SPE-171732-MS

Impact of Surfactants on Fracture Fluid Recovery

Chandra Palla, Jim D. Weaver, Denise Benoit, Zheng Lu, and Noe Vera, Halliburton

Copyright 2014, Society of Petroleum Engineers

This paper was prepared for presentation at the Abu Dhabi International Petroleum Exhibition and Conference held in Abu Dhabi, UAE, 10 –13 November 2014.

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Abstract
One of the many challenges of unconventional reservoirs is maximizing the recovery of fracturing fluid
following hydraulic fracturing treatments. Effective fracturing fluid recovery reduces water saturation of
the fractured network and fluid invasion into the formation, enabling better hydrocarbon production from
the reservoir. Each chemical component present in complex fracturing fluid systems should first be
carefully formulated to achieve the stimulation design requirements for the well and second to help ensure
complete or maximum recovery of the broken fracturing fluid.
To help achieve maximum fracturing fluid recovery, it is necessary to understand the complex,
multistep processes that occur during the fracturing fluid breaking chemistry (gel degradation) and to
incorporate this understanding into the fracturing fluid design. Considerable attention has been given to
insoluble residue, breaker concentration, break time, and broken fluid viscosity, all which are crucial for
fluid recovery, but these do not address the tendency of insoluble materials contained within the fluid or
formed during the polymer degradation process to aggregate, which can result in a significant loss of
proppant pack permeability. Polysaccharide-based polymers are typically degraded by breakers composed
of enzymes, oxidizers, or acids. These breakers are designed to reduce viscosity of the fluid to enable easy
flowback, but they generally do not degrade the polymer completely to the monosaccharide state; rather
they leave fairly long chained oligomers. These broken polymer fragments tend to aggregate, forming
malleable flocs. The nature of these oligomeric fragment aggregates, such as type, size, and strength of
the association, affect the efficiency of fluid debris recovery following a fracture stimulation treatment.
Surfactants added to the fracturing fluids, if properly chosen, can also act as inhibitors to the formation
of the oligomeric aggregates and prevent flocculation, thus helping to avoid a significant loss of proppant
bed permeability. This paper demonstrates the importance of surfactants in preventing permeability
damage resulting from oligomeric polysaccharide aggregation. Selection of the proper surfactant helps
prevent flocculation and enhances the recovery of broken fluids from proppant packs.
Fracture design engineers can use these strategies to maximize both the rate and efficiency of fracturing
fluid recovery following the fracture stimulation of a well. This can lead to improved hydrocarbon
recovery and is particularly important for the stimulation of extremely low permeability, unconventional
reservoirs.
2 SPE-171732-MS

