SPE 82273
Gas Assisted Acidizing of Carbonate Formations
S. Shukla, SPE, D. Zhu, SPE, and A. D. Hill, SPE, The University of Texas at Austin
Copyright 2003, Society of Petroleum Engineers Inc.
This paper was prepared for presentation at the SPE European Formation Damage
Conference to be held in The Hague, The Netherlands 13-14 May 2003.
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Abstract
Matrix acidizing is a commonly used well stimulation
technique in which acid is injected into the formation in order
to dissolve a portion of the rock and hence, recover or enhance
the permeability in the near well-bore region. In carbonates,
when acid is injected, selective dissolution of the rock takes
place creating highly permeable flow channels, called
wormholes. In general, for a matrix acidizing treatment in
carbonates, the deeper the wormholes penetrate into the
formation, the better the outcome, as characterized by a lower
skin factor. Thus, the deeper the wormhole penetration
achieved with a given volume of acid, the more efficient the
treatment. In this paper, we present laboratory results that
show that wormhole propagation is enhanced by injecting
nitrogen gas ahead of the acid.
As wormholes are being created, not all of the acid
reaches the wormhole tip. A significant part of the acid is lost
as fluid loss to adjacent pores. If this fluid loss can be
controlled, then more of the acid can reach the wormhole tip,
and hence the penetration of wormholes can be more efficient.
This paper investigates the effect of saturating the carbonate
rock with gas (nitrogen) prior to the injection of acid in order
to reduce the permeability to acid, and thus reduce the fluid
loss from the main wormhole.
It was found that gas injection prior to acid injection does
significantly reduce the volume of acid required to propagate
wormholes through cores. This effect is observed both at room
temperature and at higher temperatures. The presence of gas in
the core reduced the acid volume needed for wormhole
propagation through the core by a factor of up to 3. The paper
presents an extensive set of experimental results for both gas-
and liquid- saturated carbonate cores subsequently treated with
strong HCl solutions. We show that the acid volumes are
generally smaller for the nitrogen-saturated cores, and that the
wormholes created are narrower and less branched than in the
case of water saturated rocks. We also show that the presence
of oil saturation at residual water saturation in the core has a
similar beneficial effect on wormhole propagation to gas
injection. On the other hand, oil present at its residual
saturation had little effect on the acidizing process. All of
these results confirm the strong influence that fluid loss from a
propagating wormhole has on the efficiency of the acidizing
process in carbonates.
Introduction
Acid stimulation with strong hydrochloric acid solutions is a
common method to increase well productivity in carbonate
reservoirs. When hydrochloric acid is injected into the
formation, the acid dissolves carbonate rocks in a highly non-
uniform pattern. Large channels, known as wormholes, are
created by the acid dissolution. Wormholes are very important
in carbonate acidizing because of their high conductivity
compared with the Darcy-scaled porous medium. Wormholes
dominate the near-wellbore flow after stimulation.
Effectiveness of acid treatments is mainly determined by the
geometry and pattern of the wormholes created. In general, the
effectiveness of a matrix acid treatment in carbonates depends
strongly on the depth of penetration of wormholes into the
formation. Since the conductivity of the wormholes is almost
infinite compared with the matrix, if wormholes penetrate
beyond any near wellbore formation damage, the post-
stimulation skin factor is given by
r 
s = ln wh 
 (1)
 rw 
where rwh is the radial distance to which wormholes have
penetrated and rw is wellbore radius. Thus, an acid treatment in
carbonates is improved if wormhole penetration can
be increased.
The structure of wormhole channels is strongly dependent
on the rates of mass transfer and surface reaction, which may
vary among different acid/rock systems. The most efficient
process is the one propagating wormholes as far as possible
using the least acid volume. Numerous previous studies
(summarized in Chapter 16 and its Appendix in Reference 1)
