SPE 86504

Diversion and Cleanup Studies of Viscoelastic Surfactant-Based Self-Diverting Acid

Bernhard Lungwitz, SPE, Chris Fredd, SPE, Mark Brady, SPE, and Matthew Miller, SPE, Schlumberger; Syed Ali, SPE
and Kelly Hughes, SPE, ChevronTexaco

Copyright 2004, Society of Petroleum Engineers Inc.

This paper was prepared for presentation at the SPE International Symposium and Exhibition
on Formation Damage Control held in Lafayette, Louisiana, U.S.A., 1820 February 2004.
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Abstract
A self-diverting-acid based on viscoelastic surfactant (SDVA)
has been used recently on stimulation treatments of carbonate
formations. The new system has been proven successfull in
more than 250 field applications.
The decrease of acid concentration during the spending
process viscosifies the fluid by the transformation from
spherical micelles to an entangled wormlike micellar structure
while penetrating the carbonate rock. The highly viscous fluid
acts as a temporary barrier and diverts the fluid into the
remaining lower-permeability treating zones. After treatment,
the SDVA barrier breaks when contacted either by formation
hydrocarbons or pre-and post-flush fluids. Quantifying
diversion, fluid efficiency, and cleanup are important factors
for successful candidate selection and job design. Laboratory
tests defining these key factors are presented in this paper.
This paper demonstrates the diverting ability of the acid as
a function of permeability, characterized by introducing the
concept of maximum pressure ratio (dPmax/dPo) supported by
core-flow and acid conductivity tests using limestone and
dolomite cores. Results demonstrate high dPmax/dPo in highpermeability cores and low dPmax/dPo in low-permeability
cores. Retained permeability measurements are presented that
assesses the level of cleanup. Flow initiation experiments of
spent acid systems with gas and brine were performed to
illustrate the cleanup behavior of SDVA in comparison to
gelled acid systems under conditions encountered in gas and
oil wells. The results indicate that SDVA systems clean up
easily and that SDVA provides higher regained permeability
than conventional gelled acid systems.
Background
The purpose of matrix stimulation in limestone and dolomite
reservoirs is the formation of wormholes, which can bypass
the damaged areas and increase the effective wellbore area.

When acid enters the formation with the highest injectivity it

creates highly conductive flow channels, called wormholes, by
dissolving the carbonate-containing minerals. Consequently,
the injectivity will be further increased. The other zones are
left untreated by the acid. To overcome this problem, a
diverting agent is used. Mechanical diverters such as ball
sealers, degradable ball sealers, rock salt, and benzoic acid
flakes are used alone or in conjunction with chemical diverters
based on foams or polymeric gels.1,2 These materials can work
effectively only in a narrow permeability contrast and may
result in residual damage.3 These characteristics are highly
undesirable, particularly in low-pressure gas wells, and in long
vertical and horizontal sections.
Polymer based systems such as in-situ crosslinked gelled
acids (XLGA) have been used in the field as self-diverting
fluids. These systems rely on a pH-triggered increase of
viscosity during the acid spending process. Essentially, the pH
change activates a metallic reagent that crosslinks the polymer
chains, and the resulting viscosity increase causes a higher
flow resistance.4,5 Further increase of the pH deactivates the
metallic crosslinker and breaks the fluid down to the original
linear gel with dissociated polymer chains. However, because
of the nature of the long polymer chains, potential damage of
the formation may occur.3
Recently, a new polymer-free self-diverting acid system
was developed with a fluid stability in temperatures greater
than300oF.6,7 The fluid system has been applied successfully
in both matrix8 and acid fracturing9,10 treatments. It causes
rapid viscosity development throughout the spending process.
The reduction in acid concentration, together with the
simultaneous release of ions in solution, promotes the
transformation from spherical micelles into worm-like
micelles, resulting in increased viscosity of the fluid. The
highly viscous fluid subsequently diverts the remaining acid
treatment fluid into zones of lower injectivity by reducing the
acid loss into wormholes, resulting in an improved zonal
coverage of the treatment interval. Diversion tests using
multiple parallel cores with varying permeabilities showed
effective stimulation in all cores.6,7
This paper presents new data providing further insight into
the understanding of the unique properties of this selfdiverting acid (SDVA) based on laboratory studies.
Specifically described are the chemical and physical properties
of the SDVA fluid, including cleanup efficiency that is
relevant to low-pressure reservoirs.