Introduction
Hydraulically fractured unconventional reservoirs are currently the major source for hydrocarbon pro-
duction in North America. The hydraulic fracturing process can be generally described as pumping a
proppant-laden fluid into a well and through perforations into a hydrocarbon-rich formation at a rate and
pressure that causes the formation to fracture. The fracture propagates away from the well and creates a
network of proppant-filled cracks. Once pumping ceases, the pressure decreases and the cracks begin to
close. The role of the proppant is to hold open the fracture network so the path to the wellbore remains
conductive. To produce hydrocarbons from the reservoir and through the fracture network, it is necessary
to first flow back the aqueous-based fracturing fluids. The incomplete removal of fracturing fluid from the
fracture network and the associated loss of hydrocarbon conductivity is one of the major issues impacting
the hydraulic fracturing results (Balhoff and Miller 2005; Cooke 1975; Sherman and Holditch 1991).
Maximizing the recovery of aqueous fracturing fluid from the network is essential to create an open
path for hydrocarbon to flow and achieve the best production from a well. Hydraulic fracturing fluids have
advanced technologically since their commercial introduction in 1949. With this understanding, polymer
concentrations in fracturing fluids are designed to be near the critical overlap concentration (Weaver et al.
2001). This concentration is the point at which sufficient polymer exists to form a stable gel to provide
proppant suspension, and the gel will quickly become unstable after the molecular weight begins to
decrease by the action of gel breakers. Working near the critical overlap concentration is driven by two
reasons. The first is to minimize the polymer cost of the fluid system, and the second is to minimize the
amount of insoluble residue, which can damage the conductivity of a proppant-packed fracture.
The amount of insoluble residue in a particular fluid system not only depends on the polymer
concentration but also the source of the polymer. Most polymers used in fracturing fluids are based on
polysaccharides, which are produced agriculturally. Often, these can contain up to 15% water-insoluble
residues, such as cellulose and protein, which can cause significant damage to the conductivity of the
proppant pack. Further mechanical and chemical treatments can reduce insoluble contaminates to yield
higher quality materials but result in an increased cost.
However, even these higher-quality polysaccharides with reduced insoluble residues have been found
to form insoluble residue during the gel breaking process. This residue is generally referred to as
breaker-generated and can occur in most polysaccharide fluid systems. Breaker-generated residue is
formed when the polymer chains are broken into shorter chain fragments and oligomers; some of these
have poor solubility in water because they contain too few of the water-solubilizing branches (Weaver et
al. 2003). These broken polymer fragments can aggregate, forming large malleable flocs through
inter-molecular interactions, such as hydrogen bonding, resulting in dramatic damage to the conductivity
of the proppant-packed fracture network. Polymer chain-to-chain interaction can be influenced by the
addition of different types of surfactants. Such polymer-surfactant interaction has been well documented
(Hornof et al. 1983; Kalpakci et al. 1981; Piculell et al. 2003; Prud’homme and Uhl 1984). It is
conceivable that with the addition of surfactant additives into the fracturing fluids, the inter-molecular
interaction between polymer fragments can be changed, and if properly chosen, the surfactant can be used
to inhibit the formation of the oligomeric aggregates and prevent flocculation.
This paper describes the importance of surfactant selection in preventing permeability damage caused
by oligomeric polysaccharide aggregation. By using the proper surfactant, oligomer flocculation can be
minimized and the recovery of broken fluids from proppant packs enhanced. This study used a recently
introduced simple and rapid method (Weaver et al. 2013) instead of standard API conductivity measure-
ments (API 1989), which can be costly and time consuming, to understand the effect of the polymer-
surfactant aggregates on regain permeability. The design principles can be used by engineers to help
maximize both the rate and efficiency of fracturing fluid recovery following the fracture stimulation of a
SPE-171732-MS 3

Table 1—Experiment design.

w/o Non-encapsulated (Instant) Breaker With Non-encapsulated (Instant) Breaker

Components 1 2 3 4 5 6

Polymer Yes Yes Yes Yes Yes Yes

Instant Crosslinker Yes Yes Yes Yes Yes Yes
Delayed Crosslinker Yes Yes Yes Yes Yes Yes
Buffer Yes Yes Yes Yes Yes Yes
Delayed breaker (encapsulated) Yes Yes Yes Yes Yes Yes
Non-encapsulated Breaker No No No Yes Yes Yes
Anionic Surfactant No Yes No Yes Yes No
Non-ionic Surfactant No No Yes No No Yes

well. Proper surfactant selection can lead to improved hydrocarbon recovery and is particularly important
for the stimulation of extremely low permeability, unconventional reservoirs.
Experimental Section
Materials
The fracturing fluid chosen for this study was a low-residue, non-guar, polysaccharide-based polymer
system. The base fluid polymer weight, non-encapsulated (instant) and encapsulated (delayed) cross-
linkers, and pH were kept constant for all of the test fluids. Evaluations were performed by changing the
breakers (encapsulated or encapsulated plus non-encapsulated) and the surfactants (anionic or non-ionic).
The design of experiments to study the effect of both the breaker-type and the surfactant-type on the
regain permeability is shown in Table 1.
Sample Preparation
A polymer concentration of 0.54 wt% was added to 400 mL of tap water and mixed using a blender
for 15 min. Once the polymer was completely hydrated, acidic buffer and surfactant (if present) were
added and mixed thoroughly. Encapsulated breaker and instant non-encapsulated breaker (if present) were
added next. At this stage, 278 g of 20/40-mesh Ottawa sand (proppant) was added to the fracturing fluid,
which made approximately 500 mL of nominal 0.7 kg/L proppant slurry (this is representative of a typical
proppant concentration often used near the end of a fracturing treatment [~6 lbm/gal]), and mixed until
the proppant was uniformly dispersed. Delayed and instant crosslinkers were added at the end and mixed
further for 10 min. The samples were transferred into Mason jars and put into a water bath at 180°F to
break the fluids. Samples were taken from the water bath after 24, 48, or 72 hours for the regain
permeability measurements. The same fluid preparation was performed omitting the proppant materials to
determine fluid viscosity, pH, and particle size.
Measurements
Regain Permeability
The sand (proppant) pack column experimental setup, described in detail by Weaver et al. (2013), was
used to measure the regain permeability of the fluids. The test cell was a transparent PVC column and had
a total capacity of 540 mL. The broken fracturing fluid (~500 mL) was transferred to the column and
topped off with wash water to completely fill and to exclude any air from the column. Note that the Mason
jar containing the proppant and broken fracturing fluid was shaken to thoroughly disperse the broken
fracturing fluid fragments and proppant before loading into the PVC column.
Once sealed, the column was vibrated for a defined time to achieve maximum proppant compaction,
and the proppant height was measured. The column was connected to a flow system that uses dual syringe
pumps to inject water at a programmed rate. The flow rate was increased from 0 to 120 mL/min in step
4 SPE-171732-MS

