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Performance comparisons for the SDVA system in Attempts were made to measure the effective diffusion
dolomite and limestone cores at 200 to 208oF are shown in coefficient of the SDVA system using a rotating disk
Fig. 8. The SDVA fluid resulted in wormhole breakthrough apparatus. However, a direct measurement of the SDVA
after 1.1 and 1.6 pore volumes injected into 4.5 and 0.5 mD diffusion coefficient by rotating disk is not possible because of
dolomite cores. The maximum pressure ratios (dPmax/dPo) its highly non-Newtonian behavior. Anomalies in the rate of
were 20 and 4, respectively. Two experiments were also reaction and the scatter in the data were observed due to a
conducted in limestone cores at a similar temperature. The transition from reverse flow to toroidal flow to centrifugal
cores used were of 1.7 and 38 mD, and the responses showed flow (all of which are laminar flow regimes), which occurs
similarly effective stimulation as observed for the dolomite with non-Newtonian fluids as the rotating speed is increased.18
cores. These results demonstrate that the generation of both In addition, the complex viscosity gradient during SDVA
CaCl2 and MgCl2 during the reaction of acid with dolomite is spending could have affected the ability to obtain
not detrimental to the effectiveness of the viscoelastic representative samples during the spending process. The
surfactant in stimulation and diversion. highly viscous nature of the fluid also prevented the use of a
diffusion cell for the diffusion coefficient measurements.
Acid Fluid-Loss Tests. Acid fluid loss-tests were These same problems occur when trying to measure the
performed to compare the SDVA with that of a self-diverting effective diffusion coefficients of crosslinked gelled acids.
polyacrylamide polymer system (XLGA) under constant Unfortunately, despite these technical issues, erroneous data
pressure conditions. Straight 15% HCl and a linear gelled acid have been used to incorrectly claim that gelled acids are
(GA) (incorporating 70 lbm/thousand gal of a polyacrylamide highly retarded.19
polymer) were also included in the comparison. Fig. 9 shows To overcome these measurement issues, the theory of the
the fluid-loss tests for these fluids. The XLGA system has a existence of an optimum Damköhler number was used to
comparable initial viscosity to the unspent SDVA fluid of estimate the apparent effective diffusion coefficient from the
about 30 cp at 170 1/s and 70oF, and both exhibit the same pore volume-to-breakthrough curve for SDVA. It is reported
leakoff control characteristics. An additional experiment was that the minimum number of pore volumes to breakthrough
conducted in which a mutual solvent [10% EGMBE in KCl occurs for a variety of acid and chelant systems at about the
brine] was injected as a preflush to the SDVA system and the same optimum Damköhler number of 0.29.15-17 Under the
results show no detrimental impact to leakoff control. As assumption that SDVA follows the same dependency on the
expected, the straight HCl without diverter and the GA system Damköhler number, an approximate effective diffusion
show lower leakoff control than the self-diverting fluids. coefficient of 2.5E-05 cm2/s was estimated for SDVA at
The effects of temperature on the leakoff characteristics of 200oF. For comparison, straight 15% HCl, gelled 15% HCl,
SDVA are shown in Fig. 10. Significant leakoff control was and emulsified 15% HCl have effective diffusion coefficients
achieved with limestone cores over the temperature range of of about 5.0E-05 cm2/s, 3.1E-05 cm2/s, and 2.5E-06 cm2/s,
150 to 250oF. respectively, at 200oF.20 Hence, the apparent effective
diffusion coefficient is estimated to be slightly lower than that
Fluid Efficiency. Wormhole formation during the for straight HCl and comparable to that of gelled acid.
