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1uu (10)
Where K
i
is the initial core permeability in md, and K
f
is the final core permeability in md.
Coreflood #2, Bandera sandstone, Fig. 3: For this test, the regular sandstone acid was evaluated without injecting a
preflush or postflush stage of HCl acid. Initially 5 wt% NH
4
Cl was injected at rate of 5 ml/min, then reduced to 2 ml/min
to determine the initial permeability. The acid injection rate was then kept constant at 2 ml/min until the end of the
experiment. As the regular sandstone acid entered the core, the pressure drop continuously increased from 10 to 40 psi.
This is an indication of damage inside the core, and in fact the final measured permeability reflected a 67.5 permeability
reduction. It is most probably due to CaF
2
and MgF
2
precipitation because the Bandera cores contained 5 wt% dolomite.
Secondary and tertiary precipitation also likely came from clay minerals.
Table 2 shows the summary of the four experiments to show the effect of adding preflush and postflush of HCl. The
highest permeability enhancement was obtained when only a preflush stage of HCl was used (Experiment #3: Table 2)
followed by the case where both preflush and postflush stages were used (Experiment #1: Table 2). As discussed earlier,
the Bandera cores contained HCl-sensitive clay; therefore, the HCl postflush stage damaged the core. The need for a
postflush stage must be confirmed before use because it can damage the permeability of sandstone that has HCl-sensitive
clay mineral (illite, chlorite, and kaolinite). However, in the cases without the preflush stage of HCl, it became apparent
that a postflush of HCl was important to reduce the damage from the HF acid: See Table 2, experiments #2 and 4, where
the permeability reduction was reduced from 67.5 to 53.3. Ultimately, however, regular sandstone acid should be used
with a preflush stage of HCl acid to maximize its performance and minimize any CaF
2
/MgF
2
precipitation and damage.
One-Step Sandstone Acid
As discussed earlier, four different fluid formulas (Acids A, B, C, and D) were selected to be tested as one-step
sandstone acid systems without any preflush or postflush stages of HCl acid. The main difference among the four
formulations is the HCl:HF ratio:
Acid A is equivalent to 15 wt% HCl + 1.9 wt% HF
SPE 164491 5
Acid B is equivalent to 10 wt% HCl + 2.3 wt% HF
Acid C is equivalent to 5 wt% HCl + 2.6 wt% HF
Acid D is equivalent to 3 wt% HCl + 2.8 wt% HF
Coreflood #5, Bandera sandstone, Fig. 4: The 5 wt% NH
4
Cl solution was injected at 5 ml/min then reduced to 2
ml/min to determine the initial core permeability. Acid A was injected inside core #5 at rate of 2 ml/min. As expected
because of the high HCl concentration of Acid A, the pressure drop increased from nearly 12 to 154 psi within the first 2
PV of Acid A injection. After that, the pressure drop decreased rapidly for the next 2 PV to 40 psi. The decrease in the
pressure drop slowed upon reaching 12 psi (initial pressure drop), after total injection of 12 PV. At the end of the
experiment, 113% permeability enhancement was calculated.
Coreflood #6, Bandera sandstone, Fig. 5: The 5 wt% NH
4
Cl solution was injected at 5 ml/min then reduced to 2
ml/min to determine the initial core permeability. Acid B was injected inside core #6 at rate of 2 ml/min. The pressure
drop increased from nearly 12 to 120 psi within the first 3 PV of Acid B injection. After that, the pressure drop decreased
rapidly for the next 3 PV to 38 psi. The decrease in the pressure drop slowed upon reaching 12 psi (initial pressure drop)
,after total injection of 15 PV. At the end of the experiment, 104% permeability enhancement was calculated.