have shown that the dissolution structures created by acid in
carbonates can be characterized as dissolution of the rock face
2 SPE 82273
(compact dissolution), wormhole formation, characterized by
the creation of one or perhaps a few major wormholes, and
uniform dissolution (ramified wormholes), in which the
structure is so highly branched that it resembles pore-level
dissolution (Figure 11). The structure created depends on many
factors, including injection rate, mass transfer rates, and
reaction rates. Some of the previous modeling studies2,3 have
shown that the propagation of wormholes depends very
strongly on the fluid loss out of the walls of the major
wormholes. High fluid loss results in highly branched
wormhole structures, and therefore reduces the efficiency of
wormhole propagation.
Fluids such as water in oil emulsions4 have been shown to
improve wormhole propagation in the past. These effects were
attributed to the reduced diffusion rates in the bulk acid
solution, but were likely also a result of reduced fluid loss
from the main wormhole. In this work, we have
unambiguously tested the benefit of reducing fluid loss from a
wormhole by saturating the matrix with an inert gas (nitrogen)
prior to injection of the acid. This process will not affect the
diffusion of acid in the wormhole, but will change fluid loss
because of the reduced relative permeability to the aqueous
phase in the matrix surrounding the wormhole. The process
studied is also distinct from the process of injecting CO2 ahead
of acid solutions in sandstone oil reservoirs5. In that process,
displacement of the oil is thought to be a primary cause of
beneficial effects of the CO2 injection.
A series of experiments were conducted in this study to
examine the effect of nitrogen injection ahead of the acid on
the wormhole structures created, and, hence, on the efficiency
of the acidizing process. Metal castings of the wormholes
were made to study the generated wormhole patterns.
Experiments without gas injection were also performed to
provide a direct measure of the effect of gas injection. Finally,
experiments were also conducted with oil saturating the matrix
before acid injection. These experiments provided further
evidence of the effect of fluid loss on wormhole propagation.
Experiment Apparatus and Procedures
The experiments were conducted using 6-inch long and 1 inch
diameter cores of Texas Cream chalk. This rock is a
homogeneous carbonate with no vugs or fractures, and is
composed of greater than 99% CaCO3. The core samples had
permeabilities and porosities of about 6 md and 28%,
respectively. The gas used in the experiments was nitrogen
and decane was used as the oil phase in experiments
including oil. The acid in all experiments was a 15 weight %
solution of HCl.
Figure 2 shows the experimental apparatus. The core
sample was held in a Hassler-sleeve type coreholder, with
confining pressure of 1500 psi applied to the sleeve. A back
pressure of 1000 psi was maintained in all experiments.
Liquids were pumped through the core sample using a
positive displacement pump. Nitrogen was supplied from a
high pressure gas cylinder through a throttling valve.
A typical experimental procedure for an experiment in
which gas was injected ahead of the acid was as follows.
After the core was placed in the coreholder and confining
pressure applied, the core was evacuated. Brine was then
pumped through the core to establish initial saturation of the
pore spaces with brine. The backpressure valve was then set
to 1000 psi and nitrogen injection started. Gas injection
continued until no more brine was observed in the effluent,
indicating that the core had reached residual water saturation.
Finally, acid was injected at a constant rate until wormhole
breakthrough at the exit of the core was observed.
The pressure drop across the core sample was
continuously monitored during each experiment to determine
when a wormhole had propagated through the entire core.
Because the wormholes are such large structures, the pressure
drop though the wormhole is very small compared with the
pressure drop through the original rock. Thus, wormhole
breakthrough was indicated by the time the pressure drop
across the core reached near zero. This was confirmed in
many experiments by also monitoring the pH of the effluent.
Wormhole breakthrough was indicated by a sudden drop in
pH when acid solution was able to pass through a wormhole
