SPE 86494
An Innovative System for Complete Cleanup of a Drill-In Fluid Filter Cake
Brad Todd, Halliburton; Syed Ali, ChevronTexaco E&P Technology Company; Donald L. Whitfill and Tim Haggerty,
Halliburton
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., 18–20 February 2004.
This paper was selected for presentation by an SPE Program Committee following review of
information contained in a proposal submitted by the author(s). Contents of the paper, as
presented, have not been reviewed by the Society of Petroleum Engineers and are subject to
correction by the author(s). The material, as presented, does not necessarily reflect any
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Proposal
As part of a comprehensive program to develop delayed filter
cake breakers, a drill-in fluid with magnesium oxide (mag-ox)
bridging particles and an ammonium chloride-based cleanup
solution was developed. The mag-ox particles are insoluble in
water and standard drill-in fluid-based brine such as sodium
chloride, but these particles are readily soluble in ammonium
chloride or ammonium citrate. Thus, an ammonium chloride-
based cleanup can be formulated that will dissolve the
bridging particles and other drill-in fluid components without
using acid-based systems. Because this technology was of
specific interest for injector well applications, a laboratory
study was undertaken to evaluate this novel system. This
paper summarizes laboratory work and radial flow loop test
results, and discusses possible field applications.
Filter-cake cleanup of injection wells can be especially
problematic because operational constraints often preclude
backflowing the well to remove the residual filter cake.
Consequently, injection remains impaired if the residual filter
cake is not removed by other means. The highly reactive
nature of standard treatments may remove the filter cake at the
point of circulation before the treatment can be placed over the
entire openhole interval. A need exists for cleanup solutions
that have a delayed effect on filter-cake integrity, allowing the
cleanup solution to be circulated across the entire interval.
Preferably, the treatment’s reaction with the filter cake would
commence when the entire solution is in place and continue
until the filter cake is uniformly removed. The ideal placement
of a treatment would be in the gravel-pack carrier fluid, where
it would provide enough of a delayed reaction to allow the
gravel pack to be placed with an alpha/beta wave technique
before fluid-loss control is lost.
Introduction
Many examples can be cited1,2 where the performance of
openhole completions is greatly reduced as a result of damage
caused by drill-in fluid filter-cake residue. Filter-cake cleanup
of injection wells is especially problematic because
operational constraints often preclude backflowing the well to
remove the residual filter cake. In fact, even if flowback is
used to lift off the filter cake, the residual filter cake may
reheal if not removed from the formation face when injection
has started. Consequently, fluid injection remains impaired if
the residual filter cake is not removed by other means.
The cleanup solutions for calcium carbonate-based drill-in
filter cake could be acids, chelating agents, oxidizers or
enzyme treatments, or a combination of these materials. A
common disadvantage of these treatments is that they are
highly reactive and may remove the filter cake at the point of
circulation before the treatment can be placed over the
openhole interval. Consequently, a need exists for cleanup
solutions that have a delayed effect on filter-cake integrity,
allowing the cleanup solution to be circulated across the entire
interval. Ideally, the treatment’s reaction with the filter cake
would commence when the entire solution is in place and
would continue until the filter cake is uniformly removed.
As a part of a comprehensive program to develop delayed
filter-cake breakers, a drill-in fluid with mag-ox bridging
particles and an ammonium chloride-based cleanup solution is
being developed.3 The mag-ox particles are insoluble in water
and standard drill-in fluid-based brine, such as sodium
chloride, but are readily soluble in ammonium chloride
(Table 1: Dissolution of Particulate Solid Bridging Agents
with Ammonium Salt Solutions). Thus, an ammonium
chloride-based cleanup can be formulated that will dissolve
the bridging particles and other drill-in fluid components
without using acid-based systems. Therefore, a laboratory
study was undertaken to evaluate this system.
Experimental Results and Discussion
Metal Salts Soluble in Ammonium Solutions. A number of
metal salts were screened for their solubility in ammonium
solutions. The results are shown in Table 1. Based on
availability, water solubility, specific gravity, and cost, mag-
ox appears to be the best candidate to evaluate for use in drill-
in fluids.
2 SPE 86494
Static Filtration in a High-Pressure High-Temperature
(HPHT) Cell. The equipment used in this study is described
and shown in Appendix A. A filter cake was built, using the
mud formulation shown in Table 2: Drill-In Fluid
Formulation Based on Mag-Ox 10cr for Static Fluid Loss
Testing, on a 35-micron aluminum oxide (aloxite) disk at
150°F and 500 psi differential pressure using a 30-minute
filtration period. The excess mud was poured off and the cell
was loaded with 100 cm3 of 11.8-lb/gal calcium chloride fluid
containing 15 grams of ammonium chloride. The cell was shut
in overnight at 150°F, and 500 psi pressure was applied. After
a 24-hour soak period, the cell was opened and the filter cake
examined. No visible traces of mag-ox remained on the disk.
The particle-size distribution of a commercially available
mag-ox used in this testing is shown in Fig. 1: Particle-size
distribution of mag-ox 10cr.
