SPE-191606-MS

Evaluation of New Viscoelastic Surfactant Systems in High-Temperatures

Carbonates Acidizing

Ahmed Farid Ibrahim and Hisham Nasr-El-Din, Texas A&M University; Jaqueline de Paulo, Conrado Ewbank, and
Olívia Cueva C. Poltronieri, Oxiteno Company

Copyright 2018, Society of Petroleum Engineers

This paper was prepared for presentation at the 2018 SPE Annual Technical Conference and Exhibition held in Dallas, Texas, 24-26 September 2018.

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Abstract
Viscoelastic surfactants (VES) have been introduced as acid divergent agents for easier cleaning and mixing
advantage over in-situ gelled acid systems. Thermal stability and compatibility with the other additives,
such as corrosion inhibitors, are the main problems with conventional VES. This work introduces five VES-
based acid systems for diversion in matrix acidizing.
A series of VES samples were developed, hereinafter named samples A, A1, B, C and C1 according to
their chemical composition, and evaluated for various applications. The initial screening was conducted by
viscosity measurements of the spent acid system at 150°F and shear rates of 10 and 100 s−1. The effects of
different corrosion inhibitors on the viscosity of the selected VES were then examined. The viscosity of the
VES system was then measured as a function of temperature (77 to 300°F) and shear rate (10 and 100 s−1) to
evaluate thermal stability. The diversion characteristic of the VES systems was evaluated with single core
flood experiments on Indiana limestone cores with a permeability range of 10-200 md. CT-scan imaging of
the cores after the acid treatment was used to evaluate the structure and the propagation of the wormhole.
Dual coreflood experiments were conducted on Indiana limestone cores with permeability contrast of 1.5-50
to examine the ability of the VES to divert the acid system on heterogeneous limestone formations.
Phase separation was observed during the preparation of the systems with a samples C and C1 VES
samples. High viscosity was found in the case of A and B VES systems with the viscosity of 2,500, and 350
cP at 10 and 100 s−1, respectively, at 150°F. The viscosity of the Sample A1 and B VES systems were not
affected by the tested corrosion inhibitor. The single coreflood experiments revealed the ability of the VES
to divert the acid system. The breakthrough injected acid volumes were 0.7 and 0.6 in the case of Sample A1
and Sample B, respectively. The wormhole tortuosity was 1.8 in sample A, compared to 1.4 in Sample B.
This work introduces VES systems with superior divergent ability and viscosity measurements at high
temperature even when in contact with the other acid additives, which leads to less acid spending and better
wormhole structure.
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Introduction
Matrix acidizing is one of the effective well stimulation methods to overcome the formation damage. The
acid system injects at a pressure less than the fracturing pressure to dissolve the damaging materials plugging
the pore as in sandstone formations or creating new wormholes as in carbonates formations. Hydrochloric
acid (HCl) is the most common acid system in carbonate reservoirs acidizing due to its availability and
low cost. In heterogeneous formations, proper acidizing diversion is important during the acid injection to
achieve the maximum benefit.
Viscoelastic surfactants (VES) were introduced as a replacement for the crosslinked-polymers applied
to increase the viscosity of an acid fluid for acid divergent purpose. Several issues were associated with
the crosslinked-polymer including formation damage and loss of permeability (Taylor and Nasr-El-Din
2002; 2003; Taylor et al. 2003; Lungwitz et al. 2007). Permeability reduction was found to be the result of
polymer retention in the core and the core inlet. At high-temperature tight sandstone formations and sour
environment, precipitation of the ferric chloride crosslinker was found by Lynn and Nasr-El-Din (2001) and
Nasr-El-Din et al. (2002). VES were introduced to solve these problems and increases acid system viscosity
for acid divergent purpose.
If the concentration of the surfactant is above the critical micelle concentration (CMC), it forms spherical
micelles. The hydrophobic tails of the surfactants will be inside, leaving the hydrophilic heads outside the
spherical micelle. During carbonates acidizing, HCl dissolves the carbonate minerals. Hence, the calcium
chloride, magnesium chloride increases in the solution. These reaction products will cause the spherical
micelles to develop into worm-like micelles, which entangle together to form 3D network structures (Nasr-
El-Din et al. 2008). As a result, the apparent viscosity of the solution increases (Zeiler et al. 2004; Gomaa
et al. 2011; Al-Ghamdi et al. 2014.
The existence of Fe (III) as a contaminant in VES acid system could reduce the effectiveness of VES-
based acid systems and may lead to formation damage. Shu et al. (2013) showed that acid viscosity decreased
when Fe (III) concentration was higher than 2,300 ppm. Corrosion inhibitors, non-emulsifiers, mutual
solvents, and iron-controlling agents, were found to have a negative impact on VES performance and lower
its viscosity (Nasr-El-Din et al. 2008; Li et al. 2010; Shu et al. 2013; Rabie and Nasr-El-Din 2015).
After the acidizing job spent acid viscosity should be decreased to allow better cleaning and prevent
formation damage. Mutual solvents and crude oil were used to break the gelled spent acid. The hydrocarbon
phase converts the rod-shape micelles into spherical-shape micelles that decrease the viscosity (Nasr-El-
Din et al. 2008).
This paper introduces new VES-based acid systems for acid divergent applications. Rheology
measurements were conducted for initial screening. The passed VES-acid system was then studied at
different temperature and corrosion inhibitor concentrations.