injection of an acid in a carbonate core is typically
characterized by the number of pore volumes required for Regained Permeability. The effects of various acid
wormhole breakthrough (PVbt) as a function of the injection systems on the regained permeability were evaluated under
rate. Fig. 11 shows the number of pore volumes to two experimental conditions. In the first type of experiment,
breakthrough for SDVA and straight HCl injected in limestone one pore volume of the acid system was injected such that the
cores in the 1 to 3 mD permeability range. The data for 3.4% wormhole did not break through the core. These experiments
and 15% HCl were reported by Wang et al.14 The SDVA were designed to evaluate the cleanup characteristics of the
system exhibits the characteristic pore volumes to fluids under realistic conditions encountered in carbonate
breakthrough curve associated with the transition in wormhole formations (i.e., during acid spending and viscosification in
structure from face dissolution to dominant wormholes to the vicinity of the wormhole). Fig. 12 compares the regained
ramified wormhole. It is noted that a minimum number of permeability of dolomite cores after injecting SDVA and GA
pore-volumes-to-breakthrough for SDVA (ca. 1.1 PVbt) occurs acid systems. It is apparent that the SDVA system causes
at an optimum injection rate of about 1 mL/min at 200oF. This negligible permeability reduction to the core, given that the
optimum injection rate is similar to that observed for 15% HCl regained permeability as a fraction of the original permeability
at 70oF. The optimum injection rate for 3.4% HCl shifts is greater than one (k/ko). However, the polymer system, GA,
towards larger values (from 1 mL/min to 4 mL/min) as the showed a significant reduction in regained permeability with
temperature increases to 122oF based on the data form Wang k/ko values less than 0.1 despite a partial wormhole
et al.14 Additionally, at higher temperature, the acid volume penetrating the core faces. This reduction in permeability
required to breakthrough increases (from 1.5PV to 3.2PV). indicates that residual polymer inhibits the cleanup of
This change in the optimum injection rate has been shown to the cores.
depend on the effective diffusion coefficient of the acid
system and can be predicted based on the theory of the Cleanup Behavior. Although not representative of actual
existence of an optimum Damköhler number.13,15-17 The SDVA spending in carbonate formations, a worst case
SDVA system is expected to exhibit the same dependency. scenario was evaluated in which one pore volume of fully
spent fluid (i.e., viscosified and non-reactive) was injected into
4 SPE 86504
1 in.-diameter by 6 in.-long limestone cores with A series of experiments were conducted according to a
permeabilities ranging from 1.27 to 3.22 mD. Nitrogen or 2 procedure described in the literature24 to evaluate the
wt% KCl solutions were used as displacements fluids under wettability and surface tension of spent acid systems on
constant pressure to simulate the cleanup with gas or carbonate surfaces. A comparison was made with a benchmark
formation fluids. The pressure was increased in 250-psi fluid, typical of that utilized by the industry for carbonate
increments for 30 min until a steady flow rate was detected. acidizing treatments in depleted United States reservoirs: a
The retained permeability was measured after establishing a linear gelled acid (GA) with 15% HCl and a combination of
stable permeability in the production direction using 2 wt% surfactants designed to maximize spent acid cleanup. A spent
KCl brine at 1 mL/min. This test procedure does not represent SDVA fluid formulation (used to stimulate carbonate
actual well treatment conditions as the viscosification process formations in West Texas and Wyoming) was mixed with
is not allowed to occur locally in the pores as a result of acid EGMBE in a 50-50 ratio. Table 1 shows that the surface
reaction, and the viscous fluid will not penetrate the entire tension, contact angle, and capillary pressures (calculated
core, but rather be limited to regions of the porous media in based on a pore diameter of 0.1 microns) are very similar for
and immediately around the wormhole channels. Therefore, the two fluids. A comparison is included in the table for
in these experiments, the viscous fluid penetrates a measurements of two powerful surfactants, a fluorocarbon,
significantly larger percentage of the pore space and will result and an environmentally friendly alternative, Surfactant A,
in unrealistically low regained permeabilities. obtained using sand-packed capillary columns.23 The results
Results for relative cleanup pressures for SDVA using 2% show that the SDVA system in contact with mutual solvent,
KCl are shown in Fig. 13. A mutual solvent based on representative of mixing during well flow back, is strongly
ethylene glycol monobutyl ether (10% EGMBE in KCl brine) water-wetting and induces a comparatively low capillary
was used as preflush to aid in the cleanup. The polymer-based pressure. Another experiment was conducted using spent
XLGA shows the highest flow initiation pressure (FIP) and SDVA without EGMBE, also demonstrating that the system
was used as the baseline to normalize the other data to a was water wetting. The surface tension measurement was not
percentage. SDVA exhibited a FIP of about 40% of that possible due to limitations of the experimental method whilst
required to initiate cleanup of XLGA. Using EGMBE as a using viscous non-Newtonian fluids.
