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Journal of Petroleum Science and Engineering 59 (2007) 257 262

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New formula for acid fracturing in low permeability gas reservoirs:

Experimental study and field application
Z. Zhou a , X. Wang a , Z. Zhao a , Y. Xu a , K. Li b,c,
a

Changqing Petroleum Exploration Bureau, PetroChina, China

b
Peking U., China
c
Stanford U., United States

Received 4 October 2006; received in revised form 12 February 2007; accepted 17 April 2007

Abstract
One of the main stimulation techniques to enhance gas production in low permeability reservoirs is acid fracturing. Controlling
the leak-off of reactive fluids is the key to a successful acid fracturing. In this study, new chemicals and techniques have been
developed to control the leak-off by increasing the viscosity of the fluid systems after the acid fracturing fluids were injected into
formations. The initial viscosity of the acid fluids was low. The viscosity increased with the increase in the amount of acid injected.
Experiments have been conducted in laboratory to prove the efficiency of leak-off control using the new chemicals. The
experimental results showed that the new fluid systems reduced the leak-off significantly compared to the gelled and normal acids.
The leak-off rate of the new fluid systems was close to that of non-reactive fluids. Because the targeted reservoirs had a high
temperature, the thermal stability was also tested and the results showed that the new chemical fluids were stable at 120 C.
Because of the remarkable experimental results, acid fracturing stimulations have been conducted using the new chemical fluid
systems in 26 wells in Changqing gas field. The production performance has been evaluated after acid fracturing using the new
chemicals. The field test results showed that the gas production was increased remarkably using the new chemical fluids and
techniques, compared to the routine gelled acid fracturing. A plan has been embarked to apply the proposed techniques in
Changqing gas field widely because of the satisfactory pilot field test results and the low cost of the chemicals.
2007 Elsevier B.V. All rights reserved.
Keywords: Acid fracturing; Leak off control; New chemical; Low permeability; Experimental study; Field application

1. Introduction
Changqing (Jingbian) gas field is a Paleozoic Erathem
dolomite reservoir and is characteristic of low porosity,
Corresponding author. Stanford U., United States.
E-mail addresses: zzq_cq@petrochina.com.cn (Z. Zhou),
wangxd_cq@petrochina.com.cn (X. Wang),
zzf_cq@petrochina.com.cn (Z. Zhao), xyg_cq@petrochina.com.cn
(Y. Xu), kewenli@stanford.edu (K. Li).
0920-4105/$ - see front matter 2007 Elsevier B.V. All rights reserved.
doi:10.1016/j.petrol.2007.04.007

low permeability, and low productivity. The permeability

ranges from 0.1 to 2.1 mD. The depth of the gas reservoir
ranges from 3000 to 3700 m and the temperature from
99.6 to 113.5 C. The average pressure gradient of the gas
reservoir is about 0.945 MPa/100 m and the average initial
reservoir pressure is around 32.4 MPa.
Jingbian gas field is a very heterogeneous dolomite
reservoir. Usually it is difficult to conduct a successful
acid fracturing stimulation. The reason is described briefly
in the following. The high permeability zones usually

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Z. Zhou et al. / Journal of Petroleum Science and Engineering 59 (2007) 257262

Fig. 1. Difference between LCA and gelled acid.

have a tendency to absorbing more acid fracturing fluid

than the low permeability zones. So, the longest and the
most conductive fracture is generally developed and
propagated in such high permeability sections. The low
permeability zones may not get necessary treatments if
these intervals are perforated and treated simultaneously
as pointed out by Rahim and Al-Qahtani (2003).
During the period from 1986 to 1990, conventional
acid fracturing, gelled acid fracturing, multi-stage acid
fracturing (including a closed fracture acidizing stage)
were adopted as main stimulation technologies to
improve reservoir production in Changqing gas field;
these technologies have played an important role for
large-scale development in the Jingbian gas field. As
reservoir production continues, well productivity keeps
decreasing year by year, and the number of lowproduction wells has also increased gradually. To further
improve well production and final recovery in this tight
gas reservoir, it is necessary to perform deep penetrating
stimulation for the carbonate gas field. To this end, new
chemicals and techniques have been developed to
control the leak-off by increasing the viscosity of the
fluid systems. Experiments have been conducted in
laboratory to prove the efficiency of leak-off control
using the new chemicals. Pilot acid fracturing tests were
also conducted and the results were evaluated.