Corefloods #7-8, Bandera sandstone, Figs. 6 and 7: Acids C and D produced the same ressure drop performance as
Acid A and B. The pressure drop while injecting Acid C initially increased to 108 psi within the first 3 PV; after about
16 PV of Acid C, 86% permeability enhancement was calculated. For Acid D, the initial pressure drop increased to 75
psi while injecting the first 4 PV, and it took 18 PV to achieve 54% of permeability enhancement.
From Figs. 4-7, it is clear that all selected acid formulations (Acids A, B, C, and D) can successfully stimulate
Bandera sandstone cores. However, each formulation shows a different pressure drop performance with different final
permeability enhancement. Table 3 summarizes the results of Corefloods #5-8 (Figs. 4-7). Acid A gives the maximum
observed pressure drop, followed by B, C and D, in that order. Also, Acid A gives the highest permeability enhancement
with the lowest acid volume, followed by B, C and D, in that order. Because of the additional additives that control the
release and the reaction of HF and the high HCl:HF ratio, Acid A behaves similarly to HCl acid. This can be
demonstrated clearly by comparing the pressure drop curves while injecting the HCl preflush stage and while injecting
Acid A (Figs. 2 and 5), where the pressure drop increased significantly with 2 PV of injection. Therefore, as the HCl:HF
ratio decreased (changing from Acids A to D), the maximum observed pressure drop decreased.
The Bandera sandstone contains HCl-sensitive clay mineral (illite, chlorite, and kaolinite). Therefore, when Acid A
entered the core, the pressure drop significantly increased due to damage from reacting HCl with illite, chlorite, and
kaolinite. Overall, this type of damage is not permanent or significant, at least for the Bandera sandstone or sandstones
with similar compositions. The HCl content in Acid D is smaller, and so HCl-induced damage is lower. This is why the
lowest maximum pressure drop is observed for Acid D. However, HF-induced damage is higher in Acid D than in Acid
A. This type of damage develops slowly, as shown in Fig. 3 (when only regular acid is used) and is difficult to remove.
Table 3 demonstrates this: A larger volume of Acid D is required to achieve positive permeability enhancement,
compared with the other one-step acid systems. Based on these results, the one-step sandstone acid formulations that
have high HCl:HF ratio (like Acids A and B) are recommended for formations with high carbonate content and low HCl-
sensitive clay content. Conversely, one-step sandstone acid formulations with lower HCl:HF ratio (like Acids C and D)
are recommended for sandstone formations with low carbonate content and more HCl-sensitive clay. However for the
cores that has both high carbonate content and low HCl-sensitive clay content, Acids B & C should be tested.
Effect of Acid Pore Volume
In these experiment different volumes of Acid C was injected in different Bandera sandstone cores to study the effect of
injected acid volume on the final permeability enhancement. Results of these experiments were shown in Table 4. The
final core permeability was increased by increasing the injected acid volume. However, it is important to highlight that
there is a minimum acid volume need to achieve a final permeability greater than initial value (Coreflood #9-10). This
minimum depends on the HCl:HF ratio of the acid system and the composition of sandstone formation. For the Bandera
sandstone, at least 8PV of Acid C were required to achieve permeability enhancement.
Effect of Sandstone Composition
Sandstone is composed of small grains that are cemented by siliceous, felspathic or calcareous cementing material. The
cementing material determines the durability of the sandstone. Berea sandstone core, which has less clay mineral than
Bandera, will have different response when treated by the new one-step sandstone acid. Therefore, 4 PV of Acid C was
injected inside a Berea sandstone core. Table 5 shows the differences in compositions between Bandera and Berea
sandstone core. A significant different in permeability enhancement was observed: a 33% permeability reduction in the
Bandera compared with 86% permeability enhancement in the Berea. It was clear that a higher permeability
enhancement will be obtained for the core that has less clay and carbonate content.