Experimental
Core-Flow Experiments. The core flow apparatus is shown
schematically in Fig. 1. The flow procedure unless otherwise
noted was as follows:
1. Carbonate cores (0.1 to 50 mD) were saturated with 2
wt% potassium chloride brine. The cores were 1 or
1.5 in. wide and 5 to 6 in. long.
2. The initial permeability of the core was measured by
injecting 2 wt% KCl at 1mL/min.
3. Acid was injected into the core at a constant injection
rate of 1 mL/min.
4. The injection was stopped as soon as the core was
fully penetrated, as indicated by the differential
pressure dropping to zero.
5. The regained permeability to 2 wt% KCl brine was
measured in the reverse direction. The measurement
of regained permeability of the fully penetrated cores
was in most cases not applicable, because no pressure
drop
was
detected
resulting
in
an
infinite permeability.
Acid Fluid-Loss Experiments The fluid-loss tests were
performed in the above-described core apparatus on Indiana
limestone cores (1 to 3 mD) at 150oF (except where noted)
according to a procedure published by Crowe et al.11 At the
beginning of the test, 2 wt% KCl brine was flowed through the
core to establish the differential pressure required for
1mL/min initial leakoff velocity. This differential pressure
was applied during the leakoff test, and the change in flow rate
was monitored versus time.
Conductivity Experiments. The conductivity apparatus
consists of a 125,000-lbf-load press with automated hydraulic
intensifiers and a modified API conductivity cell with a 12-in.2
flow path. Fig. 2 shows a schematic diagram of the apparatus.
The apparatus can attain a maximum closure stress of 10,000
psi and a maximum temperature of 350F. The temperature of
the conductivity cell is controlled by heated platens contacting
the sides of the cell and hot oil circulated through the pistons.
Pressure transducers are used to measure the system pressure
and the pressure drop across the length of the fracture. The
transducers are plumbed with 1/8 in. lines and checked with
manometers to an accuracy of 1 in. of water. A digital caliper
is used to measure the fracture gap width. The apparatus is
capable of running both proppant and acid conductivity.
The fluid is loaded in the acid reservoir and pumped with a
diaphragm-metering pump. The pump is capable of pumping
a maximum rate of 1500 mL/min against 3,000 psi of
backpressure. Before the fluid enters the conductivity cell, it
passes through the reservoir simulator, where the fluid is
heated to the test temperature.
ISCO Chromatography pumps are used to pump brine
through the cell during conductivity measurements. The
pumps draw nitrogensparged 2 wt% KCl brine from a 100gal flowback reservoir.
Before the brine enters the
conductivity cell, it passes through the reservoir simulator and
a silica saturation system (for proppant conductivity). The
apparatus is discussed in more detail elsewhere in
the literature.12

SPE 86504

Results and Discussion

Diversion Ability. Linear coreflow experiments were
performed to evaluate the pressure response and stimulation
efficiency with three fluid systems. The fluid systems
evaluated include the self-diverting viscoelastic acid (SDVA),
the in-situ crosslinked acid (XLGA), and the gelled acid (GA).
These fluids were all formulated using 15 wt% HCl. The tests
were performed at 200 to 240F using limestone and dolomite
cores.
Fig. 3 shows the pressure response during the injection of
SDVA (15 wt% HCl with 7.5% VES surfactant) into a 4.5-mD
dolomite formation core at 1 mL/ min and 208 oF. It can be
seen that the maximum pressure is about 20 times higher than
the initial baseline pressure (dPo) observed during the
injection of KCl brine. We define this maximum pressure
ratio as dPmax/dPo. A dPmax/dPo greater than one indicates
the viscosity of SDVA increased to create a temporary plug
within the wormhole and can be considered an indication of
the diversion capabilities of the fluid system. Although
difficult to see on the log scale, irregular changes in pressure
were observed throughout the SDVA injection process as the
wormholes were plugged and the acid was subsequently
diverted to continue wormhole formation in a different
location. This continual plugging and diversion within the
wormhole resulted in a highly branched wormhole as shown in
Fig. 4. (Fig. 4 shows a Woods metal casting17 of the
wormhole structure.) It is also noted that the inlet face of the
core is free from any residue indicating that diversion occurred
inside the core (Fig. 5). SDVA required 1.1 pore volumes to
create a wormhole that penetrated the length of the core, as
shown by a sharp pressure drop in Fig. 3. The ratio between
the final regained permeability to KCl brine and the initial
permeability (k/ko) was 3625mD, indicating the formation of a
highly conductive wormhole after brine flowback.
A similar test was performed under the same conditions
with an in situ crosslinked polymer acid system (XLGA- 15
wt% HCl with 70 lbm/thousand gal of polyacrylamide
polymer). No wormhole breakthrough was observed despite
the high dPmax/dPo ratio of 11.4 and the fact that 15.2 pore
volumes of fluid were injected (Fig. 6). The k/ko was 0.19,
indicating that the core was damaged under these test
conditions. A wormhole was observed on the core face
covered with polymer residue (Fig. 5). It can be concluded
that the permeability increase caused by the partially
penetrating wormhole channel is not compensating for the
permeability reduction caused by the polymer residue.
Diversion in Dolomite and Limestone Cores. The pressure
buildup in dolomite and limestone cores as a function of initial
core permeability is shown in Fig. 7. The results indicate that
the maximum pressure (dPmax/dPo) generated during SDVA
acid injection increased with original core permeability, over
the range of 1 to 500 mD. The other polymeric systems (GA
and XLGA) exhibit essentially the same response over the
same permeability range, showing that the ability of each fluid
to divert is consistent under these conditions. For comparison,
the pressure responses for straight 15% HCl without any
diverter are included in Fig. 7 and these data show that no
pressure increase. Therefore no diversion is taking place.