preflush for SDVA further reduced the flow initiation pressure
of the SDVA fluid to about 20%. As seen in Fig. 13, the Acid Conductivity Tests. Acid conductivity tests were
regained permeability of the core after the spent XLGA performed to evaluate the fluid-loss characteristics and acid
injection was relatively low at 6%, compared to 97% (SDVA) conductivity achieved with straight 15% HCl and SDVA.
and 80% (SDVA with the EGMBE preflush). It should be Tests were performed with Edwards limestone cores at 240oF.
noted, that the pressure was increased by 250 psi increments, The 15% HCl resulted in a large amount of dissolution near
leading to an experimental error of approximately ±15%. the entrance of the flow cell (left end of cores in Fig. 15) and
Fig. 14 presents the results using nitrogen as displacement created a large wormhole that broke through the 2.5 in. thick
fluid. SDVA shows the highest FIP, which can be reduced by core within about 1.2 min (Fig. 17). The acid-etched fracture
38% using EGMBE as a preflush. The SDVA/ EGMBE (FIP conductivity was 137 mD-ft at a closure stress of 2,000 psi
of 62%) system has a comparable FIP to that of XLGA (FIP of and decreased significantly at about 2,500 psi closure stress
50%). However, the regained permeability for SDVA (65 to due to the crushing of the acid etched fracture faces (Fig. 18).
100%) is significantly higher than that observed for the XLGA In contrast to straight HCl, SDVA created effective
system (12%). differential etching of the fracture faces (Fig. 16) and provided
These cleanup experiments represent a worst-case scenario leakoff control with a wormhole that broke through in about
in which spent acid gel was unrealistically forced through a 2.5 min (Fig. 17). Therefore, leakoff control was observed
low-permeability core. These tests do, however, show that under acid fracturing conditions. The differential etching of
any spent SDVA gel that enters the matrix is removed at least the fracture faces resulted in a fracture conductivity of 1,426
as easily as XLGA systems, which have been applied mD-ft at 2,000 psi and 147 mD-ft at 4,500 psi closure
successfully on a global basis. With XLGA as the benchmark, pressure.
we show that the final regained permeability is significantly The conductivity results demonstrate that SDVA exhibited
better with the SDVA systems. 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),
Surface Tension and Capillary Pressure Measurements. resulting in higher conductivity than observed with HCl.
Numerous studies have been performed that demonstrate
the impact of surface tension and contact angle on capillary Conclusions
pressure generated by various fluids in porous media.21,22 This Laboratory tests confirm the good performance of viscoelastic
is a very important aspect to consider in the formulation of all fluids as diverting agents in field applications.
well stimulation fluids. In fact, the industry has developed
surfactants, specifically designed to ensure a water-wet • SDVA provides highly efficient wormholing
formation, reduce surface tension and minimize capillary behaviour in limestone and dolomite cores over a
pressures to facilitate recovery of both treatment fluids and wide range of conditions.
pay zone hydrocarbons.23 • SDVA exhibits similar pressure responses and
leakoff behavior as in situ crosslinked gelled acids.
SPE 86504 5
• SDVA and XLGA exhibit significantly better leakoff 4. Mukherjee, H., Gudney, G.: “Extension of acid fracture
control than straight HCl and non-crosslinked penetration by drastic fluid loss control”, paper, JPT, Feb.
gelled acid. 1993.
