PO180245 DOI: 10.

2118/180245-PA Date: 17-April-18 Stage: Page: 1 Total Pages: 13

A New Friction-Reducing Agent for

Slickwater-Fracturing Treatments
Ahmed F. Ibrahim and Hisham A. Nasr-El-Din, Texas A&M University;
and Ahmed Rabie, Genyao Lin, Jian Zhou, and Qi Qu, Solvay

Summary
Friction reducers (FRs) represent an essential component in any slickwater-fracturing fluid. Although the majority of previous research
on these fluids has focused on evaluating the friction-reduction performance of chemical components, only a few studies have addressed
the potential damage these chemicals can cause to the formation. Because of the polymeric nature of these chemicals—typically poly-
acrylamide (PAM)—an FR can either filter out onto the surface of the formation or penetrate deeply to plug the pores. In addition,
breaking these polymers at temperatures lower than 200 F remains a problem. The present study introduces a new FR that replaces the
linear gel with an enhanced proppant-carrying capacity and reduced potential for formation damage.
Friction-reduction performance, proppant settling, breakability, and coreflood experiments using tight sandstone cores at 150 F
were conducted to investigate a new FR (FR1). The performance of the new FR was compared with two different FRs: a salt-tolerant
polymer that is a copolymer of acrylamide and acrylamido-methylpropane sulfonate (FR2), and a guar-based polymer (FR3). Different
breakers were used to examine the breakability of the three FRs, including ammonium persulfate (APS), sodium persulfate (SPS),
hydrogen peroxide (HP), and sodium bromate (SB).
The friction reduction of the new chemical was higher than 70% in fresh water or 2 wt% potassium chloride (KCl) in the presence of
calcium chloride (CaCl2) or choline chloride. The presence of 1 lbm/1,000 gal of different types of breakers did not affect the friction-
reduction performance. The friction reduction of 1 gal/1,000 gal of the new FR1 was also higher than that of the guar-based FR3 at a load
of 4 gal/1,000 gal at the same conditions. The results show that the new FR is breakable with any of the tested breakers. Among the four
tested breakers, APS is the most-efficient breaker. Static and dynamic proppant-settling tests further indicated a superior performance of
FR1 for proppant suspension compared with a PAM FR (FR2). Coreflood experiments showed that FR1 did not cause any residual dam-
age to the core permeability when APS was used as a breaker, compared with 10% and 9% damage when FR2 and FR3 were tested,
respectively. Coreflood tests also showed that FR1 is breakable using SB with only 2.5% damage, whereas FR2 and FR3 resulted in 47%
and 41% damage, respectively. The results also show that higher salinity does not affect the breakability of the new FR.
The proposed FR shows higher friction-reduction performance and better proppant-carrying capacity with no formation damage,
compared with the conventional counterparts. Hence, FR1 is a viable choice for application in fracturing formations with proppants.

Introduction
With the increase in shale-gas and tight-sand production during the past decade, slickwater-fracturing fluids have become more preva-
lent because of their mobility and simplicity. However, because of the low viscosity of the fluid, the pumping rate must be increased to
achieve proppant transportation, which results in a higher energy loss caused by the friction inside the tubular. This requires more hy-
draulic horsepower to address this pressure loss. To overcome that, FRs have been used as a major component of slickwater-fracturing
fluids, which could lower the surface pumping pressure to minimize the energy loss by changing the type of flow from turbulent to lam-
inar (Ke et al. 2006; White and Mungal 2008; Aften 2010; Shah and Kamel 2010; Sun et al. 2010; Robinson et al. 2013; Ozuruigbo and
Fan 2014; Sareen et al. 2014; Zhou et al. 2014; Guerin et al. 2015). Currently, most FRs are PAM-based copolymers (Kaufman et al.
2008; Bybee 2009; Paktinat et al. 2011b; Sun et al. 2011).
PAM FRs are made of long-chain synthetic polymers combined with ionic functionality, which determines their intended use and
specific physical behavior in aqueous media. The standard normal-charge density is 30%. This charge could be positive or negative, but
additional commercial products include neutral polymers lacking any charge. With thousands of gallons of polymers pumped in a typi-
cal fracturing treatment (Paktinat et al. 2011a), the possibility that these high-molecular-weight polymers adsorb on the fracture surfa-
ces or proppant packs is significant. In tight formations, friction-reducing polymers are too large to penetrate deeply enough into the
formation, but retention of polymer molecules in the unpropped fractures will still decrease the productivity (Woodroof and Anderson
1977; Carman and Cawiezel 2007). Holditch (1979) and Ghahfarokhi et al. (2008) showed that decreasing the matrix permeability near
the fracture face causes a significant reduction in the gas production.
Different breakers are usually used to break the FRs and maintain the formation productivity. Sarwar et al. (2011) evaluated the use of
oxidative and enzymatic breakers, including APS, SPS, calcium and magnesium peroxides, and galactomannanase enzymes, to break 30
and 60 lbm/1,000 gal guar gel. They show that ammonium persulfate was the most extensively tested breaker, and that enzymatic breaker
can provide a cleaner, more-homogeneous break of the polymer compared with oxidative breakers when used at the same conditions.
Nasr-El-Din et al. (2007) showed that ammonium persulfate breaks the gel as soon as the temperature reaches 140 F, whereas
with chlorous acid and sodium bromate, the time needed to break the gel was 16 and 83 minutes, respectively, at the same temperature.
Guerin et al. (2015) showed that the conventional oxidizer breakers work effectively for well temperatures higher than 200 F, but
breaking synthetic polymer FRs at temperatures lower than 150 F is significantly more challenging, and a breaker catalyst should be
added to the fluid system.
Compatibility of FRs with scale inhibitors in hydraulic-fracturing fluids is another challenging task. Robinson et al. (2013) presented
an emulsion PAM FR, which is compatible with scale inhibitor, but no formation-damage investigation was conducted. Ozuruigbo and
Fan (2014) investigated the effect of FR on the performance of five scale inhibitors, and they found that the FR diminished the perform-
ance of the scale inhibitors.