SPE 86504

Performance comparisons for the SDVA system in

dolomite and limestone cores at 200 to 208oF are shown in
Fig. 8. The SDVA fluid resulted in wormhole breakthrough
after 1.1 and 1.6 pore volumes injected into 4.5 and 0.5 mD
dolomite cores. The maximum pressure ratios (dPmax/dPo)
were 20 and 4, respectively. Two experiments were also
conducted in limestone cores at a similar temperature. The
cores used were of 1.7 and 38 mD, and the responses showed
similarly effective stimulation as observed for the dolomite
cores. These results demonstrate that the generation of both
CaCl2 and MgCl2 during the reaction of acid with dolomite is
not detrimental to the effectiveness of the viscoelastic
surfactant in stimulation and diversion.
Acid Fluid-Loss Tests. Acid fluid loss-tests were
performed to compare the SDVA with that of a self-diverting
polyacrylamide polymer system (XLGA) under constant
pressure conditions. Straight 15% HCl and a linear gelled acid
(GA) (incorporating 70 lbm/thousand gal of a polyacrylamide
polymer) were also included in the comparison. Fig. 9 shows
the fluid-loss tests for these fluids. The XLGA system has a
comparable initial viscosity to the unspent SDVA fluid of
about 30 cp at 170 1/s and 70oF, and both exhibit the same
leakoff control characteristics. An additional experiment was
conducted in which a mutual solvent [10% EGMBE in KCl
brine] was injected as a preflush to the SDVA system and the
results show no detrimental impact to leakoff control. As
expected, the straight HCl without diverter and the GA system
show lower leakoff control than the self-diverting fluids.
The effects of temperature on the leakoff characteristics of
SDVA are shown in Fig. 10. Significant leakoff control was
achieved with limestone cores over the temperature range of
150 to 250oF.
Fluid Efficiency. Wormhole formation during the
injection of an acid in a carbonate core is typically
characterized by the number of pore volumes required for
wormhole breakthrough (PVbt) as a function of the injection
rate. Fig. 11 shows the number of pore volumes to
breakthrough for SDVA and straight HCl injected in limestone
cores in the 1 to 3 mD permeability range. The data for 3.4%
and 15% HCl were reported by Wang et al.14 The SDVA
system exhibits the characteristic pore volumes to
breakthrough curve associated with the transition in wormhole
structure from face dissolution to dominant wormholes to
ramified wormhole. It is noted that a minimum number of
pore-volumes-to-breakthrough for SDVA (ca. 1.1 PVbt) occurs
at an optimum injection rate of about 1 mL/min at 200oF. This
optimum injection rate is similar to that observed for 15% HCl
at 70oF. The optimum injection rate for 3.4% HCl shifts
towards larger values (from 1 mL/min to 4 mL/min) as the
temperature increases to 122oF based on the data form Wang
et al.14 Additionally, at higher temperature, the acid volume
required to breakthrough increases (from 1.5PV to 3.2PV).
This change in the optimum injection rate has been shown to
depend on the effective diffusion coefficient of the acid
system and can be predicted based on the theory of the
existence of an optimum Damkhler number.13,15-17 The
SDVA system is expected to exhibit the same dependency.