increments and then gradually decreased slowly to 0 Table 2—Water injection schedule used to perform regain permeabil-
ity measurements on broken fracturing fluids.
mL/min. The standard water injection schedule used
Pump Rate (mL/min) Time (min) Volume (mL)
in all experiments is given in Table 2. Sufficient
water (approximately 18 column volumes or 9 L) 20 50 1000
was flowed through the column to ensure that the 40 25 1000
80 12 960
fracturing fluid had achieved maximum cleanup.
120 45 5400
Continuous measurement of pressure drop across 40 20 800
the proppant pack during flow was obtained using a 5 10 50
low-pressure differential pressure transducer. This Total 162 9210
system can accurately measure differential pressure
from 0 to 100 kPa, and the maximum operational
system pressure pump was set at 2000 kPa for
safety. Using the proppant pack height, flow rate,
and pressure drop, the permeability of the pack was
determined. Pressure drop values at 40 mL/min (in
the step down stage), when the water flow through
the column had reached equilibrium, was used for
calculating permeability values. Regain permeabil-
ity values were determined by normalizing the per-
meability values of a fracturing fluid system with
the permeability values obtained for a water-alone
system without any fracturing fluid. Fig. 1 shows
typical pressure drop and flow rate curves for dif-
ferent fluids exhibiting varying viscosity and parti-
Figure 1—Flow rate vs. differential pressure curves for three typical
cle size characteristics, and Fig. 2 shows the regain broken fracturing fluids.
permeability values for the same three fluid sys-
tems.
Viscosity
Viscosities of the broken gels were determined using a Fann Model 35 viscometer at 300 rev/min. The
prepared solutions were removed from the water bath at the indicated time points and allowed to cool to
room temperature before viscosity measurements were recorded. Readings were taken to be the most
consistent value during a 1-minute spin.
Particle Size
Dynamic light scattering (DLS) measurements were conducted on a Malvern Instruments Zetasizer ZSP
equipped with a HeNe 633-nm laser. Undiluted 10-mm aliquots of as-prepared fluids were analyzed in a
standard cuvette at room temperature after breaking for 24, 48, 72, or 96 hours. The hydrodynamic size
of the polymer or polymer-complex was taken to be the most abundant size peak averaged over three
measurements.

Results and Discussion

To determine the interactions of surfactants on dispersion of polymer oligomers, a non-ionic and an
anionic surfactant were added to a polysaccharide-based polymer hydraulic-fracturing fluid system
containing the polymer, surfactant, buffer, two types of crosslinkers, and an encapsulated breaker. The two
fluid systems were allowed to break at 180°C for 24, 48, and 72 hr. As expected, Fig. 3 shows that the
regain permeability for the fluid system continues to increase with break time from 24 to 72 hours. The
low initial regain permeabilities are directly attributed to the gel still being highly crosslinked and
blocking the pore throats of the sandbed. It is reasonable to assume that the increase in the regain
SPE-171732-MS 5

Figure 2—Regain permeability values calculated from flow rate-differential pressure measurements.

Figure 3—Regain permeability measurements on a broken fracturing fluid without non-encapsulated breaker as a function of break time in the
presence of non-ionic (red) and anionic (green) surfactants.

permeability from 24 to 48 hours is the result of further polymer chain breaking. By 48 and 72 hours,
respectively, more of the gel has broken and the overall viscosities of these solutions dropped dramati-
cally. However, it was interesting that the results also showed a clear difference between the two
surfactants containing solutions, where the non-ionic surfactant consistently had a lower regain perme-
ability.
The regain permeability for the fracturing fluid containing non-ionic surfactant was lower in compar-
ison with the one containing anionic surfactants, even before the polymers were fully broken. The average
percent difference (across 72 hr) between the two fluids (non-ionic and anionic) was 35%, showing that
the fluid containing a charged surfactant had greater regain permeability. These trends suggest that the
non-ionic surfactant either worked to hinder the breaking process or to form surfactant-polymer aggre-
gates. In a typical polymer breaking mechanism, the polymeric materials are broken down into small
fragments, and then the solvent works to separate these fragments, dispersing them into solution.
Conversely, the inter-molecular forces between the polymer fragments tend to facilitate the formation of
6 SPE-171732-MS