2.1. Development of leak-off control acid

There have been reports to study and use leak-off
control fluids (Pichler et al., 1992; Vitthal and
McGowen, 1996; McGowen and Vitthal, 1997). Coulter
et al. (1976) reported that the leak-off might be
controlled by using viscous, non-reactive fluids. Shumaker et al. (1978) demonstrated that the leak-off of the
reactive fluids in carbonate reservoirs could be controlled to the extent that actual productivity increased
closely approximate those predicted by computer design
program. Welton and van Domelen (2006) developed a
unique in-situ crosslinkable acid system that uses a
blend of HCl/formic acid as the base acid and a synthetic
polymer gelling agent.
The main purpose of this study was to develop leak-off
control acid (LCA) systems with a satisfactory performance to reduce leak-off significantly and with a low cost.
The mechanism of LCA is simple and briefly described in
the following. The initial viscosity of LCA was designed
at a low value so that the LCA fluids could be injected into
the targeted formation easily. The value of pH of the liquid
system decreases as the acid reacts with the rock. The
Table 1
Functional components of the new LCA
Items

Code
name

Corrosion
inhibitor
Corrosion
inhibiting supporter
Fe3+ stabilizer
Leak-off reducer

HSJ-1 Protect the oil pipe from being

eroded
ZJ-1
Work as an assistant agent in the
component of the corrosion inhibitor
LS1-1 Stabilize Fe in the acid fluid
LS1-2 Increase the viscosity of the
tired-acid
DSGA Increase the viscosity of the acid fluid
YQ-1 Reduce the surface tension of the acid

2. Development and evaluation of chemicals

There are many parameters to influence the efficiency of acid fracturing stimulation in low permeability gas
field. These include heterogeneity of formation (Rahim
and Al-Qahtani, 2003), acid returns (Taylor et al., 2000),
leak-off (Charles and Xie, 1997; Gjnnes et al., 1998),
etc. In this study, we focused on the leak-off control to
improve the efficiency of acid fracturing.

Gelled acid
Surfactant

Function

Z. Zhou et al. / Journal of Petroleum Science and Engineering 59 (2007) 257262

Fig. 2. Change in viscosity of different acid fluids with pH value.

unique feature is that the viscosity of LCA increased

sharply when the value of pH decreases to a specific
value. The almost instant increase in viscosity can reduce
the leak-off significantly and then delay the acid reaction
so as to enhance the acid penetration. The reduction of
leak-off is also helpful to maintain the activity of LCA
injected later and to increase the length of fractures. The
coefficient of utilization of the acid-fracturing fluid can be
improved accordingly.
The main difference between LCA and gelled acid is
shown in Fig. 1. Initially the viscosity of gelled acid is
high and is then reduced with the increase in the pH
value. In contrast, initially the viscosity of LCA is low
and then increased with the increase in the value of pH
(24) as LCA fluids react with rock; finally the viscosity
of LCA decreases as the value of pH is greater than a
specific value (pH N 4).
A novel LCA fluid system with a low leak-off and a
low cost was developed. The additives with specific
function are listed in Table 1. Some of the functional
components are iron ion stabilizer, chemicals for
reducing leak-off, corrosion inhibitor, and surfactant.

259

Fig. 3. Comparison of leak-off coefficients among different acidfracturing fluids.

test whether the LCA fluids developed in this study

behave as supposed, experiments were conducted to
measure the viscosity of LCA at different values of pH.
The results are shown in Fig. 2. One can see that the
viscosity of the developed LCA fluid increases first and
then decreases with the pH value, as expected. The
initial viscosity of the LCA was about 40 cP. The
maximum viscosity was about 150 cP with a corresponding pH value around 2.5. Such a high viscosity
can reduce the leak-off rate significantly. The final
viscosity was 20 cP approximately. The property of low
viscosity at the high pH value can facilitate and improve
the liquid return rate, which can help enhance the
stimulation efficiency. Also shown in Fig. 2 is the effect
of pH value on the viscosity of gelled acid. The results
show that the viscosity of gelled acid almost does not
change (slightly decrease) with the pH value ranging
from 0 to about 6.0. No viscosity peak was observed. So
it may not reduce the leak-off significantly.
Note that the actual maximum viscosity of LCA may
be much greater than the maximum value shown in
Fig. 2. This was because the chemical reaction between