5. Saxon, A., Chariag, B., Reda, M.: “An Effective Matrix
• Core flow and acid fracture conductivity tests both Diversion Technique for Carbonate Formations”, SPE
demonstrate good leakoff behavior with SDVA. 37734, presented at the 1997 Middle East Oil Show held in
Hence, SDVA can be effectively used to control Bahrein, 15-18 March 1997.
leakoff during acid fracturing treatments. 6. Taylor D., Kumar P.S., Fu D., Jemmaly M., Helou H.,
• The pressure response observed during the injection Chang F., Davis S., and Al-Mutawa M.: "Viscoelastic
of SDVA increases with increasing initial core Surfactant based Self-diverting Acid for Enhanced
permeability and is similar for limestone and Stimulation in Carbonate Reservoirs,” paper SPE 82263
dolomite cores. presented at the 2003 SPE European Formation Damage
Conference in Den Hague, The Netherlands, May 13-14.
• SDVA exhibits similar or better cleanup behavior 7. Chang F., Qi Q., Frenier W.: "A Novel Self-Diverting-Acid
than polymer based acid systems, as demonstrated by Developed for Matrix Stimulation of Carbonate
the low FIP and the high regained permeabilities Reservoirs," paper SPE 65033 presented at the 2001 SPE
using gas or brine as displacement fluids. The data International Symposium on Oilfield Chemistry held in
show that the spent SDVA system should be more Houston, Texas, February 13-16.
easily recovered from low-reservoir-pressure 8. Al-Mutawa, M,. Al-Anzi, E., Ravula, C., Al Jalahmah, F.,
environments than in-situ cross- linked gelled Jemmali, M., Samuel, E. and Samuel, M.: “Field Cases of a
acid systems. Zero Damaging Stimulation and Diversion Fluid from the
Carbonate Formations in North Kuwait”, SPE 80225,
• Differential etching of the fracture faces was created presented at the International Symposium on Oilfield
when SDVA was used to stimulate Edwards Chemistry held in Houston, Texas, 5-8 February 2003.
limestone cores at 240oF. This differential etching 9. Al-Muhareb, M., Nasr-El-Din, H., Samuel, E., Marcinew,
resulted in higher conductivity with SDVA than that R. and Samuel, M.: “Acid Fracturing of Power Water
observed with straight HCl. Injectors: A New Field Application Using Polymer-free
Fluids”, SPE 82210, presented at the 2003 SPE European
Acknowledgements Formation Damage Conference in Den Hague, The
The authors would like to thank ChevronTexaco and Netherlands, May 13-14.
10. Artola, P., Alvarado, O., Huidobro, E., and Salmorán, A.:
Schlumberger for the permission to publish this paper.
“Non-Damaging Viscoelastic Surfactant-Based Fluids Used
Special thanks to Toan Bui, Jack Lie, and Aaron Galt for their for Acid Fracturing Treatments in Veracruz Basin,
hard work on laboratory testing. Thanks to Dr. Ernie Brown, Mexico”, SPE 86489, presented at the International
Curtis Boney, Dr. Dan Fu, and Dr. Steve Davies for Symposium and Exhibition on Formation Damage Control
discussions and for the critical reading of the manuscript. held in Lafayette, Louisiana, U.S.A., 18–20 February 2004.
11. Crowe C.W., Hutchinson B.H., Trittipio: “Fluid Loss
Nomenclature Control: The Key to Successful Acid Fracturing”,
SPE16883 presented at the 1987 62nd Annual Technical
Da = Damköhler number Conference and Exhibition of the Society of Petroleum
Engineers held in Dallas, Texas, September 27-30.
De = effective Diffuision coefficient, cm2/s
12. Navarrete, R.C., Holms, B.A., McConnell, S.B., and
dPo = baseline pressure drop to brine Linton, D.E.: "Emulsified Acid Enhances Well Production
dPmax/dPo = maximum pressure ratio in High-Temperature Carbonate Formations", paper SPE
FIP = flow initiation pressure, psi 50612 presented at the 1998 SPE European Petroleum
L = length scale, cm Conference, The Hague, The Netherlands, October 20-22.