Dynamic Filtration Studies in the Dynamic Filtration
System. The HPHT test proved that the mag-ox bridging
particles could be removed by ammonium chloride solution,
but did not give an indication of when the break actually
occurred. A similar mud (Table 3: Drill-In Fluid
Formulation for Dynamic Fluid-Loss Testing) was
formulated and placed in the dynamic filtration system
(Appendix A) to build a dynamic filter cake. In this case, Rev
Dust was included to simulate drill solids. The excess mud
was poured off and a 7% ammonium chloride solution was
added to the cell. The system was pressured to 800 psi with a
50-psi differential pressure across the filter cake. The system
was maintained at 150°F. Fig. 2: 7% ammonium chloride-
break of mag-ox-based drill-in fluid, shows that a significant
increase in filtrate rate occurred around 14 hours. Obtaining
these types of delays in break-time with a breaker solution that
is considered to have excellent compatibility with most
sandstone formations and gravel-pack screens is seen as an
area very much worth pursuing.
Radial Flow Model Test. Based on the initial tests described
previously, a mag-ox-based mud system was determined to be
the best option for testing. A radial flow model (Appendix A)
was used to test the mag-ox system. The mud system used for
this test is shown in Table 3. The rheological and fluid-loss
properties before and after the test are given in Table 4:
Rheological and Filtration Properties of the Drill-In Fluid
with Mag-Ox 10cr used in the Radial Flow Test.
Procedure. An initial baseline permeability of the test core
was established using ASTM seawater. The test core was a
10-micron, 3-in. ID × 6-in. aloxite filter core. The seawater
was pumped through the core at 600 mL/min for a total
volume of 25 L. The 10.0-lb/gal drill-in fluid (Table 2) was
conditioned in the flow cell for 2 hours—sheared by flowing
at 200 ft/min for 2 hours—to simulate hot rolling.
A 2-hour dynamic mud-off was started. The mud was
flowed at 150 ft/min, 250 psi, and 150°F. The fluid loss for
this period was 654 mL. Thereafter, a 16-hour static mud-off
was initiated at the same pressure and temperature. The fluid
loss for this period was 400 mL. After the dynamic and static
mud-off period, a 1-hour dynamic scouring was performed at
150 ft/min, 250 psi, and 150°F. Subsequently, the mud was
drained from the flow lines.
The trapped mud in the cell was displaced with 9.8-lb/gal
NaCl brine (conditioned to 150°F) at a rate of 75 ft/min. A
2-hour circulation period was then started at 300 ft/min, 250
psi, and 150°F. This phase was performed to reduce the
thickness of the filter cake. At the conclusion of the circulation
phase, the brine was drained from the flow lines.
The trapped brine in the cell was displaced with the
breaker package (Table 5: Breaker Formulation for Radial
Flow Test) at a rate of 76 ft/min followed by a circulation of
30 minutes at 150 ft/min, 250 psi, and 150°F. After
displacement, an additional 45-min static soak was initiated
with the fluid-loss valve open. This step was taken to help
ensure that breaker was in contact with the filter cake. A
breakthrough occurred 45 minutes after contact with the filter
cake. The flow cell was then shut in and temperature was
increased to 180°F overnight. The cell was opened the
following morning to record the breakthrough and monitor the
fluid loss after the soak period.
The cell was cooled and pressure was removed. The final
permeability was measured using ASTM seawater.
Results of Radial Flow Test. During the filter-cake
deposition, the filtrate rate was monitored. Fig. 3: Filtrate
leakoff during filter-cake deposition for radial flow test,
compares the filtrate rate of the mag-ox-based mud with that
of a previous test with a laboratory-prepared mud for Alba
Field, which should be considered a benchmark for a well-
designed mud. As Fig. 3 shows, the mag-ox-based mud had a
considerably higher leakoff, but was considered acceptable for
continuing the model test. However, additional work is
required to optimize the particle-size distribution of mag-ox to
reduce the filtrate volume.
The breaker solution for this test was not formulated for a
long break, but to provide an effective removal of the filter
cake. The breaker solution was formulated in a 9.2-lb/gal
NaCl brine with 20% ammonium citrate and 2% oxidizing
breaker (OxB). The OxB was included to break down the
starch and xanthan polymer. Fig. 4: Filtrate leakoff during
the breaker soak in the radial flow test, shows that the filter
cake started to degrade at approximately three quarters of
an hour.
The system was shut in to soak overnight. When the
breaker was removed from the system, seawater injection was
performed to obtain percent return permeability. Compared to
the initial permeability, only about 43% return permeability
was noted. At the conclusion of the test, the cell was
disassembled and core removed for inspection (Fig. 5:
Residual filter cake after cleanup in the radial flow test).
The top half of the core was clear of mud, while the bottom
half was layered with undissolved mud cake, most of which
appeared to be the Rev Dust added to simulate drill solids.
This was confirmed by X-ray diffraction where only
ammonium chloride, quartz, halite, kaolin and chlorite were
detected. The layering appeared to be a result of mud cake
sliding from the top and sides to the bottom. The following
observations include problems that were observed during
testing and corrective measures that can be taken to overcome
these problems in future analysis:
Problem 1.