2.2. Evaluation of leak-off control acid

Crosslink reaction is expected to happen when the
pH value in LCA fluids increases, which causes the
increase in viscosity of LCA. The further increase in the
pH value will reduce the viscosity of LCA, however. To
Table 2
Experimental results of dynamic leak-off tests
Serial
Acid fluid
number style
1
2
3

Brine
permeability
(mD)

Normal acid 0.2285

Gelled acid 0.1268
LCA
0.0965

Velocity of the Leak-off

acid injection
coefficient
(ml/min)
(m/min1/2)
2
5
5

1.323 10 3
5.146 10 4
2.594 10 4

Fig. 4. Relationship between leak-off and time for different acidfracturing fluids.

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Z. Zhou et al. / Journal of Petroleum Science and Engineering 59 (2007) 257262

acid and rock was fast and it was difficult to control the
pH value at a specific value or in a narrow range due to
the limitation of experimental conditions. According to
our visual observation, the status of the LCA varied from
low viscosity liquid to high viscosity gel-like liquid.
3. Evaluation of the dynamic leak-off
Actual reservoir rock from Changqing gas field was
used to conduct the dynamic leak-off tests to evaluate
the performance of the novel LCA in controlling leakoff. The reservoir depth of sampling was 3663.5 m. The
core samples looked tight and the values of permeability
measured using brine were listed in Table 2. The sizes of
all the core samples (cubic) were 2 2 2 cm. Microfractures were also observed in these core samples.
Experiments were conducted at a temperature of 90 C,
close to reservoir temperatures. Three different types of
acids, normal acid, gelled acid, and LCA, were used to
conduct the comparison of leak-off. The procedure was
similar to those reported by Vitthal and McGowen
(Vitthal and McGowen, 1996). The experimental results
of dynamic leak-off are shown in Fig. 3 and also listed in
Table 2. One can see from Table 2 that LCA had the
lowest value of leak off. Compared with the normal acid
and the gelled acid, the leak-off of the LCA was reduced
by about 75% and 36%, respectively.
Fig. 4 demonstrates the relationship between leak-off
and time for different acid-fracturing fluids. One can see
from Fig. 4 that the LCA had the smallest volume of
leak-off at a specific time. The normal acid fluid had the
greatest leak-off.
McGowen and Vitthal (1996) reported that the leakoff volume (linear gel, etc.) from dynamic leak-off tests
was proportional to the square root of time. Charles and
Xie (1997) presented this model in more detail later. To
test this, the relationship between leak-off and the square
root of time is plotted in Fig. 5. The data from LCA fluids

Fig. 5. Relationship between leak-off and square root of time for

different acid fracturing fluids.

Fig. 6. Residual acid concentrations in rock for different acidfracturing fluids.

show an approximately linear relationship between leakoff and the square root of time but the other two fluids do
not demonstrate such kind of linear relationship.
Acidrock reaction rate mainly depends on the
transportation speed of H+. The increase in viscosity of
LCA can reduce the transportation speed of H + .
Therefore the acidrock reaction rate in LCA can be
decreased so as to increase the penetrating distance of the
acid. To test this, three different acid fluids were used and
experiments of acidrock reaction were conducted. The
results are shown in Fig. 6. The solid squares represent
the results of the residual acid concentration after the
reaction between LCA acid fluid and rock was completed; the solid triangles represent the gelled acid and
the solid diamonds represent the normal acid (see Fig. 6).
One can see from Fig. 6 that LCA has the highest residual
acid concentration, which represents that the acidrock
reaction rate in LCA is the lowest. A lower acidrock
reaction rate is helpful to penetrate deeper formation
during acid-fracturing.
4. Results of field tests
Field tests of LCA fracturing were conducted in a
remote onshore dolomite reservoir, Jingbian gas field,
located in northwestern China. Initially the gas reservoir
is slightly under-pressurized with a pressure of about
32.4 MPa (average value). The gas interval is the Lower
Paleozoic Mawu l, in which Mawu 13 is the main pay
zone with an air permeability of 0.015.0 mD. The target
formation for field tests of LCA fracturing consists of
heterogeneous dolomite deposits and occurs at various
depths ranging from 3100 to 3700 m. This formation has
a net pay ranged from 0.8 to about 5 m, porosity from 1.2
to 10.3%, and effective permeability of less than 2.1 mD.
All of the wells in the region were stimulated by
conventional fracturing in an attempt to achieve
commercial production and to improve productivity.