Experimental Studies
Materials
A series of amphoteric VES samples were developed, hereinafter named samples A, A1, B, C and C1
according to their chemical composition. Samples type A, B, and C refers to Betaine, Sultaine, and
Aminoxide based systems, respectively. Acid solutions used in this work were prepared by dilution from a
concentrated HCl ACS- grade stock, obtained from Sigma Aldrich. Calcium chloride was an ACS grade.
All acid solutions were prepared using deionized (DI) water with a resistivity of 18.2 MΩ.cm at room
temperature.
SPE-191606-MS 3

Spent Acid Preparation

To prepare the spent acid system, 20 wt% CaCl2 was used to prepare the spent acid which is equivalent to
15 wt% HCl. Overhead mixer was used to ensure proper mixing of the additives. Corrosion inhibitor was
added at 1 vol% at 150°F and increased up to 3 vol% at 300°F. VES was added at different concentrations
4 and 6 vol%. pH was then adjusted to be between 4-5 using few HCl droplets. The mixture was then
transferred into 50 cm3 sample tube and the sample was then centrifuged at 2500 rpm for 10 min to remove
the trapped air bubbles.

Live Acid Preparation

Live acid was used for the coreflood experiments. Corrosion inhibitor was added at 1 vol% at 150°F and
increased up to 3 vol% at 300°F. Formic acid was added as a corrosion inhibitor intensifier at a temperature
higher than 250°F at 3 vol%. A magnetic stirrer was used to mix the solution. HCl was then added after 5
minutes to reach 15 wt% HCl concentration. After another 5 min, VES was added to the system at 6 vol%.
The acid system was mixed for 15 min before its transfer to the acid accumulator. The acid prepared only
30 min before the injection to avoid corrosion inhibitor separation with time.

Viscosity Measurements
High-pressure high-temperature viscometer (Grace 25600) was used to measure the viscosity of the spent
acid systems. Viscosity measurements were conducted at a different temperature from 150 to 300°F at 400
psi and different shear rates of 10 and 100 s−1. A fresh sample was used for each test where 50 cm3 of it was
transferred into the cup of the rheometer to measure its viscosity.

Coreflood Experiments
To understand the divergent ability for the acid system, coreflood experiments were conducted on single and
dual coreflood experiments on Indiana limestone cores. Fig. 1 shows schematic for the coreflood setup used
in the study. Two piston accumulators with the capacity of 2 liters were used to store the live acid system
and DI water. A syringe pump was used to inject the solutions from the piston accumulators. The core was
inserted on a hassler type core holder. The back pressure regulator was installed at the outlet and controlled
using nitrogen cylinder. The back pressure was set at 1,100 psi to ensure that the reaction products are soluble
in the spent acid (CO2 become supercritical at a pressure higher than 1071 psi) (Fredd and Fogler 1998).
The overburden pressure was set at 1800 psi using a hand pump. The pressure drop across the core was
monitored using pressure transducer which is connected to a computer to the data recorded using Labview.
For Dual coreflood experiments, this setup was adjusted to have two core holders connected from the inlet,
two back pressure regulators and two pressure transducers.

Core Preparation

• Indiana limestone cores with permeability range from 7 to 150 md were used in this study.

• The cores were dried at 150°F overnight and the dry weight was then measured

• The cores were saturated with DI water under vacuum for 4 hrs and then left submerged on the
water for 24 hrs.
• The cores were inserted on the core holder to measure the initial permeability at room temperature.