Copyright V
C 2018 Society of Petroleum Engineers

This paper (SPE 180245) was accepted for presentation at the SPE Low Perm Symposium, Denver, 5–6 May 2016, and revised for publication. Original manuscript received for review 16
February 2017. Revised manuscript received for review 17 November 2017. Paper peer approved 21 December 2017.

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The FR function will also be affected by the fluid salinity (Paktinat et al. 2011a). The anionic synthetic FRs are not recommended
for use in highly ionic systems because cations (such as calcium and magnesium) greatly reduce their efficiency. The anionic PAMs
give greater friction reduction in fresh water. Saline water usually requires higher concentration of the FR to attain the same level of
drag reduction as in fresh water (Paktinat et al. 2011a).
The present study introduces an FR with enhanced proppant-carrying capacity. The FR performance was evaluated with different ex-
perimental measurements and compared with two conventional FRs. Viscosity measurements were conducted to investigate the break-
ability of the new FR with different breakers. Friction-reduction performance was evaluated at different salt concentrations (5 to 20
wt% KCl) and breaker types. Proppant-carrying capacity was examined with static and dynamic settling tests. Finally, coreflood experi-
ments in tight sandstone cores at 150 F were conducted to assess the formation damage. The following sections of this paper detail the
experimental methods, results, and conclusions.

Experimental Studies
Materials. The proposed FR (FR1) was investigated and compared with a PAM-based reducer (FR2) and a guar-based reducer (FR3).
FR1 is a PAM-coacrylic acid modified with a hydrophobic monomer Z (Fig. 1). FR2 is an anionic PAM/sodium-acrylamido-methylpro-
pane sulfonate-based copolymer. To estimate the active ingredient of FR1, FR2, and FR3, acetone was used to precipitate the polymer.
The active contents of the FR1, FR2 emulsions, and FR3 were 45.3, 46.2, and 47.4 wt%, respectively. The density for FR1, FR2, and
FR3 as received were measured at room temperature and found to be 1.113, 1.106, and 1.054 g/cm3, respectively. The prepared FR sol-
utions were clear with no fish eyes.

NaO NH2
O O
R

X Y Z

Fig. 1—Chemical structure for FR1. R 5 hydrophobic monomer Z.

KCl, CaCl2, and magnesium chloride salts (ACS grade) were used to prepare brine solutions. Deionized water of a resistivity of
18.2 mXcm at room temperature was used in preparing all solutions. Some tests were conducted with saline brine with total dissolved
solids (TDS) of 20,000 ppm. The composition of this brine was 1.34 wt% sodium chloride, 0.49 wt% CaCl2, and 0.17 wt% magnesium
chloride. APS, SPS, HP, and SB were used as breakers for the three FRs. Low-permeability Kentucky sandstone cores of 1.5-in. diame-
ter and 6-in. length were used to evaluate the damage resulting from using FRs. Table 1 lists the mineralogy of the sandstone cores.

Mineral Quartz Illite K-Feldspar Plagioclase

Concentration (wt%) 66 14 3 17

Table 1—Mineralogy of Kentucky sandstone cores.

Friction Reduction. Fig. 2 shows the friction-loop setup that was used to perform the friction-reduction tests. It consists of a 20-ft-
long loop with an inner diameter of 5=16 in. The fluid was pumped at the required flow rate. Pressure transducers were used to measure
the pressure at the inlet and the outlet of the loop, and the pressure difference was recorded using a personal computer (PC) recorder.

PC recorder

Pressure transducer

10 ft
Disposal

Testing
20 ft × ⁵⁄₁₆-in. friction loop sample
Pressure transducer tank

Heat exchanger Injection

port
Centrifugal
pump

Fig. 2—Flow loop used for evaluating the performance of the three drag reducers.

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A typical procedure was as follows: First, 4 gal of water were added to a 5-gal sample tank, and the pump was adjusted to obtain a
flow rate of 5 gal/min. The fluid was circulated in the loop and was allowed to stabilize at 20 C using a heat exchanger. The pressure
difference (DPo) was then recorded. The FR was then injected directly into the loop from a port using a syringe pump. The pressure dif-
ference (DPt) was then recorded with time. Eq. 1 was used to calculate the friction reduction:
ðDPo –DPt Þ
Friction reduction ð%Þ ¼ 100  ; . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . ð1Þ
DPo
where DPo is the pressure drop between the loop inlet and outlet during circulation of fresh or saline water without the FR, and DPt is
the pressure drop at a given time after injecting the FR. Measurements of the friction reduction were consistent with an error of 62%.
The typical value for the pressure drop for the base (DPo) ranged from 140 to 180 psi, depending on the TDS of the water.

Static and Dynamic Proppant Settling. US silica sand of 100 mesh was used for the proppant-settling tests. Proppant-settling tests
were conducted in a beaker equipped with a propeller overhead mixer. For both static and dynamic proppant-settling tests, a solution
with 2 gal/1,000 gal of an FR was initially hydrated in fresh water for 1 hour under 100 rev/min of agitation. Proppant loading was 20
vol%. In the static settling tests, when all the sand was added, the agitation was stopped, and the timer was started. The sand-settling
time was recorded at 40 and 100% settling, which was determined depending on the clear height from the top of the solution. In the
dynamic proppant-settling test, the timer was started after adding all the sand and reducing the agitation speed to either 30 or 50 rev/
min. The settling time was recorded at 40% settling.