Z. Zhou et al. / Journal of Petroleum Science and Engineering 59 (2007) 257262

261

Table 3
Results of field tests of acid-fracturing
Well number

Blend of acid

Formation thickness
(m)

Porosity
(%)

Permeability
(mD)

Gas saturation
(%)

Gas production
(104 m3/day)

3
3A

LCA/Normal acid
LCA/Gelled acid

3.6
2.8

8.6
9.0

0.899
1.057

84.4
85.7

39.8
6.0

Because of high Youngs modulus and high net pressure,

placement of proppant inside fractures was always a
problem in the past. The stimulation results demonstrated
a very limited success. Actually, most of the wells suffered
from low production rates and could not produce
commercially even after conventional acid fracturing
measures. Due to this, the new formula of LCA was used
in the acid fracturing for 26 wells in the same area.
A pilot field test was discussed here to show the
effectiveness of the new LCA. Two nearby wells with
similar rock and fluid properties were acid-fractured
using different blend of acid fluid systems. As shown in
Table 3, the values of the porosity of the formations in
those two wells were 8.6 and 9.0% respectively; the
values of the permeability were 0.899 and 1.057 mD
respectively; the initial gas saturations were 84.4 and
85.7% respectively. One can see from Table 3 that the
rock properties and the fluid saturation of the formations
in the two wells were very close. Well 3 was acidfractured using a blend of LCA/normal acid and Well
3A was acid-fractured using a blend of gelled/normal
acid. The reason to use normal acid was to increase the
conductivity of the fracture; the use of LCA could
increase the length of the fracture. The volume of used
LCA was about 50 m3 and the volume of normal acid
was about 25 m3. The well test results after the acidfracturing showed that the use of the blend of LCA/
normal acid increased the gas production over six times
compared to the use of the blend of gelled acid/normal
acid (see Table 3).
Over 26 wells have been acid-fractured using the new
LCA fluid system in Jingbian gas field because of the
remarkable increase in gas production from the pilot
tests. Most of the wells resulted in satisfied gas
production after acid-fracturing by using the new LCA
fluid system. In summary, the absolute open flow
production rates in most of the wells stimulated using
the new LCA fluids increased from 1 to over 6 times,
compared to the conventional acid fracturing treatments.
Many gas wells reached a commercial gas production
after stimulation using the new LCA fluids.
However the increase of gas production in some
wells was still very limited. Our analysis showed that all
of the unsuccessful wells had a porosity of less than
5.6%. The reason for the failure of the stimulation might

be because the formation in these wells with a porosity

of less than 5.6% was too tight to be acid fractured
efficiently. We have embarked a research project to
target these very tight formations.
5. Conclusions
The following conclusions may be drawn from the
present study:
1. A novel LCA fluid system was developed to reduce
the leak-off of acid-fracturing fluid significantly at a
temperature as high as 120 C.
2. Compared with the normal acid, the leak-off of LCA
was reduced by about 75%; compared with the gelled
acid, the leak-off of LCA was reduced by about 36%.
3. The pilot test results showed that the use of the blend
of LCA/normal acid could increase the gas production over six times compared to the use of the
combination of gelled acid/normal acid.
Acknowledgments
Financial support from PetroChina is gratefully
acknowledged. The authors also thank PetroChina for
the permission to publish these results.
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