Attempts were made to measure the effective diffusion

coefficient of the SDVA system using a rotating disk
apparatus. However, a direct measurement of the SDVA
diffusion coefficient by rotating disk is not possible because of
its highly non-Newtonian behavior. Anomalies in the rate of
reaction and the scatter in the data were observed due to a
transition from reverse flow to toroidal flow to centrifugal
flow (all of which are laminar flow regimes), which occurs
with non-Newtonian fluids as the rotating speed is increased.18
In addition, the complex viscosity gradient during SDVA
spending could have affected the ability to obtain
representative samples during the spending process. The
highly viscous nature of the fluid also prevented the use of a
diffusion cell for the diffusion coefficient measurements.
These same problems occur when trying to measure the
effective diffusion coefficients of crosslinked gelled acids.
Unfortunately, despite these technical issues, erroneous data
have been used to incorrectly claim that gelled acids are
highly retarded.19
To overcome these measurement issues, the theory of the
existence of an optimum Damkhler number was used to
estimate the apparent effective diffusion coefficient from the
pore volume-to-breakthrough curve for SDVA. It is reported
that the minimum number of pore volumes to breakthrough
occurs for a variety of acid and chelant systems at about the
same optimum Damkhler number of 0.29.15-17 Under the
assumption that SDVA follows the same dependency on the
Damkhler number, an approximate effective diffusion
coefficient of 2.5E-05 cm2/s was estimated for SDVA at
200oF. For comparison, straight 15% HCl, gelled 15% HCl,
and emulsified 15% HCl have effective diffusion coefficients
of about 5.0E-05 cm2/s, 3.1E-05 cm2/s, and 2.5E-06 cm2/s,
respectively, at 200oF.20 Hence, the apparent effective
diffusion coefficient is estimated to be slightly lower than that
for straight HCl and comparable to that of gelled acid.
Regained Permeability. The effects of various acid
systems on the regained permeability were evaluated under
two experimental conditions. In the first type of experiment,
one pore volume of the acid system was injected such that the
wormhole did not break through the core. These experiments
were designed to evaluate the cleanup characteristics of the
fluids under realistic conditions encountered in carbonate
formations (i.e., during acid spending and viscosification in
the vicinity of the wormhole). Fig. 12 compares the regained
permeability of dolomite cores after injecting SDVA and GA
acid systems. It is apparent that the SDVA system causes
negligible permeability reduction to the core, given that the
regained permeability as a fraction of the original permeability
is greater than one (k/ko). However, the polymer system, GA,
showed a significant reduction in regained permeability with
k/ko values less than 0.1 despite a partial wormhole
penetrating the core faces. This reduction in permeability
indicates that residual polymer inhibits the cleanup of
the cores.
Cleanup Behavior. Although not representative of actual
SDVA spending in carbonate formations, a worst case
scenario was evaluated in which one pore volume of fully
spent fluid (i.e., viscosified and non-reactive) was injected into

1 in.-diameter by 6 in.-long limestone cores with

permeabilities ranging from 1.27 to 3.22 mD. Nitrogen or 2
wt% KCl solutions were used as displacements fluids under
constant pressure to simulate the cleanup with gas or
formation fluids. The pressure was increased in 250-psi
increments for 30 min until a steady flow rate was detected.
The retained permeability was measured after establishing a
stable permeability in the production direction using 2 wt%
KCl brine at 1 mL/min. This test procedure does not represent
actual well treatment conditions as the viscosification process
is not allowed to occur locally in the pores as a result of acid
reaction, and the viscous fluid will not penetrate the entire
core, but rather be limited to regions of the porous media in
and immediately around the wormhole channels. Therefore,
in these experiments, the viscous fluid penetrates a
significantly larger percentage of the pore space and will result
in unrealistically low regained permeabilities.
Results for relative cleanup pressures for SDVA using 2%
KCl are shown in Fig. 13. A mutual solvent based on
ethylene glycol monobutyl ether (10% EGMBE in KCl brine)
was used as preflush to aid in the cleanup. The polymer-based
XLGA shows the highest flow initiation pressure (FIP) and
was used as the baseline to normalize the other data to a
percentage. SDVA exhibited a FIP of about 40% of that
required to initiate cleanup of XLGA. Using EGMBE as a
preflush for SDVA further reduced the flow initiation pressure
of the SDVA fluid to about 20%. As seen in Fig. 13, the
regained permeability of the core after the spent XLGA
injection was relatively low at 6%, compared to 97% (SDVA)
and 80% (SDVA with the EGMBE preflush). It should be
noted, that the pressure was increased by 250 psi increments,
leading to an experimental error of approximately 15%.
Fig. 14 presents the results using nitrogen as displacement
fluid. SDVA shows the highest FIP, which can be reduced by
38% using EGMBE as a preflush. The SDVA/ EGMBE (FIP
of 62%) system has a comparable FIP to that of XLGA (FIP of
50%). However, the regained permeability for SDVA (65 to
100%) is significantly higher than that observed for the XLGA
system (12%).
These cleanup experiments represent a worst-case scenario
in which spent acid gel was unrealistically forced through a
low-permeability core. These tests do, however, show that
any spent SDVA gel that enters the matrix is removed at least
as easily as XLGA systems, which have been applied
successfully on a global basis. With XLGA as the benchmark,
we show that the final regained permeability is significantly
better with the SDVA systems.