PV = pore volumes 13. Fredd, C.N.: "Advances in Understanding and Predicting
PVbt = pore volumes to breakthrough Wormhole Formation", Reservoir Stimulation, 3rd Edition,
PVinj = pore volumes injected Edited by K. Nolte and M. Economides, (2000).
Q = injection rate. cc/min 14. Wang Y., Hill A.D., Schechter R.S.: “The Optimum
Injection Rate for Matrix Acidizing of Carbonate
Formation,” paper SPE 26578 presented at the 1993 68th
References Annual Technical Conference of the Society of Petroleum
1. Williams, B.B., Gidley J.L. and Schechter R.S.: Acidizing Engineers held in Houston, Texas, October 3-6.
Fundamentals, first edition, Society of Petroleum 15. Fredd, C.N., and Fogler, H.S.: "Optimum Conditions for
Engineers of AIME, New York, NJ (1979).
Wormhole Formation in Carbonate Porous Media:
2. Economides M. and Nolte K.: Reservoir Stimulation, Influence of Transport and Reaction", SPE J., 4 (3),
second edition, Prentice Hall Inc., Englewood Cliffs, NJ (Sept. 1999).
(1989). 16. Fredd, C.N. and Miller, M.J.: "Validation of Carbonate
3. Lynn, J.D. and Nasr-El-Din, H.A.: “A Core Based Matrix Stimulation Models", SPE 58713 presented at the
Comparison of the Reaction Characteristics of Emulsified SPE International Symposium on Formation Damage
and in-situ Gelled Acids in Low Permeability, High Control, Lafayette, LA, February 23-24, 2000.
Temperature, Gas Bearing Carbonates,” paper SPE 65386 17. Fredd, C.N. and Fogler, H.S.: "Influence of Transport and
presented at the 2001 SPE International Symposium on Reaction on Wormhole Formation in Porous Media",
Oilfield Chemistry held in Houston, Texas, February 13-16. AIChE J., 44 (9) 1933-1949 (Sept. 1998).
6 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.
dP/dPo
Regulator
K/Ko
Fluid
10.0 0.100
1.0 0.010
100
dPmax/dPo
SDVA GA
10
XLGA HCl
1
1 10 100 1000
Initial Perm [mD]
Figure 7. Pressure buildup during the injection of various acid
Residual systems as function of permeability (limestone and dolomite)
polymer
damage 45 1.8
Dolomite Limestone
40 1.6
dPmax/dPo
35 1.4
PV(bt)
30 1.2
dPmax/dPo
PV(bt)
25 1
20 0.8
15 0.6
10 0.4
5 0.2
30
10000.00 100.0000 GA
SDVA
1000.00 10.0000 25
Fluid Loss [mL]
XLGA
100.00 1.0000
dP/dPo
HCl
20
K/Ko
0.01 0.0001
10
8.0 10.0 12.0 14.0 16.0 18.0 20.0 22.0
Pore Volume 5
o
Figure 9. Leakoff characteristics for various acid systems at 150 F
using 1 to 3 mD Indiana limestone cores.
SPE86504 9
30
120 120
25 250 F Rel. FIP
Leak-off (ml)
3.4%HCl; 122F
6 120 120
5
4 100 Rel. FIP 100
Figure 11. Pore volumes to break through versus injection rate for 20 20
SDVA and HCl.
0 0
SDVA XLGA SDVA/EGM BE
1.50
k/ko
1.00
0.50
0.00
SDVA/16 mD GA/3.6 mD GA/0.7 mD
1200 10000
GA
SDVA HCl
1000 SDVA
Fluid Loss [ml/min]
1000
Conductivity
HCl
800
(mD-ft)
600
100
400 10
200
1
0
0 2000 4000 6000 8000
0 0.5 1 1.5 2 2.5 3
Closure Stress (psi)
Time^0.5
Figure 18. Acid fracture conductivity results with SDVA, GA and
o o
Figure 17. Fluid loss during conductivity experiments at 240 F. HCl with Edwards limestone at 240 F.
The rapid increase in fluid loss rate corresponds to wormholes
breaking through the 2.5 inch thick cores.