through the entire core. The volume of acid needed to
propagate a wormhole through the entire core normalized by
dividing by the initial core pore volume (the pore volumes to
breakthrough, PVbt) was determined by measuring the
pumping time from the start of acid injection until wormhole
breakthrough was observed and by measuring the volume of
liquid effluent collected. The breakthrough pore volumes
reported for all experiments was the volume of acid solution
only and did not include any gas or oil volumes that may also
have been produced from the core.
After each acidizing experiment was completed, a
Wood’s metal casting of the wormholes formed by the acid
was made. The cores were cased in a PVC pipe and Wood’s
metal placed on top of the core sample. Upon heating in an
oven to about 200 °F, the Wood’s metal drained into the core.
The core was then cooled to solidify the metal, all remaining
carbonate rock dissolved with acid, and the metal casting
recovered. A complete description of the experimental
procedures is given by Shukla6.
Experimental Results and Analysis
To evaluate the potential benefit of gas injection prior to acid
injection in carbonates, we varied the experimental conditions
extensively to clearly determine the effect of prior gas
injection on the acidizing process. The parameters that were
changed were temperature, gas injection method, injection
rates, and initial saturating fluids. All of the experimental
conditions used are summarized in Table 1. Our primary
objective with these tests was to determine if the injection of
gas prior to acid injection improved the efficiency of
wormhole propagation, as evidenced by the volume of acid
required to propagate a wormhole through the core sample.
SPE 82273
First, a series of experiments without gas injection was
performed. Then, a similar set of experiments was conducted
with gas injection and the results compared to provide a direct
indication of the effect of gas injection on the volume of acid
required for wormhole breakthrough. We attempted whenever
possible to conduct pairs of experiments in which the only
difference between the pairs was whether or not gas had been
injected before the acid. We used two temperatures, room
temperature (21 °C) and 50 °C. The initial conditions of the
core were either brine saturated or oil and brine saturated with
the water at its residual saturation.
The primary results of the experiments are summarized in
Table 2. The key indication of the efficiency of the
wormholing process in each experiment is the acid pore
volumes to breakthrough given in the last column. This is the
amount of acid that was need to propagate a wormhole
through the 6-inch long core; the smaller this number, the
more efficient the wormholing process.
Acid injection into brine saturated cores. Experiments No.
29 and 30 give a good comparison of the wormholing
behavior with and without gas injection ahead of the acid.
Both Experiments 29 and 30 used similar sized cores, with
15% HCl solution at an injection rate of 1.83 ml/min. Both
experiments were performed at 50 oC. Experiment #29 was on
a water-saturated core with no gas injection. In Experiment
#30, gas was injected prior to acid injection, creating a gas-
saturated core with residual water saturation. In Experiment
#29, 0.44 pore volumes (9 mls) of acid were required for
wormhole breakthrough. In Experiment #30, however, of only
0.28 pore volumes (5.6 mls) were required to
achieve breakthrough.
The smaller volume of acid needed to propagate the
wormhole through the core when gas was injected can be
understood by examining the structures of the wormholes
created with and without gas injection. Figure 3 shows the
metal castings of the wormhole structures created in these two
experiments. The wormhole created in the gas-saturated core
is narrower and has less branching than the wormhole created
in the water saturated core, explaining the smaller acid volume
needed for the gas injection case. Since less wormhole volume
has been created in the presence of gas, less acid has been
consumed by the time the wormhole breaks through to the end
of the core. We attribute this difference to the reduced fluid
loss through the walls of the main wormhole because of lower
relative permeability to water in the matrix surrounding the
wormhole when gas is present. With less convective transport