Surface Tension and Capillary Pressure Measurements.

Numerous studies have been performed that demonstrate
the impact of surface tension and contact angle on capillary
pressure generated by various fluids in porous media.21,22 This
is a very important aspect to consider in the formulation of all
well stimulation fluids. In fact, the industry has developed
surfactants, specifically designed to ensure a water-wet
formation, reduce surface tension and minimize capillary
pressures to facilitate recovery of both treatment fluids and
pay zone hydrocarbons.23

SPE 86504

A series of experiments were conducted according to a

procedure described in the literature24 to evaluate the
wettability and surface tension of spent acid systems on
carbonate surfaces. A comparison was made with a benchmark
fluid, typical of that utilized by the industry for carbonate
acidizing treatments in depleted United States reservoirs: a
linear gelled acid (GA) with 15% HCl and a combination of
surfactants designed to maximize spent acid cleanup. A spent
SDVA fluid formulation (used to stimulate carbonate
formations in West Texas and Wyoming) was mixed with
EGMBE in a 50-50 ratio. Table 1 shows that the surface
tension, contact angle, and capillary pressures (calculated
based on a pore diameter of 0.1 microns) are very similar for
the two fluids. A comparison is included in the table for
measurements of two powerful surfactants, a fluorocarbon,
and an environmentally friendly alternative, Surfactant A,
obtained using sand-packed capillary columns.23 The results
show that the SDVA system in contact with mutual solvent,
representative of mixing during well flow back, is strongly
water-wetting and induces a comparatively low capillary
pressure. Another experiment was conducted using spent
SDVA without EGMBE, also demonstrating that the system
was water wetting. The surface tension measurement was not
possible due to limitations of the experimental method whilst
using viscous non-Newtonian fluids.
Acid Conductivity Tests. Acid conductivity tests were
performed to evaluate the fluid-loss characteristics and acid
conductivity achieved with straight 15% HCl and SDVA.
Tests were performed with Edwards limestone cores at 240oF.
The 15% HCl resulted in a large amount of dissolution near
the entrance of the flow cell (left end of cores in Fig. 15) and
created a large wormhole that broke through the 2.5 in. thick
core within about 1.2 min (Fig. 17). The acid-etched fracture
conductivity was 137 mD-ft at a closure stress of 2,000 psi
and decreased significantly at about 2,500 psi closure stress
due to the crushing of the acid etched fracture faces (Fig. 18).
In contrast to straight HCl, SDVA created effective
differential etching of the fracture faces (Fig. 16) and provided
leakoff control with a wormhole that broke through in about
2.5 min (Fig. 17). Therefore, leakoff control was observed
under acid fracturing conditions. The differential etching of
the fracture faces resulted in a fracture conductivity of 1,426
mD-ft at 2,000 psi and 147 mD-ft at 4,500 psi closure
pressure.
The conductivity results demonstrate that SDVA exhibited
better leakoff control relative to straight HCl. Differential
etching was created when VDA was used to stimulate
limestone cores (similar results also observed with dolomite),
resulting in higher conductivity than observed with HCl.
Conclusions
Laboratory tests confirm the good performance of viscoelastic
fluids as diverting agents in field applications.

SDVA provides highly efficient wormholing

behaviour in limestone and dolomite cores over a
wide range of conditions.
SDVA exhibits similar pressure responses and
leakoff behavior as in situ crosslinked gelled acids.