Coreflood Procedures
For single coreflood experiments, single core was used in each experiment with the average permeability
of 7 md at 1 cm3/min and different temperatures 150 to 300°F.
4 SPE-191606-MS

1. The core was inserted on the core holder and the oven was turned on and the temperature was set at
the required temperature.
2. DI water was injected at 1 cm3/min for 3 hrs to ensure heating up the system and reach stabilization.
3. DI water then switched to acid injection and the effluent samples were collected every 0.33 pore
volume.
4. The pressure drop across the core was monitored until breakthrough which was observed by a sudden
drop in the pressure drop across the core.
5. The system was flushed with DI water to displace the acid out of the core.
6. The oven was turned off and the system left to cool down.
7. The core was then CT-scanned and the effluent samples were analyzed using inductive coupled plasma
(ICP) to get the Ca+2 concentrations.
For Dual coreflood experiments, two cores were used with permeability contrast from 2 to 10.

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

Results and Discussion

Initial Screening
Initial screening was first conducted to select the best VES from the different available systems. Viscosity
measurements were conducted on the spent acid system (6 vol% VES+ 20wt% CaCl2) for the five VES
samples without corrosion inhibitor at 10 and 100 s−1 at a temperature of 150°F. After preparing the first
two samples (C and C1) a phase separation was observed after centrifuging the mixture at 2500 rpm, or on
the raw sample after 10 min (Fig. 2). Hence, these two samples were excluded from the study.

Figure 2—phase separation for Aminoxide-based VES samples

SPE-191606-MS 5

Viscosity measurements were then conducted on Betaine based VES system (A, A1). The VES was
completely mixed on the system with no phase separation. For VES-A system, the viscosity remained stable
at 2500 cP at 10 s−1 for two hrs at 150°F. As the VES is non-Newtonian fluid, the viscosity decreases to
300 cP as the shear rate increased to 100 s−1 (Fig. 3). Similar behavior was found in VES-A1. The viscosity
stabilized at 450 cP at 10 s−1 then decreased to 70 cP when the shear rate increased to 100 s−1 (Fig. 4).

Figure 3—Viscosity measurements for 6 vol% VES-A spent acid ta 150°F, and a shear rate of (A) 10 and (B) 100 s−1.
6 SPE-191606-MS

Figure 4—Viscosity measurements for 6 vol% VES-A1 spent acid ta 150°F, and a shear rate of (A) 10 and (B) 100 s−1.

Viscosity measurements were then conducted on Sultaine-based VES system (B). No phase separation
was observed after mixing the VES. The viscosity remained stable at 2600 cP at 10 s−1 for two hrs at 150°F,
then the viscosity decreases to 300 cP as the shear rate increased to 100 s−1 (Fig. 5).
SPE-191606-MS 7

Figure 5—Viscosity measurements for 6 vol% VES-B spent acid ta 150°F, and a shear rate of (A) 10 and (B) 100 s−1.

To continue screening, the compatibility of the three VES samples with corrosion inhibitor was examined.
1 vol% of commercial corrosion inhibitor (CI-1) was added during the spent acid preparation. The viscosity
was then measured for the spent acid system at 150°F at a shear rate of 10 and 100 s−1. Betaine- Based VES-
A was not compatible with the corrosion inhibitor and the viscosity decreased to 10 cP at 100 s−1. Hence,
VES-A was excluded from the study (Fig. 6).
8 SPE-191606-MS

Figure 6—Viscosity measurements for 6 vol% VES-A spent acid ta 150°F,

and a shear rate of (A) 10 and (B) 100 s−1 in the presence of 1 vol% CI-1.

The viscosity of Sultaine-based VES-B system slightly decreased in the presence of CI-1 to 2200 cP at
10 s−1 compared to 2600 cP without corrosion inhibitor (Fig. 7).
SPE-191606-MS 9

Figure 7—Viscosity measurements for 6 vol% VES-B spent acid ta 150°F, and a shear rate of 10 in the presence of 1 vol% CI-1.

VES-A1 showed an excellent synergy with CI-1. CI-1 improve the formation of the wormlike micelles
which led to higher viscosity, where the viscosity of the spent acid system increased to 2000 cP at 10 s−1 in
the presence of corrosion inhibitor comparing to 450 cP without corrosion inhibitor (Fig. 8).