of acid to the walls, fewer branches are created and the
wormhole diameter is enlarged less, as is observed from
the castings.
Another direct comparison of experiments with and
without gas injection is Experiments #16 and #28. Both of
these experiments were conducted on water-saturated cores at
an acid injection rate of 4.12 ml/min at 50 °C. Experiment #16
was with gas injection and Experiment #28 without any gas
injection. Without gas injection, 0.52 pore volumes of acid
3
were required for wormhole breakthrough, while only 0.21
pore volumes were needed in the gas injection case. The
castings of the wormhole structures for these experiments
(Figure 4) show a larger diameter main wormhole and more
branching when there was no gas injection, just as occurred in
Experiments 29 and 30.
The results of all the experiments conducted at room
temperature with the core initially brine saturated are
summarized in Figure 5. The acid pore volumes to
breakthrough required in the case of gas-saturated cores are
1.5 – 3 times less than those required for water-saturated
cores. Figure 6 shows a similar comparison of the acid pore
volumes required for breakthrough for experiments with gas-
saturated and water-saturated cores at a temperature of 50 oC.
Just as in the room temperature experiments, the acid
volumes required to propagate wormholes through the gas-
saturated cores was 1.5 – 3 times less than the volumes
required for water-saturated cores.
Acid injection into oil saturated cores having residual
brine saturation. In contrast to these cases, when the core
was initially oil saturated, injection of gas had no apparent
effect on the wormholing process. Figure 7 shows the Wood’s
metal castings for Experiments #37 and #38. Both of these
experiments were conducted on oil-saturated cores at an acid
injection rate of 2.3 ml/min. Experiment #37 was without gas
injection and Experiment #38 with gas injection. The volume
of acid needed for wormhole breakthrough in the two
experiments was virtually identical – 0.24 pore volumes
without gas injection and 0.27 pore volumes with gas
injection. The wormhole in the gas-saturated core is as
densely branched as the wormhole in the oil-saturated core
and of the same thickness. Apparently, the relative
permeability to water in the matrix surrounding the main
wormhole is about the same when oil is present in the matrix
at residual water saturation as when gas has displaced the
initial oil. This result is to be expected for a water-wet
medium. The acid volume requirements for the cases when
the cores were initially oil saturated are summarized in Figure
8. The acid volumes were very similar for both cases, with
slightly less acid needed for wormhole breakthrough with no
gas injection.
The effect of oil saturation prior to acid injection
compared with gas injection ahead of the acid is also seen by
comparing experiments with gas injected into water saturated
cores prior to acid injection with the experiments with oil
saturated cores before acid injection. This compares acid
injection into gas saturated cores with no oil present with acid
injection into oil saturated cores with no gas present. Such a
comparison is shown in Figure 9, which summarizes the
results of Experiments 4, 8, 12, 34, 36, 37, and 39. It appears
that whether the non-wetting phase is oil or water
is inconsequential.
Acid injection into cores having residual oil saturation. To
further explore the effect of the presence of oil on the
wormholing process, we conducted another series of
experiments in which the oil in the core was displaced with
4 SPE 82273
brine before the injection of acid. These experiments
simulated acid injection into a formation at residual oil
saturation, a likely initial condition for acidizing if an
aqueous preflush has preceded the acid injection. These
experiments mimicked the results obtained with only brine
present in the core prior to gas or acid injection. The volume
of acid needed for wormhole breakthrough when gas was
injected ahead of the acid was on the order of ½ to 1/3 less
than when acid was injected with no gas (Figure 10). These
results further support the supposition that reduced relative
permeability to water promotes the propagation of a major
wormhole. The oil present only at residual saturation has a
small influence on water relative permeability, and thus, the
gas injection in these experiments has almost the same effect