6 SPE 164491
In the next experiments, 8 PV of Acid C were injected into cores obtained from three different sandstone formations
(FM #1, FM #2, and FM #3). Table 6 shows the compositions of the three cores and compares the permeability
enhancement of these cores after injection of 8 PV of Acid C with Bandera sandstone core. Core from FM #1 has slightly
higher quartz content than Bandera sandstone. Also, it has less clay and carbonate content. However, the main difference
is the higher feldspar content. Comparing the permeability enhancement obtained from Bandera and FM 1, it can be
concluded that increased feldspar content significantly reduces the permeability enhancement capability of the new one-
step sandstone acid. A larger volume of the new one-step sandstone acid will be required for sandstone formations with
high feldspar content.
Core from FM #2 has higher quartz content than Bandera sandstone. This core can be considered clean core at 92%
quartz. Therefore, the permeability enhancement of this core was significantly higher than for the Bandera. Core from
from FM #3 also had more quartz than the Bandera, but slightly less than FM #2. In addition, there is slightly less
siderite (3 vs. 2 wt%) and more kaolinite (4 vs. 10 wt%). Permeability enhancement in both cores (FM #2 and FM #3) is
nearly the same. This suggests that kaolinite (a clay mineral) has a minimal effect on achievable permeability
enhancement.
Fractured Sandstone Formation
8 PV of Acid C was injected into two fractured cores: the first has the fracture direction in the direction of acid injection
(parallel direction) and the second has the fracture direction perpendicular to direction of acid injection, Fig. 8. For the
first core, although the tested core composition has a significant amount of illite clay which can cause damage during
sandstone acid injection, a 330% permeability enhancement was calculated, Table 7. Because the acid flows in same
direction as the fracture, acid will react with the fracture face and cause an etching profile that significantly enhances the
permeability of the fracture. In the second core, which with 94% quartz composition should be considered clean, the
same acid volume produced a 165% permeability enhancement. As the acid flow is perpendicular to the fracture, acid
reaction on the fracture face will not significantly enhance the overall core permeability as it does in the case of a parallel
fracture.
Corrosion Test
Table 8 shows the summary of corrosion test result for Acids A, B and C at 180F for 6 hrs using a two pipe grades (Cr-
13 and N-80). Two corrosion inhibitors (CI-A and CI-B) were evaluated at different concentrations. CI-A is preferred to
for Cr-13 pipe grades, and CI-B is preferred for N-80. All results shows low corrosion rate for all tested acids less than
0.03 lb/ft
2
for the three tested acid systems (Acids A, B and C). For both corrosion inhibitor types, increasing the
inhibitor concentration reduced the corrosion rate as it is shown in Test #1-3, Table 8. For both corrosion inhibitors, the
corrosion rate increased as the HCl:HF ratio decreased (Tests #1, 7, and 13). At the same conditions, Acid A has a lower
corrosion rate than Acid B, which has lower corrosion rate than Acid C. Also, only in Acid A, the corrosion rate in Cr-13
pipe grade is less than in N-80 regardless of the inhibitor used (Tests #3 and4, 1 and 5 or 2 and 6). For Acids B and C,
the corrosion rate in Cr-13 pipe grade is higher than in N-80.
Conclusions
This study introduces a new sandstone acid system that eliminates the need for preflush and postflush HCl acid stages,
reduces acid treatment complexity, reduces the HCl volumes needed, and reduces the overall treatment/rig time. Based
on the results obtained, the following conclusions can be drawn:
Regular sandstone acid must be used with a preflush stage of HCl acid to maximize its performance and
eliminate CaF
2
/MgF
2
precipitation. The need for a postflush stage must be confirmed with testing, as it can
damage sandstone that has HCl-sensitive clay mineral.
All selected one-step sandstone acid formulations (Acids A, B, C, and D) were able to successfully improve
permeability of Bandera sandstone cores.
For Bandera sandstone cores, increasing HCl/HF ratio increased the permeability enhancement and reduced the
injected acid volume.
Using the same acid volume and composition, a higher permeability enhancement was observed for a core that
had less clay and carbonate content.