Table 3—Viscosity, particle size, and regain permeability measurements in the presence non-encapsulated breaker for non-ionic and anionic sur-
factants.
Non-encapsulated breaker Control Non-ionic Surfactant Ionic Surfactant

24 hours 48 hours 24 hours 48 hours 24 hours 48 hours

Viscosity (cp) 1.0 1.0 1.2 1.0 1.8 1.2

Particle size (nm) 244 137 2227 1876 212 300
Regain Permeability (%) 92.11 84.71 77.09 73.38 86.74 95.5

larger aggregates. These aggregates cannot be broken down by the same breaker because the breaking
mechanism is not applicable to the interaction between oligomers, as the interaction between oligomers
relies on inter-molecular forces instead of chemically bonded acetals. The aggregation and dispersion
process will eventually reach a dynamic equilibrium, in which a narrow size distribution of aggregates will
result. Incorporating different surfactants into the solution will influence the equilibrium by interacting
with the oligomers, subsequently influencing the interaction between oligomer chains.
In the initial set of tests, it was difficult to discern the role of the surfactant as either hindering the
breaking process or dispersing the oligomer fragments. Therefore, to better understand the mechanism of
the surfactant, a more intense breaker (non-encapsulated breaker) was used to speed up the polymer
breaking process, and the degree of breaking was evaluated for the solutions more closely. Three solutions
were prepared— one without any surfactant, one with the anionic surfactant, and one with the non-ionic
surfactant; everything else was consistent with the first set of tests, except a non-encapsulated oxidative
breaker was added. Each solution was then monitored for viscosity, pH, and polymer size to ensure a
complete fluid break had occurred.
Viscosity is the most notable change used to monitor a broken fracturing fluid. As the crosslinked
polymer system is degraded, the material changes from a thick, viscoelastic gel to a low-viscosity fluid.
As shown in Table 3, after 24 hours, all fluids exhibited water-type viscosities (1.2 and 1.8 cp), indicating
that the polymers were broken. By comparison, in the first study, the solution viscosities were still greater
than 2 cp at the end of 72 hours. However, because the fluid can still have regions of unbroken gel, further
evaluations were performed to determine if the fracturing fluid was fully broken. An indirect measurement
of the polymer break was used, comparing the pH of the solution for an unbroken and a broken fluid. One
of the plausible mechanisms is an oxidative breaker reacts with water to generate a hydroxyl radical and
proton. Hydroxyl radicals break the acetal chemical bonds within the polymer while the generation of
protons will result in a lower pH (Duan and Kasper 2011). Therefore, by measuring the pH value of the
fluid system, the degree of polymer breaking can be deduced. In the presence of the non-encapsulated
oxidative breaker, the initial pH of the crosslinked gel was 4.6, and the final pHs for the broken fluids were
lower: 4.31 (non-ionic surfactant) and 4.39 (ionic surfactant). The pHs of the fluids used in the study
without the non-encapsulated breaker were 4.53 and 4.48, for the non-ionic and the ionic surfactants,
respectively, indicating that the fluids were broken down more completely (all pH measurements were
performed with the same pH meter, which was calibrated prior to measurement).
The final analysis of the degree of breaking for the fluids was to study the particle sizes in solution
using DLS. DLS uses light scattered from the particles in solution to track the Brownian motion over short
intervals of time and then uses those changes to determine the overall sizes of the particles in solution.
The particle size of a crosslinked hydrogel is basically infinite and cannot be measured through DLS;
however, as the polymer is broken into disperse fragments, those materials can be measured based on their
movement in solution. As a control, DLS was used to evaluate a hydrated sample of the polymer without
any crosslinkers before and after breaking. The hydrated polymer had an average particle size of ~900 nm,
and the broken polymeric fragments (oligomers) were ~250 nm. As shown in Table 3, the measured
particle sizes for the fluids broken with the non-encapsulated oxidative breaker were relatively small by
SPE-171732-MS 7

Figure 4 —Regain permeability measurements on a broken fracturing fluid with non-encapsulated breaker as a function of break time in (a) no
surfactant (blue), (b) non-ionic surfactant (red), and (c) anionic (green) surfactant.