SPE 86504

SDVA and XLGA exhibit significantly better leakoff

control than straight HCl and non-crosslinked
gelled acid.
Core flow and acid fracture conductivity tests both
demonstrate good leakoff behavior with SDVA.
Hence, SDVA can be effectively used to control
leakoff during acid fracturing treatments.
The pressure response observed during the injection
of SDVA increases with increasing initial core
permeability and is similar for limestone and
dolomite cores.
SDVA exhibits similar or better cleanup behavior
than polymer based acid systems, as demonstrated by
the low FIP and the high regained permeabilities
using gas or brine as displacement fluids. The data
show that the spent SDVA system should be more
easily recovered from low-reservoir-pressure
environments than in-situ cross- linked gelled
acid systems.
Differential etching of the fracture faces was created
when SDVA was used to stimulate Edwards
limestone cores at 240oF. This differential etching
resulted in higher conductivity with SDVA than that
observed with straight HCl.

Acknowledgements
The authors would like to thank ChevronTexaco and
Schlumberger for the permission to publish this paper.
Special thanks to Toan Bui, Jack Lie, and Aaron Galt for their
hard work on laboratory testing. Thanks to Dr. Ernie Brown,
Curtis Boney, Dr. Dan Fu, and Dr. Steve Davies for
discussions and for the critical reading of the manuscript.

4.

5.

6.

7.

8.

9.

10.

11.

Nomenclature
Da
De
dPo
dPmax/dPo
FIP
L
PV
PVbt
PVinj
Q

= Damkhler number
= effective Diffuision coefficient, cm2/s
= baseline pressure drop to brine
= maximum pressure ratio
= flow initiation pressure, psi
= length scale, cm
= pore volumes
= pore volumes to breakthrough
= pore volumes injected
= injection rate. cc/min

12.

13.

14.

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SPE 86504

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of
Straight/Gelled/Emulsified
Hydrochloric Acid Diffusivity Coefficient Using
Diaphragm Cell and Rotating Disk, SPE 56532 presented
at the 1999 Annual Technical Conference and Exhibition
held in Houston, Texas, October 3-6.
21. Hall, B.E.: The Effect of Mutual Solvents on Adsorption
in Sandstone Acidizing, JPT (Dec 1975) 1439-42.
22. Clark, H.B., Pike, M.T., Rengel, G.L.: Water Soluble
Fluorochemical Surfactant Well Stimulation Additives,
SPE 9008 presented at the SPE International Symposium
on Oilfield and Geothermal Chemistry, Stanford, CA., May
28-30, 1980.
23. Hinkel, J.J., Brown, J.E., Gadiyar, B.R. and Beyer, E.:
New Environmentally Friendly Surfactant Enhances Well
Cleanup, paper SPE 82214 presented at the 2003 SPE
Formation Damage Conference held in the Hague,
Netherlands, May 13-14.
24. Rosen, M., Dahanayake, M.: Industrial Utilization of
Surfactants: Principles and Practice, Amer Oil Chemists
Society, (2000).

SPE 86504

Table 1. Comparison of surface tension, contact angle and capillary pressure for SDVA (EGMBE) and a GA
system formulated with a surfactant blend.
Surface Tension

Contact Angle, q

Capillary Pressure, Pc

g or ST, mN/m

degrees

psi

SDVA (EGMBE)

31.5

9.7

90

GA

31.2

8.9

89

23

33.0

81.6

141

Fluorcarbon23

21.0

54.8

351

Water23

72

0.0

2089

Surfactant A

Baseline 3%
NH4Cl at 1 ml/min
(4.5 mD)

Inlet Pressure
Gauge

100.000

1000.0

Hassler Cell
Water Inlet

10.000
dPmax/dPo
= 20

100.0
K/Ko

Back Pressure
Regulator

Fluid

Regain 3% NH4Cl at 9
ml/min (3625 mD)

10000.0

Differential
Pressure
Gauge

Pump

SDVA at 1
ml/min

1.000

10.0

0.100

1.0

0.010

0.1

0.001

dP/dPo

Sample

0.0
0.000
11.0 11.5 12.0 12.5 13.0 13.5 14.0 14.5 15.0 15.5 16.0
Pore Volume
o

Computer Automation

Overburden Pressure

Figure 3. Coreflow test with SDVA in dolomite at 208 F; initial

permeability= 4.5 mD; regained permeability=3625 mD; 1.1 pore
volumes to breakthrough.