Breakability. A rotational viscometer (bob and cup) was used to investigate the breakability of the FR. The viscometer had 12 fixed
speeds from 1 to 600 rev/min; variable speeds from 0.006 to 1,000 rev/min with a speed accuracy of 60.001 rev/min; and a shear rate
range of 0.01 to 1,700 1/s. A solution of 3 gal/1,000 gal of the FR was hydrated for 1 hour in tap water and heated to 140 F. The lower
end for the breaker activation is 140 F (Al-Muntasheri 2014), at which point breakability tests were performed. If the polymer breaks at
this temperature, then it will break at higher temperatures. The initial viscosity of the solution was measured at 300 rev/min (511 1/s).
The breaker was then added at the desired loading, and the timer was started. The viscosity as a function of time was used to monitor
polymer degradation.

Evaluation of Formation Damage. Core Preparation. Coreflood experiments were conducted in low-permeability Kentucky sand-
stone cores to evaluate the damage resulting from using an FR. Table 2 shows the permeability and porosity of the cores used in this
study. Kentucky sandstone cores were drilled with 6-in. length and 1.5-in. diameter. The cores were dried in an oven for 6 hours at
160 F, and the dry weight was measured. The cores were saturated under vacuum with 5 wt% KCl brine overnight, and then the satu-
rated weight was measured. The pore volume (PV) was calculated from the brine density (1.035 g/cm3) and the weight difference
between the saturated and the dried cores. The saturated cores were stored in 5 wt% KCl solutions until the time of the experiment. Ini-
tial and final permeability measurements were conducted with 5 wt% KCl solutions at room temperature to assess the damage.

Initial KCl FR Solution

Coreflood Porosity Permeability Concentration FR/Load Breaker/Load Viscosity at
Set No. (vol%) (md) (wt%) (gal/1,000 gal) (lbm/1,000 gal) 150°F (cp)
01 14.1 0.22 5 FR1/2 APS/3 0.86
02 14.4 0.21 5 FR2/2 APS/3 1.3
1 03 14.3 0.2 5 FR3/2 APS/3 1.5
04 14.3 0.2 5 FR1/2 SB/3 0.86
05 14.6 0.2 15 FR1/2 APS/3 0.88
06 14 0.2 5 FR1/3 APS/3 0.55
07 13 0.15 5 FR2/3 APS/3 0.47
08 14.6 0.17 5 FR3/3 APS/3 0.9
2 09 15 0.21 20 FR1/3 APS/3 0.6
10 12.7 0.17 5 FR1/3 SB/3 0.6
11 14.7 0.2 5 FR2/3 SB/3 0.8
12 13.8 0.19 5 FR3/3 SB/3 0.92

Table 2—Porosity, permeability, and test conditions for coreflood experiments. Viscosity was measured by a capillary viscometer size 0C.

Coreflood Setup. Fig. 3 shows a schematic of the coreflood setup. Two piston accumulators with a capacity of 2 L were used to
store KCl brine and the tested FR solution. A syringe pump was used to displace the solutions from the piston accumulator. Valves
were installed at the inlet and outlet of the accumulators to control the fluid switching during the injection. A pressure transducer was
used to measure the pressure drop across the core, and the results were sent through a data-acquisition system to a computer-operating
software. Valves were installed at the inlet and the outlet of the core holder to control the flow direction. A backpressure regulator was
installed at the core outlet to maintain a backpressure of 500 psi adjusted by a nitrogen cylinder. A hand pump was used to apply an
overburden pressure of 300 psi above the injection pressure (overburden ranged between 1,400 and 1,800 psi). The core holder and inlet
lines were kept in an oven to maintain the temperature at 150 F. This temperature was selected to ensure that the core temperature is
higher than 140 F, which is needed to activate some breakers.
Experimental Procedure for Coreflood Testing. Table 2 provides the permeability and porosity of the cores used in this study. All
experiments were conducted in an oven at 150 F with 500 psi of backpressure at a flow rate of 0.5 cm3/min. The fluid-injection stages
were conducted to simulate the actual hydraulic-fracturing procedures. The permeability measurements and the brine-injection stages

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were conducted in the production direction (to simulate the flow from the formation to the wellbore). The FRs and the breakers were
injected in the reverse direction (to simulate the flow from the wellbore to the formation).

1 2
3

10
8

9
7

Fig. 3—Schematic for coreflood setup. 1, 2 5 accumulators; 3 5 core holder; 4 5 pressure transducer; 5 5 PC recorder; 6 5 hand
pump for overburden pressure; 7 5 syringe pump; 8 5 N2 cylinder; 9 5 backpressure regulator; and 10 5 oven.

Two sets of experiments were conducted to evaluate the proposed FR (FR1). The first set of experiments included injecting the FR
and the breaker in separate stages to evaluate FR performance in absence of the breaker. The main objective of separating the breaker
from the FR stage was to investigate the difference in the pressure-drop response for each FR and to observe if that will be related to
the final degree of breakability by the end of the injection stages. As a result, a sufficient shut-in period of 12 hours was used to ensure
that the breakability is not affected by the kinetics. The first set was conducted using the following steps:
1. Each experiment started by injecting a brine solution (5 or 20 wt% KCl) at 0.5 cm3/min in a direction imitating the flow in a pro-
duction mode from the reservoir to the wellbore.
2. After pressure stabilization, 2 gal/1,000 gal of the FR was injected at 0.5 cm3/min in a reverse direction simulating the flow from
the wellbore to the formation.
3. The second stage of KCl brine was injected at 0.5 cm3/min in the original direction until stabilization to investigate formation
damage caused by the FR under test.
4. 3 lbm/1,000 gal of the breaker was then injected at 0.5 cm3/min in the reverse flow direction for a cumulative volume equal to
the injected FR volume.
5. The system was shut down for 12 hours and the temperature was maintained at 150 F.
6. A final stage of KCl brine (same concentration as the first stage) was injected at 0.5 cm3/min in the original direction until stabili-
zation to evaluate the breakability and final formation damage.
The second set of experiments included injecting both the FR and the breaker as a mixture to evaluate its performance with the
breaker included. A typical procedure for a coreflood experiment involved the following steps:
1. Each experiment started by injecting a brine solution (5 or 20 wt% KCl) at 0.5 cm3/min in a direction imitating the flow in a pro-
duction mode from the reservoir to the wellbore.
2. After pressure stabilization, a solution containing 3 gal/1,000 gal of the FR and 3 lbm/1,000 gal of the breaker (in KCl brine) was
injected at 0.5 cm3/min for 3 hours in the reverse direction, simulating the flow from the wellbore to the formation.
4. The system was shut in for 2 hours at 150 F and a backpressure of 500 psi.
6. A final stage of KCl brine was injected at 0.5 cm3/min in the original direction until stabilization to evaluate the final damage.