Figure 8—Viscosity measurements for 6 vol% VES-A1 spent acid

ta 150°F, and a shear rate of 10 in the presence of 1 vol% CI-1.
10 SPE-191606-MS

In order to compare the performance of VES-A1 and VES-B, coreflood experiments were conducted
with the live acid for these systems at 150°F on Indiana limestone cores with the permeability of 7 md. Live
acid system was prepared with 15 wt% HCl, 6 vol% VES, and 1 vol% CI-1.
The pressure drop across the core was monitored during the coreflood experiment and the core scanned
after the experiment. For VES-B, the pressure drop was stable at 17.5 psi during DI water injection (Fig. 9a).
Once the acid system reached the core inlet, the pressure drop across the core increased due to the change
of the viscosity from deionized water to VES-acid and the reaction with core matrix. This was followed
by three intervals of pressure drop increase and decrease with a fluctuation magnitude of 5 to 10 psi. This
fluctuation is a typical response for in-situ gelled acids that describes the dissolution of the calcite minerals
and then the gel formation to divert the acid (Hanafy et al. 2016). The pressure drop across the core dropped
to zero which indicates to the breakthrough. The injected acid volume to a breakthrough was 0.5 PV.

Figure 9—Coreflood experiment for 6 vol% VES-B and 15 wt% HCl acid system at 150°F, and 1 cm3/
min. A) The pressure drop across the core, and B) CT scan image for the core after the treatment.
SPE-191606-MS 11

For VES-A1, the pressure drop across the core stabilized at 16 psi during DI injection (Fig. 10a). During
acid injection, successive pressure drop fluctuations up to 17 times were observed that indicate more gel
formations and acid divergent. The injected acid volume to a breakthrough was 0.6 PV.

Figure 10—Coreflood experiment for 6 vol% VES-A1 and 15 wt% HCl acid system at 150°F, and 1 cm3/
min. A) The pressure drop across the core, and B) CT scan image for the core after the treatment.

CT scan analysis for the two core shows wormhole divergence in both cases (Fig. 9b and Fig. 10b).
The wormhole tortuosity (wormhole length/the core length) was measured to be 1.8 in the case of VES-A1
compared to 1.4 in the case of VES-B. This indicates that VES-A1 has higher divergent ability than VES-B.

Effect of Temperature
The rheology properties for VES-A1 was more investigated at a higher temperature. In acid stimulation
process, as the temperature increases the acid reactivity increases. Hence, the corrosion inhibitor
concentrations should be increased. Viscosity measurements were conducted on the VES-A1 acid system
at higher temperature up to 300°F with increasing the CI-1 concentrations up to 3 vol%.
12 SPE-191606-MS

Fig. 11 shows the viscosity measurements at 200°F at 100 s−1. The viscosity started at 250°F and then
decreased with time at temperature increases to stabilize at 175 cP after 2 hrs. At 250°F, CI-1 concentrations
increased to 2 vol%. The viscosity of the spent acid 200 cP after 2 hrs (Fig. 12). Complete synergy
was observed between CI-1 and VES-A1, as the viscosity of the spent acid increased with increasing
the corrosion inhibitor concentrations even with increasing the system temperature. This behavior was
confirmed at 300°F, where the viscosity of the spent acid stabilized at 300 cP with increasing the corrosion
inhibitor concentrations to 3 vol% (Fig.13). Similar results were observed by Wang et al. (2012) where the
VES acid viscosity increases if it mixed with the compatible corrosion inhibitor.

Figure 11—Viscosity measurements for 6 vol% VES-A1 spent acid

ta 200°F, and a shear rate of 100 s−1 in the presence of 1 vol% CI-1.
SPE-191606-MS 13

Figure 12—Viscosity measurements for 6 vol% VES-A1 spent acid

ta 250°F, and a shear rate of 100 s−1 in the presence of 2 vol% CI-1.

Figure 13—Viscosity measurements for 6 vol% VES-A1 spent acid

ta 300°F, and a shear rate of 100 s−1 in the presence of 3 vol% CI-1.

Coreflood experiments were conducted also at 250 and 300°F using a live acid system of VES-A1. At
250°F, corrosion inhibitor was used with a concentration of 2 vol% and 3 vol% formic acid was used as an
14 SPE-191606-MS

intensifier. Fig. 14a shows the pressure drop across the core. The pressure stabilized at 15.5 psi during DI
water injection and then started to increase as the acid reaches the core inlet. Fluctuations were observed
on the pressure drop data as an indication for the divergent. Acid reached a breakthrough after injection of
0.52 PV. Fig. 14b shows the CT scan images for the core after the acid treatment. It shows branching and
diverted wormhole along the core.

Figure 14—Coreflood experiment for 6 vol% VES-A1 and 15 wt% HCl acid system at 250°F, and 1
cm3/min. A) The pressure drop across the core. B) CT scan image for the core after the treatment.