Based on HCl:HF ratio and sandstone composition, a minimum acid volume is required to achieve a
permeability enhancement.
For Acid C, the feldspar content of sandstone can significantly affect the permeability enhancement acid, while
kaolinite content has no obvious effect.
All tested formulas had a very low corrosion rate (less than 0.03 lb/ft
2
).For both corrosion inhibitor types (CI-A
and B), the corrosion rate increased by reducing the HCl:HF ratio and/or inhibitor concentration.
SPE 164491 7
Recommendation
Three main steps are involved in conventional sandstone matrix treatment: preflush, main acid stage, and postflush.
However, based on the results obtained from this study Four one-step sandstone acid formulations (Acids A, B, C, and
D) were able to successfully improve permeability of sandstone cores. Formulations with high HCl:HF ratio (like Acid
A and B) are recommended for formations with high carbonate content and low HCl sensitive clay content While
formulations with lower HCl:HF ratio (like Acid C and D) are recommended for sandstone formations with low
carbonate content and more HCl-sensitive clay. However for the cores that has both high carbonate content and low HCl-
sensitive clay content, Acids B & C should be tested.
References
Bryant, S.L. and Buller, D.C. 1990. Formation Damage from Acid Treatments. Journal of SPE Production
Engineering 5(4): 455 -460.
Crowe, C.W. 1986. Precipitation of Hydrated Silica from Spent Hydrofluoric Acid: How Much of a Problem is it?
Journal of Petroleum Technology 38(11): 1234 - 1244.
Economides, M.J. and Nolte, K.G. 2010. Reservoir Stimulation. 3rd Edition, John Wiley Sons, ISBN: 0471491926
Ch 13 and 18.
Economides, M.J., Hill, A.D., and Economides, C.E. 1993. Petroleum Production System.. Prentice Hall PTR, New
Jersey, Ch. 14 and 15.
Gdanski, R. 1996. Kinetics of Tertiary Reactions of Hydrofluoric Acid on Aluminosilicates. Journal of SPE
Production & Facilities 13(2):75-80.
Gdanski, R.D. 1994. Fluosilicates Solubilities Impact HF Acid Compositions. Paper SPE 27404 presented at the
SPE Symposium on Formation Damage, Lafayette, Louisiana, USA, 7-10 February.
Hartman, R.L., Lecerf, B., Frenier, W., Ziauddin, M., and Fogler, H.S. 2006. Acid-Sensitive Aluminosilicates:
Dissolution Kinetics and Fluid Selection for Matrix Stimulation Treatments. Journal of SPE Production &
Operations 21(2): 194-204;
Ke, M. and Qu, Q. 2010. Method for Controlling Inorganic Fluoride Scales. US Patent 778138.
Kline, W.E. and Fogler, H.S. 1981. Dissolution Kinetics: Catalysis by Strong Acids. Journal Of Colloid And
Interface Science 82(1) 93:102.
Lullo, G.D. and Rae, P. 1996. A New Acid for True Stimulation of Sandstone. Paper SPE 37015 presented at the
6
th
SPE International Asia Pacific Oil & Gas Conference, Adelaide, Australia, 28-31 October.
Martin, A.N. 2004.Stimulating Sandstone Formations with non-HF Treatment Systems. Paper SPE 90774
presented at the SPE Annual Technical Conference and Exhibition, Houston, Texas, USA, 26-29 September.
Nasr-El-Din, H.A., Hopkins, J.A., Shuchart, C.E., and Wilkinson, T. 1998. Aluminum Scaling and Formation
Damage due to Regular Mud Acid Treatment. Paper SPE 39483 presented at the International Symposium on
Formation Damage Control, Lafayette, Louisiana, USA, 18-19 February.
Simon, D.E. and Anderson, M.S.1990. Stability of Clay Minerals in Acid. Paper SPE 19422 presented at the SPE
Formation Damage Control Symposium, Lafayette, Louisiana, USA, 22-23 February.