Results and Discussion

Friction-Reduction Performance. Table 3 summarizes the friction reduction in the flow loop through use of FR1 in both fresh water
and 2 wt% KCl with different concentrations of CaCl2. In 2 wt% KCl, a friction reduction of 71% was obtained, which slightly
increased at 150 ppm CaCl2.

Friction-Reduction Performance (%)

Time 2 wt% KCl+20 ppm 2 wt% KCl+50 ppm 2 wt% KCl+150
(minutes) 2 wt% KCl CaCl2 CaCl2 ppm CaCl2
0.5 71.4 72.3 72.6 72.7
1 71.2 72.4 72.6 72.6
2 71.2 72.3 72.5 71.7
3 71.1 72.1 71.7 71.7

Table 3—Friction-reduction performance of 1 gal/1,000 gal of FR1 in 2 wt% KCl and different
CaCl2 concentrations.

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Table 4 shows the friction reduction of 1 gal/1,000 gal of FR1 prepared in the saline water (TDS ¼ 20,000 ppm). The data indicated
almost no change in friction reduction in the presence of different loadings of choline chloride (as a replacement for KCl for clay stabi-
lization) (67%), compared with the 2 wt% KCl.

Friction-Reduction Performance (%)

20,000 ppm TDS + 20,000 ppm TDS + 20,000 ppm TDS +
Time 20,000 ppm 0.1 wt% Choline 0.3 wt% Choline 0.5 wt% Choline
(minutes) TDS Chloride Chloride Chloride
0.5 67.4 66.9 66.3 66.8
1 67.3 66.8 67.1 66.7
2 66.6 66.8 67.1 66.7
3 65.9 65.5 65.7 65.4

Table 4—Friction-reduction performance of 1 gal/1,000 gal of FR1 in 20,000 ppm TDS and different
loadings of choline chloride.

The effect of breakers was investigated next, and Table 5 shows the results. APS, SPS, and HP were used as breakers, and the data
show a minimal effect of these breakers on the friction reduction.

Friction-Reduction Performance (%)

Time 1 lbm/1,000 gal 1 lbm/1,000 gal 1 lbm/1,000 gal
(minutes) No Breaker APS HP SPS
0.5 68.7 67.3 68.3 68.8
1 69.1 67.2 68.3 68.7
2 69.1 67.2 68.4 68.2
3 68.5 66.7 67.7 68.2

Table 5—Friction-reduction performance of 1 gal/1,000 gal of FR1 in fresh water with different breakers.

The performance of the new FR1 was compared with FR2 and FR3. Fig. 4 shows a lower performance of 68% and 58% for FR2 and
FR3, respectively, compared with 71.5% for FR1.

75

71
Friction Reduction (%)

67

FR1
63 FR2
FR3

59

55
0.5 1 1.5 2 2.5 3
Time (minutes)

Fig. 4—Friction reduction of 1 gal/1,000 gal of FR1, FR2, and FR3 in 2 wt% KCl.

Breakability. FR breakability is an important and desired feature to prevent formation damage that may result if the FR plugs the pores
of the formation and causes a significant reduction in the well production (Holditch 1979; Ghahfarokhi et al. 2008). Three typical break-
ers—APS, SPS, and HP—were selected to test the degradation of 3 gal/1,000 gal of FR1 at 140 F. The results, shown in Figs. 5
through 8, indicate that FR1 is breakable with any of the breakers tested. The rate of degradation became faster by increasing the con-
centration of the breaker. At the tested conditions, a significant reduction in the breaking time was observed when the breaker load was
increased from 0.1 to 0.2 lbm/1,000 gal. However, less effect was noted above this loading. These results indicate that the degradation
kinetics of FR1 can be optimized by either changing the loading of a specific breaker or the type of the breaker.
Fig. 8 compares the three breakers at a loading of 0.25 lbm/1,000 gal and shows that among the three, APS was the most-efficient
breaker. SPS exhibited lesser but comparable degradation kinetics, whereas HP showed a much-slower effect. These results demonstrate
that for the degradation kinetics of FR1, both the quantity of a specific breaker and/or the type of breaker can be adjusted for optimal
breaking efficiency. A similar behavior was found in the degradation of FR2 and FR3 with the three different breakers (Figs. 9 and 10).

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18

0.1 lbm/1,000 gal APS

15 0.2 lbm/1,000 gal APS
0.25 lbm/1,000 gal APS
12

Viscosity (cp)
9

0
0 20 40 60 80
Time (minutes)

Fig. 5—Viscosity of 3 gal/1,000 gal of FR1 at 1408F and 511 1/s in 0.1, 0.2, and 0.25 lbm/1,000 gal of APS.

18

0.1 lbm/1,000 gal SPS

15 0.2 lbm/1,000 gal SPS
0.25 lbm/1,000 gal SPS

12
Viscosity (cp)

0
0 20 40 60 80
Time (minutes)

Fig. 6—Viscosity of 3 gal/1,000 gal of FR1 at 1408F and 511 1/s in 0.1, 0.2, and 0.25 lbm/1,000 gal of SPS.

