sectional image
is shown, the average CT number used for the PM calculations was taken from the whole core, which comprises more than 1,000 images.
Because the CT number is dependent on the density of the whole system, imbibition performance could be analyzed by comparing the
initial and final CT numbers. As the denser fluid (the aqueous-phase solution) replaces the lighter fluid (the hydrocarbon or entrapped
gas), the total CT number increases because of an increase in density. This means that if the PM is higher, more hydrocarbon is likely to

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be replaced by aqueous-phase solution, potentially resulting in a higher RF. Overall results of PM, experimental parameters, and their
comparison with RF are shown in Table 6, and the overall imbibition-performance comparison for WT CR and WT QR is displayed in
Fig. 13. As explained previously, the higher RF occurred when the PM was higher. Consequently, each surfactant interacted differently
with each rock type, and the performance improvements of each solution varied with salinity and rock type. Therefore, it is again impor-
tant to thoroughly investigate and understand the interactions of surfactant, salt, and reservoir rock before actual implementations in the
completion process.

RF vs. Time
18
DW_C D_NF_C D_S01_C
FW_C F_NF_C F_S01_C

15 PW_C P_NF_C P_S01_C F_S01_C, 14.5%

F_NF_C, 13.3%

12
D_S01_C, 10.6%
RF (%)

D_NF_C, 9.7%
9 FW_C, 8.3%
DW_C, 8.0%
P_NF_C, 6.6%
6 P_S01_C, 5.9%
PW_C, 5.7%

0
1 10 100
Time (hours)

Fig. 10—Results of SSASI for WT CR.

RF vs. Time
40
DW_Q D_NF_Q D_S01_Q
FW_Q F_NF_Q F_S01_Q F_NF_Q, 33.5%
35
PW_Q P_NF_Q P_S01_Q F_S01_Q, 30.7%
30

25
P_S01_Q, 22.2%
RF (%)

20 D_S01_Q, 20.6%

P_NF_Q, 16.1%
15 D_NF_Q, 15.6%
FW_Q, 13.1%

10 PW_Q, 11.7%

DW_Q, 11.0%

0
1 10 100
Time (hours)

Fig. 11—Results of SSASI for WT QR.

Lower RFs of WT CR can be explained by the original wettability, physical properties, and rock quality. CA measurements con-
firmed that the original condition of WT CR was more oil-wet than WT QR, and less-effective wettability alteration occurred with the
addition of salt and surfactant. Also, WT CR showed extreme heterogeneity, containing white calcite blocks throughout the formation,
with much higher matrix density compared with WT QR, as shown in Fig. 14. These sample 3D generated CT images of a whole core
for each rock type clearly display the heterogeneity and the poor rock quality of WT CR, whereas WT QR was shown to be less dense
and more homogeneous, with bedding planes that allow fluids to have easier access to the matrix. Because of these characteristics and
properties of each rock type, large differences in oil recovery and PM between two rock types took place. Another interesting observa-
tion was a scaling tendency, or crystallization, of salt when fluids contained high salinity of 80,400 ppm. Fig. 15 includes images of
core samples after SSASI with high-salinity aqueous-phase solutions. Salt deposits occur on the contact area of core, and solutions and
are also most likely to occur within the matrix, causing the blockage of pore throats and limiting the path for hydrocarbon to flow out
to the surface. Despite their ability to lower the IFT further after CSC, high-salinity solutions can be detrimental to the flow of hydro-
carbon during imbibition.

Correlations. It is important to understand how much effect each parameter has on oil recovery when establishing the screening crite-
ria for surfactant/salinity in future applications. All the experimental parameters (ZP, IFT, CA, and PM) and calculated oil RF were
used and analyzed to find the relationship and to determine the most impactful parameter that can lead to better oil recovery. In addition
to 18 sets of experimental results presented previously, 22 more variations of aqueous-phase solutions were formulated with numerous
types of surfactant and salinity, and were tested with core samples from the same formation to strengthen the overall correlations.

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2,400

2,300

FW_C 2,200

2,100
2,000

2,300

2,200
F_NF_C 2,100
2,000
1,900

2,300

2,200
F_S01_C 2,100
2,000
1,900

1,850
1,792
FW_Q
1,735

1,678
1,620

1,850

1,788
F_NF_Q 1,725

1,662
1,600

1,850

1,762
F_S01_Q 1,675

1,588
1,500

4 hours 12 hours 24 hours 96 hours 144 hours 240 hours

Fig. 12—CT image analyses for PM for both rock types at the most optimal salinity.