24 hours and did not change drastically from 24 to 48 hours of breaking, which indicated that the polymers
were fully broken.
Regain permeability studies were run on the fully broken polymer system at 24 and 48 hours, and two
things were noticed: 1) the regain permeabilities with the fully broken polymers were much greater than
the previous study and 2) the non-ionic- surfactant-containing fluid still had much lower regain perme-
abilities.
In the earlier study, the regain permeability ranged from 13.6 to 58.7%, and there was a break-time-
dependent increase of the regain permeability. For the current set of tests, the initial regain permeabilities
were much higher (73.4%), and there was no substantial break-time-dependent increase, which was
expected when using fully broken fluids. Even though the regain permeabilities are much higher for the
fully broken fluids, a noticeable difference still existed for the control and ionic-surfactant-containing
solutions compared to the non-ionic-surfactant-containing solution. Overall, the control and ionic surfac-
tants had very similar regain permeabilities: 92.1 and 84.7% for the control and 86.7 and 95.5% for the
ionic surfactant solution at 24- and 48-hour break times, respectively (Fig. 4). These solutions also showed
very similar particle sizes, from 100 to 300 nm, which were close to the average size measured for the
broken uncrosslinked control (250 nm) mentioned previously. These similarities show that the oligomer
fragments for these two solutions remain dispersed and do not form measurable aggregates during the
48-hour time frame. However, the regain permabilities for the control decreased from 24 to 48 hours,
while the sample containing the anion surfactant increased. These changes signify that the polymer
fragment remained more dispersed with the anionic surfactant than without. Conversely, the measured
particle size for the non-ionic-surfactant-containing solution was much larger (~2,000 nm), which would
mean that larger particles exist (most likely aggregates because the fluid is fully broken). The presence
of these larger particles explains the lower regain permeabilities and signifies the presence of polymer-
surfactant interactions.
Polymer-surfactant interactions have been well documented in the literature; for example, for a
hydroxyethylcellulose polymer, the polymer-non-ionic surfactant interaction enhanced the polymer-
polymer associations when the surfactant concentration was near its critical micelle concentration (CMC).
However, for the same system, an ionic surfactant reduced the inter-polymer associations at concentra-
8 SPE-171732-MS

Figure 5—Schematic illustration of the interaction between oligomer chains and different types of surfactants.

tions near its CMC (Sivadasan and Somasundaran 1990). For the fluid in this study, the ionic surfactant
had a similar charge (anionic) as the oligomers and worked to impart additional electrostatic repulsion to
the system, thus keeping the fragments isolated. The reduced interaction between oligomers inhibited the
oligomer-oligomer aggregation process, keeping the particle sizes small and the regain permeability high.
However, the non-ionic surfactants did not impart a charge in solution and were more likely to interact
with the oligomers through Van der Waals forces (Fig. 5). Such associations allow the surfactant to act
as a glue to bring oligomers together. With the enhanced oligomer-surfactant and oligomer-oligomer
associations, large aggregates form, which can block pore throats and hinder the regain permeability.
The results of these studies reveal that the regain permeability of a fluid system is not solely dependent
on the polymer. The type of surfactant used in a hydraulic fracturing fluid system affects the oligomer
aggregation/dispersion process. By selecting a surfactant that minimizes the broken polymer chains’
ability to aggregate in a fast and effective way, the surfactant will allow the fluid system to retain a higher
regain permeability.
Conclusion
The regain permeabilities for polysaccharide-based hydraulic fracturing fluid were used to determine the
influence of surfactants on dispersed polymer fragments, or oligomers. Non-ionic surfactants were found
to reduce the regain permeability compared to anionic surfactants. Further analysis of the surfactant-
oligomer interaction found that surfactants with a similar charge to the oligomers work to disperse and
isolate oligomers, preventing aggregates from forming. These smaller, dispersed particles can pass more
readily through a packed sandbed and enhance the regain permeability for the system. However, choosing
a surfactant that does not carry a charge similar to the oligomer will induce surfactant-oligomer or
oligomer-oligomer interactions and form large aggregates. These aggregates can block pore throats and
hinder the regain permeability for the solutions. Therefore, it is important to properly select a surfactant
for a fracturing fluid system based on its ability to disperse the broken polymer oligomer chains in a fast
and effective way to retain high regain permeability.

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SPE-171732-MS 9

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