as when no oil was present.
Alternating injection of gas and acid. Acid treatments are
sometimes conducted with so-called “energized” fluids, a
procedure in which nitrogen gas is added continuously to the
acid stream. A two-phase injection system is difficult to
reproduce with small core tests, particularly since phase
segregation may occur in the wellbore, leading to the gas and
liquid injection not being coincident. Our experimental
apparatus did not permit continuous addition of gas to the
acid, so to emulate the simultaneous injection of gas and acid,
we conducted a few experiments in which gas and acid
injection were alternated, with approximately one minute
intervals of injection of each phase. Figure 11 shows the
wormhole castings for Experiments #2, #12 and #46. All three
of the experiments were conducted on water-saturated cores at
an acid injection rate of 1 ml/min. Experiment #2 was without
any gas injection, Experiment #12 was with continuous gas
injection, and Experiment #46 had alternating gas and acid
injection. The pore volumes required to breakthrough were
highest for the alternating gas/acid injection experiment and
the pore volumes were lowest for the continuous gas injection
method. The wormhole in the alternate gas injection case was
the thickest and both the no gas injection and the alternate gas
injection wormholes had larger amounts of branching
compared with the continuous gas injection case. We infer that
the slugs of gas between the acid slugs tended to block the
acid from the main wormhole path, leading to more branching,
and thus, less efficient wormhole propagation.
Conclusions
This study has demonstrated that the injection of nitrogen gas
ahead of acid injection into carbonate rocks decreases the
amount of acid needed to propagate a wormhole through a 6
inch core sample. Compared with a sample that is initially
water saturated, the gas injection reduced the acid volume by a
factor of 1.5 to 3 times. When gas was injected, the
wormholes were narrower and less branched than those
formed under equivalent conditions without gas injection.
Presumably, the increased efficiency in creating wormholes
when gas is first injected is because of the reduced fluid loss
from the wormhole, which in turn results from the reduced
relative permeability to water in the gas saturated matrix.
Essentially identical results were obtained when the core
was saturated with oil at residual brine saturation. Again, the
increased wormhole propagation efficiency is attributed to the
lower relative permeability in the matrix to the acid solution,
resulting in less fluid loss through the walls of the
main wormhole.
When gas and acid were alternated, the efficiency of the
acidizing process was less than in the case of no gas injection.
This result suggests that the presence of gas in a propagating
wormhole (as opposed to the presence of gas in the matrix
surrounding a wormhole) causes more branching by blocking
the transport of acid to the tip of the main wormhole.
These results suggest that matrix acidizing of carbonates
can be enhanced by injecting a preflush of nitrogen or oil
ahead of the acid. This should lead to deeper wormhole
penetration with the same volume of acid.
Nomenclature
rw = wellbore radius
rwh = radius penetrated by wormholes
s = skin factor
Acknowledgements
The authors thank the sponsors of the Improved Well
Performance Research program for support of this work.
References
1. Economides, Michael J., and Nolte, Kenneth G., eds.:
Reservoir Stimulation, 3rd ed., John Wiley and Sons Ltd.,
Chichester, England, 2000.
2. Hung, K. M., Hill, A. D., and Sepehrnoori, K.: “A
Mechanistic Model of Wormhole Growth in Carbonate
Matrix Acidizing and Acid Fracturing,” Journal of
Petroleum Technology, 41, No. 1, p. 59-66, January 1989.
3. Huang, T., Hill, A. D., and Schechter, R. S.: “Fluid Loss:
The Keys to Wormhole Initiation and Propagation in
Carbonate Acidizing," SPE Journal 5 (3),
September 2000.
4. Hoefner, M. L. and Fogler, H. S.: “Effective Matrix
Acidizing in Carbonates Using Microemulsions,” Chem.
Eng. Prog., May, 1985.
5. Gidley, J. L., Brezovec, E. J. and King, G. E.: “An
Improved Method for Acidizing Oil Wells in Sandstone
Formations,” SPE Production and Facilities, Feb., 1996.
6. Shukla, Suneet, “Gas Assisted Acidizing Of Carbonate
Reservoirs,” M. S. thesis, University of Texas at Austin,
May 2002.
SPE 82273 5