Core CA
Type Fluid PM (HU) ZP (mV) IFT (mN/m) (degrees) RF (%)
DW_C 2 –35.89 24.66 132.25 8.0%
D_NF_C 5 –26.88 10.68 108.40 9.7%
D_S01_C 6 –58.91 1.65 97.60 10.6%
FW_C 4 –11.42 11.88 107.75 8.3%
WT CR F_NF_C 15 –6.75 6.56 85.30 13.3%
F_S01_C 13 –23.49 0.96 73.80 14.5%
PW_C 4 5.63 10.69 126.90 5.7%
P_NF_C 5 3.22 4.85 108.50 6.6%
P_S01_C 4 –5.23 0.90 90.75 5.9%
DW_Q 12 –35.98 24.66 118.75 11.0%
D_NF_Q 7 –40.42 10.68 87.60 15.6%
D_S01_Q 15 –56.84 1.65 89.95 20.6%
FW_Q 9 –7.68 11.88 101.00 13.1%
WT QR F_NF_Q 38 –5.23 6.56 69.10 33.5%
F_S01_Q 26 –19.41 0.96 71.25 30.7%
PW_Q 4 1.33 10.69 119.35 11.7%
P_NF_Q 7 3.58 4.85 86.30 16.1%
P_S01_Q 15 –9.48 0.90 78.65 22.2%

Table 6—Results of all experimental parameters. D, DW 5 distilled water (0 ppm brine) 1 4 wt% Kl;
F, FW 5 fracture water (26,800 ppm brine) 1 4 wt% KI; P, PW 5 produced water (80,400 ppm brine) 1
4 wt% KI; C 5 carbonate-rich rock type; Q 5 quartz-rich rock type.

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RF vs. Time
35 DW_Q D_NF_Q D_S01_Q F_NF_Q, 33.5%
FW_Q F_NF_Q F_S01_Q
F_S01_Q, 30.7%
30 PW_Q P_NF_Q P_S01_Q
DW_Q D_NF_C D_S01_C

25 FW_C F_NF_C F_S01_C

P_S01_Q, 22.2%
PW_C P_NF_C P_S01_C
D_S01_Q, 20.6%
P_NF_Q, 16.1%

RF (%)
20
D_NF_Q, 15.6%
F_S01_C, 14.5%
F_NF_C, 13.3%
15 FW_Q, 13.1%
PW_Q, 11.7%
DW_Q, 11.0%
10 D_S01_C, 10.6%
D_NF_C, 9.7%
FW_C, 8.3%
DW_C, 8.0%
5 P NF_C, 6.6%
P_S01_C, 5.9%
PW_C, 5.7%
0
1 10 100
Time (hours)

Fig. 13—Overall results and comparison of SSASI for WT CR and WT QR.

2,400 1,800
2,288 1,750
2,175 1,700
2,052 1,650
1,950 1,600

Fig. 14—Example CT images of the whole core for (left) WT CR and (right) WT QR.

Fig. 15—Observation of salt scaling on the core sample after SSASI with high-salinity fluids.

ZP did not show much of a relationship with RF for both rock types, as displayed in Fig. 16. Because ZP determines the stability of
EDL according to magnitude, all ZPs were converted to an absolute value. As observed in the results, although some surfactants
strengthen the repulsive energy between rock particles, salinity causes thinning of the EDL. However, wettability alteration still occurs
in such conditions, and the performance improvement of aqueous-phase solutions also happens even at the low magnitude of ZP. There-
fore, it is difficult to conclude that ZP, by itself, has an effect on oil recovery, but it still holds a value in analyzing the surface charge,
EDL strengths, and other electrophoretic properties of solutions and rocks. IFT also showed a weak relationship with oil recovery, but
in general better RFs were observed when IFT was less than 10 mN/m, as shown in Fig. 17. This explains the effect of gravity drainage
and that buoyancy functions as one of the dominant oil-recovery mechanisms during the imbibition process when IFT between crude
oil and fluids is low.
Among all experimental parameters, CA showed the strongest relationship with oil recovery—nearly a direct correlation. Fig. 18
shows that when the surface is oil-wet, a maximum of 11% RF was observed, but when surface wettability was shifted to the
intermediate-wet range, RF improved up to 20%. Last, when the rock surface experienced strong wettability alteration to the water-wet
region, oil recovery increases significantly, to nearly 30% or more. This relationship shows that the capillary pressure works as a more-
dominant oil-drive mechanism during the imbibition, as capillary pressure changes from negative when CA is larger than 90 to posi-
tive when CA is shifted to less than 90 , or a more water-wet surface. The shift of capillary pressure and the ability to access the
retained oil in the pore spaces result in more extraction of hydrocarbon in the matrix. Another strong relationship was observed between

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PM and oil recovery, as shown in Fig. 19. This can be considered as an apparent phenomenon; as more aqueous-phase solution pene-
trates into the core, more oil is likely to be displaced out of the pore space through the combination of buoyant force and
capillary force.

RF vs. ZP
40
Unstable EDL Stable EDL
35

30

RF (%) 25

20

15

10

0
0 10 20 30 40 50 60 70 80 90
ZP (mV)

Fig. 16—Relationship between RF and ZP.

RF vs. IFT
40

30
RF (%)

20

10

0
0 5 10 15 20 25 30
IFT (mN/m)

Fig. 17—Relationship between RF and IFT.

RF vs. CA
50
Water-wet Intermediate Oil-wet

40

30
RF (%)

20

10

0
40 50 60 70 80 90 100 110 120 130 140
CA (degrees)

Fig. 18—Relationship between RF and CA.

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RF vs. PM
40

30

RF (%)
20

10

0
0 5 10 15 20 25 30 35 40 45
PM (HU)

Fig. 19—Relationship between RF and PM.