18

0.1 lbm/1,000 gal HP

15 0.2 lbm/1,000 gal HP
0.25 lbm/1,000 gal HP

12
Viscosity (cp)

0
0 20 40 60 80 100 120 140 160
Time (minutes)

Fig. 7—Viscosity of 3 gal/1,000 gal of FR1 at 1408F and 511 1/s in 0.1, 0.2, and 0.25 lbm/1,000 gal of HP.

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18
APS SPS HP
15

12

Viscosity (cp)
9

0
0 20 40 60 80 100 120
Time (minutes)

Fig. 8—Viscosity of 3 gal/1,000 gal of FR1 at 1408F and 511 1/s in 0.25 lbm/1,000 gal of APS, 0.25 lbm/1,000 gal of SPS, and 0.25
lbm/1,000 gal of HP.

30
APS SPS
25

20
Viscosity (cp)

15

10

0
0 20 40 60 80 100
Time (minutes)

Fig. 9—Viscosity of 3 gal/1,000 gal of FR2 at 1408F and 511 1/s in 0.25 lbm/1,000 gal of APS and 0.25 lbm/1,000 gal of SPS.

12

APS SPS HP

9
Viscosity (cp)

0
0 20 40 60 80 100 120 140
Time (minutes)

Fig. 10—Viscosity of 3 gal/1,000 gal of FR3 at 140 F and 511 1/s in 0.25 lbm/1,000 gal of APS, 0.25 lbm/1,000 gal of SPS, and 0.25
lbm/1,000 gal of HP.

To confirm the breakability of the polymer solution, the molecular weight of the products was measured using gel-permeation chro-
matography as a function of temperature and APS concentration (Neira-Velazquez et al. 2013). The molecular weight was measured 1
day after breaking all the samples. Table 6 presents the breakability results of FR1.

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Molecular Weight (g/mol)

APS Concentration
(lbm/1,000 gal) 150°F 180°F
0.5 590,000 260,000
1 530,000 127,000
3 43,000 30,000

Table 6—The breakability of 1 gal/1,000 gal of FR1 in fresh water

with APS at 150 and 180º F. The solutions were maintained at
test temperature for 2 hours, and then were allowed to cool down
to room temperature, and maintained at room temperature for
24 hours. Finally, the molecular weight was measured using gel-
permeation chromatography.

Proppant-Settling Tests. Following the procedure detailed previously in the text, the proppant-settling tests were conducted at 2 gal/
1,000 gal FR in static and dynamic conditions. The results, shown in Table 7, indicate that proppant settling is slower with FR1 than
with FR2 and FR3. In static mode, 40% proppant settling was observed after 400 seconds for FR1, whereas the same level of settling
occurred after 24 seconds when FR2 was tested and 10 seconds in the case of FR3. In dynamic conditions with 30 rev/min of agitation
in fresh water, 40% settling was observed for FR1 after 300 seconds, whereas the same level of settling was observed after 45 seconds
for FR2 and 12 seconds in the case of FR3. At 50 rev/min of agitation, the proppant did not settle in the FR1 solution during the test pe-
riod (30 minutes), whereas it settled in the FR2 solution after 60 seconds and 13 seconds in the FR3 solution.

FR1 FR2 FR3

40% settling 100% settling 40% settling 100% settling 40% settling 100% settling
Static test
400 seconds > 30 minutes 24 seconds 1 minute 10 seconds 18 seconds
30 rev/min 50 rev/min 30 rev/min 50 rev/min 30 rev/min 50 rev/min
Dynamic test at 40% settling
300 seconds > 30 minutes 45 seconds 60 seconds 12 seconds 13 seconds

Table 7—Results of proppant-settling tests in static and dynamic conditions at 2 gal/1,000 gal of FR1, FR2, and FR3 in fresh water.

Table 8 presents the proppant-settling results in the case of 0.1 wt% choline chloride. The addition of choline chloride to the system
lowered the carrying capacity for FRs, but the proppant settling is still slower with FR1 than FR2 and FR3.

FR1 FR2 FR3

40% settling 100% settling 40% settling 100% settling 40% settling 100% settling
Static test
62 seconds 2 minutes 20 seconds 35 seconds 8 seconds 18 seconds
Dynamic test at 30 rev/min 50 rev/min 30 rev/min 50 rev/min 30 rev/min 50 rev/min
40% settling 63 seconds 200 seconds 24 seconds 34 seconds 10 seconds 11 seconds

Table 8—Results of proppant-settling tests in static and dynamic conditions at 2 gal/1,000 gal of FR1, FR2, and FR3 in 0.1 wt% choline
chloride brine.

Measuring the viscoelastic properties of the fracturing fluids can give an indication for the proppant-transport capacity. The storage
of elastic (G0 ) and loss of viscous (G00 ) modules provide insight into how elastic and viscous the network structure is at a given fre-
quency. The frequency at which the storage and the loss modules intersect is the frequency at which the material is storing as much
energy elastically as it is losing viscously. This frequency reflects the relaxation time of the network structure. The faster the network
relaxes, the higher the ability for a suspended particle to settle (Loveless et al. 2011). Fluids with higher elasticity characteristics show
better proppant-suspension properties in static and dynamic conditions (Haghshenas and Nasr-El-Din 2014).
A dynamic strain-sweep test was first conducted to define the linear-viscoelastic region. In this test, the strain, ranging from 0.1 to
100%, was applied at constant frequency (0.1 Hz). In the frequency test, the frequency varied from 0.01 to 5 Hz at a constant strain of
5%. The applied strain was selected depending on the strain-sweep test.
G0 and G00 were measured for FR1, FR2, and FR3 at different frequencies ranging from 0.01 to 5 Hz (Fig. 11). G00 values vary from
1 to 3 Pa, and there was no difference between FR1 and FR2 with slightly lower values for FR3. G0 values vary from 0.1 to 1 Pa, where
G0 for FR1 was slightly higher than for FR2 and FR3. Low G0 values for FR solutions were anticipated because the proppant-carrying
capacity on slickwater-fracturing fluids depends mainly on the high flow rate, not the elasticity and viscosity of the fluid.