Smith, C.F. and Hendrickson, A.R. 1965. Hydrofluoric Acid Stimulation of Sandstone Reservoirs. Journal of
Petroleum Technology 17(2): 215222.
Smith, C.F., Ross, W.M. and Hendrickson, A.R. 1965. Hydrofluoric Acid StimulationDevelopments for Field
Application. Paper SPE 1284 presented at the SPE Annual Meeting, Denver, Colorado, USA, 3-6 October.
Thomas, R.L., Nasr-El-Din, H.A., Lynn, J.D., Mehta, S., and Zaidi, S.R. 2001. Precipitation During the Acidizing
of a HT/HP Illitic Sandstone Reservoir in Eastern Saudi Arabia: A Laboratory Study. Paper SPE 71690
presented at the SPE Annual Technical Conference and Exhibition, New Orleans, Louisiana, 30 September-3
October.
Thomas, R.L., Nasr-El-Din, H.A., Mehta, S., Hilab, V., and Lynn, J.D. 2002.The Impact of HCl to HF Ratio on
Hydrated Silica Formation During the Acidizing of a High Temperature Sandstone Gas Reservoir in Saudi
Arabia. Paper SPE 77370 presented at the SPE Annual Technical Conference and Exhibition, San Antonia,
Texas, USA, 29 September-2 October.
Wamser, C.A. 1948. Hydrolysis of Fluoboric Acid in Aqueous Solution. J. Am. Chem. Soc. 70:12091215.
Williams, B.B., Gidley, J.L., and Schechter, R.S. 1997. Acidizing Fundamentals. SPE Monograph Volume 6,
chapters 3, 4, 8 and 9.
8 SPE 164491
Table 1: The mineralogy of the Bandera sandstone cores.
Mineral Composition Wt%
Quartz 61
Feldspar 15
Dolomite 5
Illite 12
Kaolinite 4
Chlorite 2
Table 2: Summary of the core test results for regular sandstone acid system.
No.
Injection Fluid Sequence Permeability
Enhancement, %
Base fluid Preflush Main Treatment Postflush Base Fluid
1 5 wt% NH4Cl 10 wt% HCl regular sandstone acid 10 wt% HCl 5 wt% NH
4
Cl 28
2 5 wt% NH4Cl - regular sandstone acid - 5 wt% NH
4
Cl -67.5
3 5 wt% NH4Cl 10 wt% HCl regular sandstone acid - 5 wt% NH
4
Cl 32
4 5 wt% NH4Cl - regular sandstone acid 10 wt% HCl 5 wt% NH
4
Cl -53.30
Table 3: Summary of the core test results for Acids A, B, C, and D.
No.
Main
Treatment
Maximum Observed
Pressure Drop, psi
Injected
Volume, PV
Permeability
Enhancement, %
5 Acid A 154 12 113
6 Acid B 120 15 104
7 Acid C 105 16 86
8 Acid D 75 18 54
Table 4: The effect of injected acid volume.
No. Main Treatment Injected Volume, PV Permeability Enhancement, %
9 Acid C 4 -33
10 Acid C 8 26
11 Acid C 12 35
7 Acid C 16 86
Table 5: The effect of sandstone composition on the performances of 4 PV of Acid C.
Mineral Composition Bandera Berea
Quartz 61 87
Feldspar 15 3
Dolomite 5 1
Calcite - 2
Illite 12 1
Kaolinite 4 5
Chlorite 2 2
4 PV of Acid C
Permeability enhancement, % -33 86
SPE 164491 9
Table 6: The effect of sandstone composition on the performances of 8 PV of Acid C.
Mineral Composition Bandera FM #1 FM #2 FM #3
Quartz 61 69 92 86
Feldspar 15 23 - -
Dolomite 5 - - -
Siderite 0 - 3 2
Illite 12 2 Tr Tr
Kaolinite 4 4 4 10
Chlorite 2 Tr - -
8 PV of Acid C
Permeability enhancement, % 26 2.5 52.5 53.2
Table 7: The effect of fracture direction on the performances of 8 PV of Acid C.