Table 1 Experimental Conditions

Series Initial Fluid Acid Injection Temperature Rock Type Secondary Gas
Saturation Rate Liquid Injection
Saturation
O
A Brine Varied from 70 F (Room Texas Cream None No
0.25 ml/min to Temperature) Chalk
8 ml/min
O
B Brine Same as set A 70 F (Room Texas Cream None Yes
Temperature) Chalk
o
C Brine Same as set A 50 C Texas Cream None No
Chalk
o
D Brine Same as set A 50 C Texas Cream None Yes
Chalk
O
E Oil Same as set A 70 F (Room Texas Cream None No
Temperature) Chalk
O
F Oil Same as set A 70 F (Room Texas Cream None Yes
Temperature) Chalk
O
G Oil Same as set A 70 F (Room Texas Cream Water No
Temperature) Chalk
O
H Oil Same as set A 70 F (Room Texas Cream Water Yes
Temperature) Chalk
O
I Brine Same as set A 70 F (Room Texas Cream None Inject with
Temperature) Chalk acid
6 SPE 82273

Table 2 Experimental Results

Expt No. Temperature Initial Saturating Fluid Gas Injected Injection Acid PVbt
Rate
(ml/min)
1 Room Water No 2.7 0.38
2 Room Water No 1.0 0.25
3 Room Water No 1.5 0.33
4 Room Water Yes 2.7 0.38
5 Room Water Yes 1.83 0.24
6 Room Water No 5.3 0.49
7 Room Water Yes 4.12 0.26
8 Room Water Yes 2.7 0.28
9 Room Water Yes 5.8 0.30
10 Room Water Yes 8.0 0.40
12 Room Water Yes 1.0 0.16
13 Room Water Yes 1.5 0.13
14 Room Water Yes 0.5 0.18
15 Room Water Yes 0.3 0.20
o
16 50 C Water Yes 4.12 0.21
o
17 50 C Water Yes 5.8 0.20
o
19 50 C Water Yes 1.18 0.28
o
20 50 C Water Yes 0.5 0.45
o
21 50 C Water No 0.5 0.8
o
22 50 C Water Yes 1.5 0.48
o
23 50 C Water No 1.18 0.56
o
24 50 C Water No 1.83 0.31
o
26 50 C Water No 5.8 0.55
o
28 50 C Water No 4.12 0.52
o
29 50 C Water No 1.83 0.44
o
30 50 C Water Yes 1.83 0.28
o
31 50 C Water Yes 2.7 0.25
o
32 50 C Water Yes 1.18 0.32
33 Room Water No 2.3 0.5
34 Room Oil No 1 0.15
35 Room Oil Yes 1 0.24
36 Room Oil No 1 0.17
37 Room Oil No 2.25 0.24
38 Room Oil Yes 2.25 0.27
39 Room Oil No 2.25 0.33
40 Room Oil Yes 3 0.31
41 Room Oil then Water Yes 1 0.11
42 Room Oil then Water No 0.5 0.3
43 Room Oil No 3 0.28
44 Room Oil then Water Yes 0.5 0.14
45 Room Oil then Water No 1 0.26
46 Room Water Alternate 1 0.63
47 Room Water Alternate 2.1 0.48
48 Room Water Alternate 3 0.42
49 Room Water Alternate 4 0.37
SPE 82273 7

1
Figure 1. Wormhole structures .

PR PG vacuum pump

PR pump acid Pump

water brine
accumulator

water
N2 PG hydraulic oil Electrical
Enerpac pump
1500 psi Oven
Core
PG 1000 psi Holder PT
PT
Back 2000 psi 1200 psi
pressure

Back Pressure
Regulator
To drain

mixed fluid nitrogen PR: pressure regulator

hydraulic oil water/brine PG: pressure gauge
Acid vacuum PT: pressure transducer
Computer

Figure 2. Experimental apparatus.

8 SPE 82273

A B

Figure 3. Wormhole castings from Experiments 29 and 30;

(A) without gas injection and (B) with gas injection.

A B

Figure 4. Wormhole castings from Experiments 28 and 16;

(A) without gas injection, and (B) with gas injection.
SPE 82273 9

0.6

0.5
Acid Pore Volume Injected

0.4

0.3

0.2

With Gas
0.1
Without Gas
0.0
0.0 1.0 2.0 3.0 4.0 5.0 6.0 7.0 8.0 9.0
Acid Injection Rate (ml/min)

Figure 5. Summary for water saturated cores at room temperature.

0.9

0.8 With Gas

0.7
Without Gas
Acid Pore Volume Injected

0.6

0.5

0.4

0.3

0.2

0.1

0
0 1 2 3 4 5 6 7
Acid Injection Rate (ml/min)

Figure 6. Summary for water saturated cores with or without gas injection at 50 °C.
10 SPE 82273

A B

Figure 7. Wormhole castings from Experiments 37 and 38;

(A) without gas injection and (B) with gas injection.

0.35

0.30
Acid Pore Volume Injected

0.25

0.20

0.15

0.10

With Gas
0.05
Without Gas
0.00
0 0.5 1 1.5 2 2.5 3 3.5
Acid Injection Rate (ml/min)

Figure 8. Oil saturated cores with and without gas injection at room temperature.
SPE 82273 11

0.4
oil-saturated, no gas
0.35
water-saturated, with gas

0.3
PVbt

0.25

0.2

0.15

0.1
0 0.5 1 1.5 2 2.5 3
injection rate (ml/min)
Figure 9. Comparison of gas and oil saturation effects.

0.35

0.3
Acid Pore Volume Injected

0.25

0.2

0.15

0.1

0.05 With Gas

Without Gas
0
0 0.2 0.4 0.6 0.8 1 1.2
Acid Injection Rate (ml/min)

Figure 10. Oil saturated cores at residual oil saturation

with and without gas injection at room temperature.
12 SPE 82273

A B C

Figure 11. Wormhole castings from Experiments 2, 12, and 46;

(A) without gas injection, (B) with gas injection,
and (C) with alternating gas and acid injection.