Coreflood Study. Coreflood experiments were conducted at 150 F to investigate the potential of the formation damage caused by the
three FRs and the breakability using different breakers. Fig. 12 shows the general pressure drop across the core during the coreflood
experiment following the first procedure. The FRs were tested at 2 gal/1,000 gal, while breakers were applied at 3 lbm/1,000 gal. After
measuring the initial permeability at room temperature, the initial brine flow in the main (production) direction and the pressure drop
across the core were recorded until stabilization at DP1.
The flow was then switched to the FR in the opposite (injection) direction. The pressure drop across the core increased during injec-
tion. The reasons for this behavior could be formation damage caused by polymer residue, and filter-cake building on the core inlet.
KCl brine was then injected in the main (production) direction, and as a result it dislodged some of the residual polymer inside the core
or on the face of the core inlet. The KCl brine was injected until the pressure drop across the core stabilized (DP2). The difference
between DP2 and DP1 provides an indication of the formation damage caused by the FR injection without a breaker.

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4
G′, FR3 G′′, FR3
G′, FR2 G′′, FR2
G′, FR1 G′′, FR1
3

G′ and G′′ (Pa)

2

0
0.01 0.1 1 10
Frequency (Hz)

Fig. 11—G0 and G00 for FR1, FR2, and FR3 at 808F and 2 gal/1,000 gal FR loading.

1,400
5 wt% KCl and 5 wt% KCl and
5 wt% KCl 2 gal/1,000 gal 5 wt% KCl 3 lbm/1,000 5 wt% KCl
Pressure Drop Across the Core (psi)

1,200 FR gal Breaker

1,000

800

ΔP2
600
ΔP3
ΔP1

400

200 Shut-in
i ffor
12 hours

0
0 4 8 12 16 20
Cumulative Injected Volume (PV)

Fig. 12—The pressure drop across the core during the coreflood experiment following the first procedure with 2 gal/1,000 gal FR
and 3 lbm/1,000 gal breaker at 1508F (Coreflood-02; 5 wt% KCl 1 2 gal/1,000 gal FR2; 3 lbm/1,000 gal APS).

The flow was then switched to the breaker in the same direction of the FR injection and continued for the same PV. The system was
then shut down for 12 hours to allow ample time for the breaking reaction. Finally, KCl brine was injected in the main (production)
direction to flow back the broken-residue polymer until the pressure drop across the core stabilized (DP3). The difference between DP3
and DP1 provides an indication of the formation damage caused by the FR injection.
Table 9 summarizes the permeability reduction on the first set of coreflood experiments before and after breaker injection. In the
first experiment, Coreflood-01, FR1 was tested at 2 gal/1,000 gal, and APS was applied as a breaker at 3 lbm/1,000 gal. The data indi-
cate a damage of 10% after FR1 injection, which was removed completely after using APS. The permeability of the core after injection
of FR1 and then the breaker increased by nearly 10.3%. One of the reasons for this increase in permeability could be the breaker. Per-
sulfate breaks at temperatures higher than 140 F to provide sulfuric acid. This acid can dissolve oxides and carbonate present in the
core. Dissolution of these minerals will result in higher permeability (Al-Muntasheri et al. 2017).

Reduction in
Permeability Reduction in
Coreflood After FR Permeability After
Set No. FR Solution Injection (%) Breaker Solution Breaker Injection (%)
01 5 wt% KCl+ 2 gal/1,000 gal FR1 10 5 wt% KCl+ 3 lbm/1,000 gal APS –10.3
02 5 wt% KCl+ 2 gal/1,000 gal FR2 29 5 wt% KCl+ 3 lbm/1,000 gal APS 9.5
1 03 5 wt% KCl+ 2 gal/1,000 gal FR3 25 5 wt% KCl+ 3 lbm/1,000 gal APS 6.7
04 5 wt% KCl+ 2 gal/1,000 gal FR1 9.3 5 wt% KCl+ 3lbm/1,000 gal SB 2.5
05 15 wt% KCl+ 2 gal/1,000 gal FR1 16 15 wt% KCl+ 3 lbm/1,000 gal APS 0

Table 9—The permeability reduction of the first set of coreflood experiments before breaking and after breaking the FR.

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In the second experiment, Coreflood-02, the same procedure was followed with FR2 of 2 gal/1,000 gal. The pressure drop increases
from 370 to 1,225 psi after the injection of FR2. This increase in the pressure drop was higher than that observed when FR1 was tested
(1,000 psi). This increase in the pressure drop was observed after 3 PV of injection only compared with 6 PV of injection when FR1
was tested. After injecting the breaker at 3 lbm/1,000 gal, the pressure drop was 477 psi, and a value of 405 psi was reached after the
final brine stage. The data indicate a damage of 29% after FR2 injection, which decreased to 10% after using the breaker.
In Coreflood-03, FR3 was used at 2 gal/1,000 gal. The pressure drop after injection of 5 PV of FR3 was 1,460 psi, which is signifi-
cantly higher than was observed when FR1 or FR2 were tested. After the final stabilization of KCl injection, the pressure drop was 375
psi, which corresponded to 7% damage in the core permeability. Among the three, FR1 was the only FR that did not cause damage to
the tight sandstone core at 150 F.
The degradation of FR1 using a different breaker (sodium bromate) was tested next in Coreflood-04. The initial and the final pres-
sure drops were 390 and 400 psi, respectively. The data revealed that there was a damage of 2.5% to the core permeability.
Coreflood-05 examines FR1 at 2 gal/1,000 gal in a 15 wt% KCl brine solution. The APS breaker was used at 3 lbm/1,000 gal, as in
the previous experiments. The data of the initial, the pressure drop after the breaker, and the final pressure drop reveal no formation
damage, showing that FR1 is not affected by high salinity.
The second set of coreflood experiments was conducted by injecting the FR and the breaker in the same stage. Fig. 13 shows the
general pressure drop across the core during the coreflood experiment following the second procedure, in which the FR was tested at 3
gal/1,000 gal with 3 lbm/1,000 gal breaker in 5 wt% KCl. The brine was initially injected in the main (production) direction and the
pressure drop across the core was recorded until stabilization at DP1. After stabilization, the flow switched to the FR/breaker solution in
the opposite (injection) direction, which resulted in an increase in the pressure. After 2 hours of shut-in, 5 wt% KCl brine was injected
in the main direction to remove the broken-residue polymer or any polymer filtered out on the core inlet. The brine injection continued
until the pressure drop stabilized (DP2). Table 10 summarizes the fluid composition and the final reduction in permeability on the sec-
ond set of coreflood experiments.