Mineral Composition
Fracture Direction Is
Parallel To Flow
Direction
Fracture Direction
Is Perpendicular To
Flow Direction
Quartz
57 94
Feldspar 3 Tr
Dolomite - Tr
Calcite - Tr
Illite 33 4
Kaolinite
3 Tr
Chlorite - Tr
Siderite 3 1
8 PV of Acid C
Permeability Enhancement, % 330 165
Table 8: Corrosion test values for Acids A, B, and C at 180
o
F for 6 hrs.
Test
Acid
Type
Metal
Type
Inhibitor Type
Inhibitor
Concentration, gpt
Corrosion Rate,
Lbs./Sq. Ft.
Pitting
1 Acid A Cr-13 CI-A 2 0.0077 0
2 Acid A Cr-13 CI-A 5 0.0044 0
3 Acid A Cr-13 CI-A 10 0.0034 0
4 Acid A N-80 CI-A 10 0.004 1
5 Acid A N-80 CI-B 2 0.0095 1
6 Acid A N-80 CI-B 5 0.0051 0-1
7 Acid B Cr-13 CI-A 2 0.0132 0-1
8 Acid B Cr-13 CI-B 5 0.0123 0
9 Acid B Cr-13 CI-B 10 0.0047 0
10 Acid B N-80 CI-B 2 0.0072 1
11 Acid B N-80 CI-B 5 0.0052 1
12 Acid B N-80 CI-B 10 0.0043 1
13 Acid C Cr-13 CI-A 2 0.0162 1
14 Acid C Cr-13 CI-A 5 0.0267 1
15 Acid C N-80 CI-B 2 0.004 1
16 Acid C N-80 CI-B 5 0.004 0
10 SPE
164491
Fig. 1: Diagram of the coreflood setup.
Fig. 2: Pressure drop across the core during injection of 4PV of preflush of HCl, 8 PV of conventional sandstone acid, 4
PV of postflush of HCl acid, temperature is 180
o
F, acid injection rate is 2 ml/min, and Bandera sandstone core.
Back Pressure
Regulator (1000 psi)
Fraction Collector
Differential Pressure
Transducer
Core Holder
Acid Accumulator
Heated Water
Accumulator
Pump
Heating
System
Data Acquisition
Overburden Pressure Pump
SPE 164491 11
Fig. 3: Pressure drop across the core during injection of only 8 PV of conventional sandstone acid (no preflush or
postflush of HCl acid), temperature is 180
o
F, acid injection rate is 2 ml/min, and Bandera sandstone core.
Fig. 4: Pressure drop across the core during injection of 12 PV of Acid A (no preflush or postflush of HCl acid),
temperature is 180
o
F, acid injection rate is 2 ml/min, and Bandera sandstone core.
12 SPE
164491
Fig. 5: Pressure drop across the core during injection of 15 PV of Acid B (no preflush or postflush of HCl acid),
temperature is 180
o
F, acid injection rate is 2 ml/min, and Bandera sandstone core.
Fig. 6: Pressure drop across the core during injection of 16 PV of Acid C (no preflush or postflush of HCl acid),
temperature is 180
o
F, acid injection rate is 2 ml/min, and Bandera sandstone core.
5ml/min
2ml/min
SPE 164491 13
Fig. 7: Pressure drop across the core during injection of 18 PV of Acid D (no preflush or postflush of HCl acid),
temperature is 180
o
F, acid injection rate is 2 ml/min, and Bandera sandstone core.
Top view of the core that has
fracture direction parallel to
flow direction
Side view of the core that
has fracture direction parallel
to flow direction
Side view of the core that has
fracture direction Perpendicular to
flow direction
Fig. 8: Photos of the fractured sandstone cores
5ml/min