At 300°F, the concentration of the corrosion inhibitor increased to 3 vol% and 3 vol% of formic acid was
also added to the system. Fig. 15a shows the pressure drop across the core. The pressure stabilized at 15.9
psi during DI water injection and then started to increase as the acid reaches the core inlet. Fluctuations
were observed on the pressure drop data as an indication for the divergent. Acid reached a breakthrough
after injection of 0.4 PV. Fig. 15b shows the CT scan images for the core with diverted wormhole along the
core which proves the ability of the VES to divert the acid at high temperature.
SPE-191606-MS 15

Figure 15—Coreflood experiment for 6 vol% VES-A1 and 15 wt% HCl acid system at 300°F, and 1
cm3/min. A) The pressure drop across the core. B) CT scan image for the core after the treatment.

Effect of VES Concentration

To examine the ability to reduce the VES dosage, viscosity measurements were conducted on a spent acid
system with 4 vol% VES (Fig. 16). The viscosity of the system maintained at 250 cP at a temperature of
250 °F and shear rate of 100 s−1. These results indicate the ability to lower the concentration of VES and
getting the same viscosity.
16 SPE-191606-MS

Figure 16—Viscosity measurements for 4 vol% VES-A1 spent acid

ta 250°F, and a shear rate of 100 s−1 in the presence of 2 vol% CI-1.

Dual Coreflood
Dual coreflood experiments were conducted on Indiana limestone cores at 250 °F and injection flowrate
of 3 cm3/min. The live acid system was consist of 15 wt% HCl, 6 vol% VES-A1, 2 vol% CI-1, and 3 vol
Formic acid. Two experiments were conducted to evaluate the effect of permeability contrast on the VES
ability to divert the acid system.
On the first experiment two cores with permeability of 80, and 14.8 md, and the initial permeability
contrast was calculated to be 5.4. Fig. 17 shows the pressure drop across the cores during the acid injection.
The pressure drop was stable at 8.5 psi during the DI water injection, then it increased once the acid
reached the high permeability core inlet. The injected acid to breakthrough was found to be 0.8 PV, which
is calculated based on the pore volume for both cores.
SPE-191606-MS 17

Figure 17—The pressure drop across the core during the first dual coreflood experiment for 6 vol
% VES-A1 and 15 wt% HCl acid system at 250°F, and 3 cm3/min with permeability contrast of 5.4.

Fig. 18 shows CT-scan analysis for the cores after acid treatment. Clear acid break through can be
observed on both cores from the inlet and the outlet images. The high permeability core shows some
branching on the main wormhole, comparing to straight single wormhole on the low permeability core.

Figure 18—CT-scan analysis for the cores after acid treatment for the first dual coreflood experiment.
18 SPE-191606-MS

The second dual coreflood experiment was conducted to examine the diversion ability of the VES acid
system at high permeability contrast. Indiana limestone cores were used with permeability of 224, and 9
md with initial permeability contrast of 25. Fig. 19 shows the pressure drop from the inlet to the outlet. The
pressure drop stabilized at 6.4 psi during DI water injection and then increased as the acid start to react with
the rock. The injected acid volume to breakthrough was found to be 0.71 PV.

Figure 19—The pressure drop across the core during the second dual coreflood experiment for 6
vol% VES-A1 and 15 wt% HCl acid system at 250°F, and 3 cm3/min with permeability contrast of 25.

Fig. 20 shows CT-scan analysis for the cores after acid treatment. Breakthrough was happened on the
high permeability cores and wormhole was propagated to 2.8 in. which is 47% of the length of the low
permeability core. These results are shows higher divergent ability comparing to Hanafy et al. (2016) results,
where the stimulation percent of the low permeability core were 45 and 18.6 % with permeability contrast
of 14.4, and 28.3.
SPE-191606-MS 19

Figure 20—CT-scan analysis for the cores after acid treatment for the second dual coreflood experiment.

Conclusions
This study introduces a new VES acid system for acid divergent application in carbonate acidizing. Results
lead to the following conclusions:
1. Phase separation was observed during preparing the spent acid of aminoxide-based VES samples
2. Complete synergy was observed between betaine-based VES sample and the used corrosion inhibitor,
and the viscosity increased as the corrosion inhibitor concentration increased at 300°F.
3. A low dosage of VES can be used, where decreasing the VES concentration from 6 to 4 vol% didn't
affect the system viscosity.
4. Single coreflood experiments revealed the acid divergent ability of VES-A1, where the wormhole
length was double the core length.
5. Dual coreflood show high divergent ability for the VES-A1 acid system, where the stimulation percent
of the low permeability core were 100, and 47 % at peremability contrast of 5.4 and 25, respectively.
VES-A1 shows superior divergent ability and viscosity measurements at high temperature even when in
contact with the other acid additives, which leads to less acid spending and better wormhole structure.

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