1,400
5 wt% 5 wt% KCl + 3 gal/1,000 gal FR
5 wt% KCl
Pressure Drop Across the Core (psi)

1,200 KCl + 3 lbm/1,000 gal Breaker

1,000

800

600
ΔP1 ΔP2

Shut-in for
400 2 hours

200

0
0 2 4 6 8 10
Cumulative Injected Volume (PV)

Fig. 13—The pressure drop across the core during the coreflood experiment following the second procedure with 3 gal/1,000 gal
FR and 3 lbm/1,000 gal breaker at 1508F (Coreflood-06; 5 wt% KCl 1 3 gal/1,000 gal FR1 1 3 lbm/1,000 gal APS).

Set Coreflood No. FR Solution Reduction in Permeability After Injection (%)

06 5 wt% KCl + 3 gal/1,000 gal FR1 + 3 lbm/1,000 gal APS 0
07 20 wt% KCl + 3 gal/1,000 gal FR1 + 3 lbm/1,000 gal APS 0
08 5 wt% KCl + 3 gal/1,000 gal FR2 + 3 lbm/1,000 gal APS 24
2 09 5 wt% KCl + 3 gal/1,000 gal FR3 + 3 lbm/1,000 gal APS 20.2
10 5 wt% KCl + 3 gal/1,000 gal FR1 + 3 lbm/1,000 gal SB 9
11 5 wt% KCl + 3 gal/1,000 gal FR2 + 3 lbm/1,000 gal SB 47
12 5 wt% KCl + 3 gal/1,000 gal FR3 + 3 lbm/1,000 gal SB 41.5

Table 10—The permeability reduction of the second set of coreflood experiments after breaking the FR solutions.

In the first experiment, Coreflood-06, the data indicate that the breaker degrades FR1 in the core and that the flow in the production
direction was sufficient to remove FR1 that might filter out on the core surface, which was the reason for the increase in the pressure
drop during the FR1 injection stage. The values of the initial and the final pressure drop showed that FR1 did not cause any damage to
the tested core at 150 F.
In the second experiment, Coreflood-07, the same procedure was followed with the same loads of the FR1 and the APS
breaker; however, salt concentration was increased to 20 wt% KCl. The data of the initial and the final pressure drop reveal no forma-
tion damage.
FR2 and FR3 were then tested at the 3 gal/1,000 gal with 3 lbm/1,000 gal APS. Damages of 24% and 20.2% were observed in the
cases of FR2 and FR3, respectively.

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The breakability of FR1 with sodium bromate was tested next; 3 gal/1,000 gal FR1 with the breaker at 3 lbm/1,000 gal were
injected at 150 F. In this case, the injection of the FR/breaker solution was scheduled for 3 hours. This was equivalent to 4.5 PV at 0.5
cm3/min. At the end of this stage, the pressure drop increased from 496 to 740 psi. A shut-in period of 2 hours was followed by a final
stage of 5 wt% KCl injection. The final stabilization pressure drop was 545 psi. This was equivalent to a 9% reduction in permeability.
FR2 was tested next. However, during the injection of FR2/breaker solution, the pressure drop reached 1,300 psi after only 2 PV.
Because of the limitation of the injection pump, the flow was switched to the final stage of 5 wt% KCl after the same period of shut-in
time. The final pressure drop was 759 psi. This is an equivalent to 47% reduction in core permeability.
A similar response was observed with FR3. The pressure drop increased in the FR3/breaker injection and reached up to 1,500 psi,
and the pressure drop after the final 5 wt% KCl injection stabilized at 710 psi. This was equivalent to 41.5% reduction in permeability.
The increase in the pressure with FR injection could be caused by internal formation damage (permeability reduction), or formation
of a cake on the inlet of the core. Derived from Rojas et al. (2008), the apparent shear rate that the FR solution will be subjected to in a
porous medium can be calculated by Eq. 2:
u
c¼ ; . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . ð2Þ
/L

u
where is the superficial velocity (in m/s); L is a characteristic length representative of the pore-scale velocity gradients (L ¼ 0.05D);
/
and D is the average pore diameter. Dick et al. (2000) explained that the average pore size (in mm) can be estimated by taking the
square root of the core permeability (in md). Because the permeability for the Kentucky cores varied between 0.17 and 0.21 md, the av-
erage pore size varied from 0.41 to 0.46 mm. At flow rate of 0.5 cm3/min, the shear rate will be nearly 2,000 1/s. At this high shear rate,
there was no difference in the viscosity between the different FRs. As a result, the pressure-drop increase depends mainly on the forma-
tion damage. This work mainly focuses on the internal formation damage, and as a result, the permeability was measured in the opposite
direction of the FR injection to ensure that the filter-cake formation does not affect the assessment.
FR1 has higher friction-reduction performance and better proppant-carrying capacity with no formation damage. With this new FR,
the slickwater-fracturing process will be more efficient in avoiding the formation damage and productivity loss associated with conven-
tional FRs.