Figure 1. Core flow apparatus for acid response and regained

permeability studies.

Figure 2: Schematics of Conductivity Apparatus.

Figure 4. A Woods metal casting of a wormhole formed by SDVA

o
injected at 1 ml/ min into a 4.5 mD dolomite core at 208 F.

SPE 86504

dPmax/dPo

100

10

SDVA

GA

XLGA

HCl

1
1

10

100

1000

Initial Perm [mD]

Figure 7. Pressure buildup during the injection of various acid
systems as function of permeability (limestone and dolomite)

Residual
polymer
damage

45

1.8

Dolomite

Limestone

40

1.6

dPmax/dPo
1.4

PV(bt)

1.2

25

20

0.8

15

0.6

10

0.4

0.2

dPmax/dPo

30

Figure 5. Wormholes penetrating the inlet core faces after

exposure to SDVA (top), and GA (bottom).

PV(bt)

35

4.5 mD

0.5 mD

38 mD

1.7 mD

Figure 8. Pressure buildup and pore volumes to break through

during the injection of SDVA as function of permeability for
dolomite and limestone cores.

1000.00

10.0000

100.00

1.0000

dPmax/dPo
= 11.4

10.00

0.1000

1.00

0.0100

0.10

0.0010

0.01

GA

0.0001

8.0

10.0

12.0

14.0

16.0

18.0

20.0

SDVA

25

22.0

Fluid Loss [mL]

100.0000

dP/dPo

K/Ko

30
10000.00

XLGA
HCl

20

SDVA/EGM BE

15
10
5

Pore Volume

Figure 6. Coreflow test with XLGA in limestone at 208 F; initial

permeability= 1.51 mD; regained permeability=0.29mD; 15.2 pore
volumes to breakthrough.

0
0

Time^0.5
o

Figure 9. Leakoff characteristics for various acid systems at 150 F

using 1 to 3 mD Indiana limestone cores.

SPE86504

120

250 F
200 F

20

120
Rel. FIP
Reg. Permeability

100

100

150 F

15

80

60

60

40

40

Time^0.5

20

20

Figure 10. Effects of temperature on leakoff characteristics of

SDVA in Indiana limestone cores.

Rel. FIP [%]

80

10
5
0

9
8
7
6
5
4
3
2
1
0
0.01

0
SDVA

XLGA

SDVA/EGMBE

Figure 13. Relative flow initiation pressure (FIP) and regained

permeabilities using 2% KCl as displacement fluid.

SDVA; 15% HCl; 200F

3.4% HCl; 70F
15% HCl; 70F
3.4%HCl; 122F

120

120
Rel. FIP

100

100

Reg. Permeability

0.1

1
Flowrate [ml/min]

10

100

Figure 11. Pore volumes to break through versus injection rate for
SDVA and HCl.

Rel. FIP [%]

Pore Volumes to
Breakthrough

Reg. Permeability [%]

25

80

80

60

60

40

40

20

20

Reg. Permeability [%]

Leak-off (ml)

30

0
SDVA

XLGA

SDVA/EGM BE

Figure 14. Relative flow initiation pressure (FIP) and regained

permeabilities using nitrogen as displacement fluid.

2.00

k/ko

1.50
1.00
0.50
0.00

SDVA/16 mD

GA/3.6 mD

GA/0.7 mD

Figure 12. Regained permeabilities of cores after injection of one

pore volume of SDVA and GA systems. No wormhole break
through occurred in these tests.

Figure 15. Post-acidizing picture of top and bottom limestone

o
cores after exposure to 15% HCl at 240 F.

Figure 16. Post-acidizing picture of top and bottom limestone

o
cores after exposure to SDVA at 240 F.

10

SPE 86504

10000

1200
1000

SDVA

SDVA
HCl

800

HCl

1000

Conductivity
(mD-ft)

Fluid Loss [ml/min]

GA

600
400

100
10

200

1
0
0

0.5

1.5

2.5

2000

4000

6000

8000

Closure Stress (psi)

Time^0.5
o

Figure 17. Fluid loss during conductivity experiments at 240 F.

The rapid increase in fluid loss rate corresponds to wormholes
breaking through the 2.5 inch thick cores.

Figure 18. Acid fracture conductivity results with SDVA, GA and

o
HCl with Edwards limestone at 240 F.