Conclusions
The purpose of this investigation was to analyze the interactions of surfactant, salt, and unconventional liquids-rich rocks to find the
most favorable condition of the injected fluid, as well as to identify the most influential experimental parameter on improved oil recov-
ery. This study has a practical applicability for maximizing efficiency in the stimulation-fluid-design process and ultimately achieving
improved oil recovery from complicated ULRs. With the ongoing problems associated with excessive water use, a large volume of
high-salinity FPW, and low RF, the results presented here potentially provide a guidance for several aspects of the oil and gas industry.
Identifying the most favorable salinity level for improved oil recovery unlocks the potential for dilution of FPW and fresh water, which
reduces both water use and the number of saltwater-disposal-well operations, and determining the most influential parameter provides
criteria for surfactant screening before actual field applications for completions. These advantages reduce and possibly solve the envi-
ronmental concerns and provide economic benefits in numerous ways. As stated throughout this paper, surfactants and salinity levels
behave and interact differently with different rock types. Therefore, extensive research and understanding of their interactions are criti-
cal, depending on the location of the reservoir and the petrophysical properties of the ULR. The main conclusions of this study can be
summarized as follows:
1. Extreme heterogeneity and ultratight formation were observed in the WT ULR. Two dominant rock types (WT CR and WT QR) are
present throughout the WT formation.
2. The original condition of the WT formation was oil-wet. The carbonate-rich rocks showed a more-oil-wetting surface than the
quartz-rich rocks.
3. The ZP magnitude decreased with increasing salinity for all aqueous-phase solutions. This indicates the thinning of the EDL sur-
rounding the rock particles, the weakening of repulsive energy between them, and a more hydrophobic surface of the rock.
4. The IFT between crude-oil and aqueous-phase solutions decreases with increasing salinity. Reduction of IFT is significant until it reaches
the CSC at approximately 30,000 ppm. IFT reduction occurs gradually, but not as strongly, when salinity was increased after CSC.
5. WT QR is more favorable and effective for wettability alteration, caused by the adsorption of surfactant and salt molecules, com-
pared with WT CR. The shift of surface wettability is most effective at a salinity of 26,800 ppm with all surfactants and for both
rocks, but the surface becomes more oil-wet, reverting to its original wettability, as salinity was increased up to 80,400 ppm.
6. Highest oil recovery through SSASI occurred with aqueous-phase solutions with a low salinity of 26,800 ppm, regardless of the pres-
ence of surfactant, for both rock types. WT QR resulted in higher RF than did WT CR because of less-heterogeneous and better rock
quality, with bedding planes throughout the formation. Imbibition performance and rate varied by surfactant, salinity, and rock type,
meaning that different surfactants interacted more favorably with different rock types. The PM also confirms that as more solution
penetrates into the rock matrix, more oil is likely to be displaced.
7. ZP and IFT did not have strong relationships with oil recovery, but higher recovery tends to occur at lower levels of IFT.
8. Surface wettability and wettability alteration determined by CA were the most influential parameters for higher oil RFs. The more
water-wet the surface is, the more oil is likely to be produced through the shift of capillary pressure. Therefore, the ability of mixed-salt/
surfactant aqueous-phase solutions to alter wettability can be considered as the most important factor for completion-fluid screening.
9. On the basis of the stability of IFT, the ability to alter wettability effectively, and the performance enhancements from SSASI, we
determined the most favorable range of salinity for blended-salt/surfactant completion fluids to be between 20,000 and 33,000 ppm.

Acknowledgments
The authors would like to thank the Harold Vance Department of Petroleum Engineering at Texas A&M University, as well as a private
operator in the Permian Basin, for providing the resources for this study.

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Kang Han Park is a technical sales engineer at Nalco Champion, an Ecolab Company, working on chemical applications and
services in the oil and gas industry. His research interests include unconventional liquids-rich reservoirs, surfactant, completion-fluid
designs, and salinity. Park holds bachelor’s and master’s degrees in petroleum engineering, both from Texas A&M University.
David S. Schechter is a professor in the Harold Vance Department of Petroleum Engineering, the director of the CO2 Enhanced
Oil Recovery Laboratory, and the manager of the Chevron Imaging Laboratory, all at Texas A&M University. He has 30 years of
direct experience in EOR with surface-active agents and gas/CO2, including everything from basic laboratory studies to the
development of full-field projects. Schechter’s main area of interest focuses on reservoir engineering in naturally fractured reser-
voirs and modeling and simulation in naturally fractured reservoirs. He also has managed a research program in EOR, with both
aqueous-phase chemical additives in completion fluids for wettability alteration and gas injection, including the hybrid applica-
tion of both aqueous-phase chemicals and gas injection. Schechter holds a bachelor’s degree in chemical engineering from
the University of Texas at Austin and a PhD degree in physical chemistry from Bristol University, UK. He has organized three SPE
Workshops on naturally fractured reservoirs and acted as the discussion leader at the SPE Forum on EOR in San Antonio, Texas,
USA, in 2017. Schechter is an SPE Distinguished Member.

14 2019 SPE Drilling & Completion

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