Conclusions
A new FR was tested, and the performance was compared with two conventional FRs. The experimental results led to the
following conclusions:
1. The friction reduction of FR1 was higher than 70% in fresh water or with 2 wt% KCl in the presence of CaCl2 or choline chloride.
The presence of 1 lbm/1,000 gal of different breakers did not affect the friction-reduction performance.
2. The new FR is breakable with the three tested breakers: APS, SPS, and HP.
3. Static and dynamic proppant-settling tests indicated a higher performance of FR1 compared with other FRs (FR2 and FR3).
4. Coreflood experiments showed that FR1 did not result in any residual damage to the formation permeability compared with 10% and
7% damage when the other two conventional FRs (FR2 and FR3) were tested, respectively.
5. Coreflood showed that the new FR is breakable using sodium bromate with a minimum of 2.5% damage. The results showed that
higher salinity did not affect the breakability of the new FR.
These conclusions apply to Kentucky cores with permeability range of 0.15 to 0.2 md. Therefore, this work targets formations with
permeability within this range. However, lower-permeability cores will have pumpability issues on the coreflood experiments and in
the field.

Nomenclature
D ¼ average pore diameter, mm
G0 ¼ fluid storage or elastic modules, Pa
G00 ¼ fluid loss or viscous modules, Pa
L ¼ characteristic length representative of the pore-scale velocity gradients, mm
u ¼ fluid velocity, m/s
c ¼ shear rate, s1
DP0 ¼ pressure drop between the loop inlet and outlet during circulation of fresh or saline water without the friction reducer, psi
DPt ¼ pressure drop at a given time after injecting the friction reducer, psi
/ ¼ core porosity, volume fraction

Acknowledgments
The authors thank Solvay USA for permission to publish this paper.

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Ahmed Farid Ibrahim is a research assistant in petroleum engineering at Texas A&M University. He has more than 7 years of diver-
sified international experience, including working for Advantek-International Company. Ibrahim’s areas of research include well
stimulation and formation-damage removal, carbon dioxide sequestration, foam injection, coalbed methane, and reservoir
modeling and simulation. He holds bachelor and master degrees from Cairo University.
Hisham A. Nasr-El-Din is a professor and holds the John Edgar Holt Endowed Chair in Petroleum Engineering at Texas A&M Univer-
sity. Previously, he worked for 15 years as principal professional and team leader of the Stimulation Research and Technology
Team at Saudi Aramco. Before joining Saudi Aramco, Nasr-El-Din worked for 4 years as a staff research engineer with the Petro-
leum Recovery Institute in Calgary. He also worked as a research associate with the University of Saskatchewan, the University of
Ottawa, and the University of Alberta, all in Canada. Nasr-El-Din’s research interests include well stimulation, formation damage,
enhanced oil recovery, conformance control, interfacial properties, adsorption, rheology, cementing, drilling fluids, two-phase
flow, and nondamaging fluid technologies. He holds more than 30 patents, has written 16 book chapters, and has published and
presented more than 660 technical papers. Nasr-El-Din has received numerous awards within Saudi Aramco for significant contri-
butions in stimulation and treatment-fluid technologies and stimulation design, and for his work in training and mentoring. He
holds bachelor and master degrees from Cairo University and a PhD degree from the University of Saskatchewan, Canada, all in
chemical engineering. Nasr-El-Din is a review chairperson for SPE Journal and is a technical editor for SPE Production & Operations
and SPE Drilling & Completion. He has been invited to give keynote presentations in various SPE and NACE conferences.

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Nasr-El-Din received the SPE Regional Technical Discipline Award for Production and Operations in 2006, was named an SPE
Distinguished Member in 2007, and received SPE awards for Outstanding Associate Editor (SPE Journal) and Outstanding Techni-
cal Editor (SPE Production & Operations) in 2008. In addition, he has received the SPE Production and Operations Award and Out-
standing Associate Editor Award (SPE Journal) in 2009. Nasr-El-Din received SPE A Peer Apart status in 2011 for reviewing more
than 100 papers and was named the 2013 recipient of the Distinguished Achievement Award for Petroleum Engineering Faculty.
Ahmed I. Rabie is a senior research scientist II working with Solvay in the Novecare Oil and Gas Group, Bristol, Pennsylvania, USA.
His research interests include fracturing fluids, acidizing, and surfactants, and their effect on increasing oil and gas recovery.
Rabie holds master and PhD degrees from Texas A&M University in chemical and petroleum engineering, respectively.
Genyao Lin is currently a senior scientist with Solvay. Before joining Solvay in 2013, he worked at the Pacific Northwest National
Laboratory as a post-doctoral research associate on water-soluble polymers and hydrogels for drug delivery. Lin’s primary
research areas include hydrophobically modified water-soluble polymers, emulsions, and FRs for the oil and gas industry. He
holds a PhD degree in materials science and engineering from the University of Utah, with a focus on stimuli-responsive polymers
for biomedical sensors.
Jian Zhou is the research and innovation director for Solvay Novecare Oil and Gas Stimulation. Previously, he was a senior
scientist and later a senior engineer at Schlumberger and the global research and innovation senior manager for oil and gas at
AkzoNobel. Zhou holds a bachelor degree in chemical engineering from Tsinghua University in Beijing, a PhD degree in chemistry
from Harvard University, and a post-doctorate from Princeton University.
Qi Qu is currently the vice president of Oil and Gas Research and Innovation at Solvay Novecare. His areas of expertise include
completion/workover fluids, matrix stimulation, and hydraulic fracturing. Previously, he worked for Schlumberger, OSCA Incorpo-
rated, BJ Services, and Baker Hughes in various technical and management positions. Qu holds bachelor’s and master’s
degrees from Beijing University and a PhD degree from the University of Oklahoma.

2018 SPE Production & Operations 13

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