• Problem: The magnesium oxide bridging particles had
a narrow particle-size distribution, which could account
SPE 86494
for thickness of the mud cake and the high volume of
fluid loss during the mud-off phases in this test. The
thickness and strength of the filter cake is apparent by
the retained low fluid loss during the completion brine
circulation period.
• Solution: A multi-sized mag-ox blend would decrease
the fluid loss, thereby laying a thinner filter cake, which
would be easier to dissolve.
Problem 2.
• Problem: Locking the cell overnight for soaking could
have negatively affected the total reaction with the mud
cake. Chemicals were spent and fresh breaker was not
supplied to replace them.
• Solution: A longer period of soaking with the leakoff
valves opened, thereby replacing spent breaker with
fresh, could improve the dissolution of the mud cake.
Overall, the new bridging material looks promising for
ease of clean up. The breaker package was simple to
blend. It is also user and environmentally friendly.
When the desired temperatures were obtained,
breakthrough seemed to increase. In addition, in field
applications to injectors, the initial injection water can
contain breaker, removing any residual polymer and
bridging material.
Problem 3.
• Problem: Drill solids, simulated here by rev dust, are a
major problem preventing complete removal of a filter
cake by chemical means.
• Solution: Either very high dilution rates must be used
to minimize drill solid content, or a new technique such
as pullback under-reaming should be employed.5 With a
conventional drilling approach little can be done to
mitigate the build up of solids in the drill-in fluid other
than dilution and attention to detail on the solids control
equipment. The continual flow of the drill solids-laden
fluid past the drilled borehole will continue to build
solids content in the filter cake.
Another operator company has proposed (and has
field-tested one time) an approach that may be a
solution in many instances. The solution involves using
a pullback under-reamer and opening a pilot hole from
the bottom up. This completion technique can be
applied in openhole gravel packs or horizontal wells to
remove a cuttings bed. It requires that the
drilling/completion rig have a top drive system. When
the hole is opened from the bottom up, drilled solids are
circulated away from the newly opened hole. Cuttings
transport is made easier because the cuttings are
transported in a narrow annulus. Thus, the newly
deposited filter cake only contains those agents used in
preparing the drill-in fluid. Without the incorporation of
drilled solids in the filter cake, the breaking of the filter
cake is more likely to be successful.
A commercial tool is now available that can be
adapted such that the pull back under reaming can be
done in a one step process - drilling and under-reaming
in a single stage.
3
Further Developments
To evaluate the less-than-expected break in the radial flow
tester, the test conditions were replicated in the laboratory
using the modified dynamic filtration equipment previously
described. A drill-in fluid with the same formulation as the
fluid tested in the radial flow tester was run. As expected, in
the case of the dynamic flow tester that deposits an ideal filter
cake, the break time was relatively short, as shown in Fig. 6:
Dynamic breaker test simulating the radial flow test. The
volume of breaker fluid per unit area of filter cake in contact
with the filter cake in the dynamic tester is greater than the
volume per unit area in contact with the filter cake in the
radial flow tester. A second test was run in the dynamic tester
with concentrations of breaker reduced to simulate the lower
amount of total active material available in the radial tester.
Again, as expected, the break time is longer than the initial test
(Fig. 7: Dynamic breaker test simulating lower radial flow
test breaker concentrations), but not as long as in the radial
tester. The 50% increase in break time makes two points:
1. The break time can be controlled to longer times
if desired.
2. The laboratory designs are more accurate for minimum
break times than the total time required.
Consequently, a test system such as the radial tester is
probably more accurate to reflect total break times.
Based on the positive results in the initial laboratory tests
and radial flow test, additional fluid development work is
being performed with various particle-size distributions of
mag-ox and different fluid-loss polymers. The bridging
combinations are being tested in four brines at both low salt
concentrations and near saturation. Screening tests are
performed on 10-, 20-, and 35-micron filter disks. These data
and further developments will be presented in a later paper.
Conclusions
• Drill-in fluids containing mag-ox as the fluid-loss
bridging material, in conjunction with an ammonium
chloride-based delayed breaker system, can offer a
unique approach for completing injection wells, which
is worth pursuing further.
• When a wider particle-size distribution is available for
the mag-ox bridging material, thinner filter cakes
should be possible, resulting in better cleanup.
• A breaker solution based on ammonium chloride can be
enhanced by the addition of citrate ion and formulated
with either oxidizers or enzymes.
Acknowledgements
The authors thank ChevronTexaco and Halliburton for their
support of this study and the permission to publish this paper.
References
1. Alfenone, J., Longeron, D., and Saintpere, S.: “What Really
Matters in Our Quest of Minimizing Formation Damage in Open
Hole Horizontal Wells,” paper SPE 54732 presented at the 1999
SPE European Formation Damage Conference, The Hague, The
Netherlands, 31 May-1 June.
2. Hodge, R. M. et al.: “Evaluation and Selection of Drill-in Fluid
Candidates to Minimize Formation Damage,” paper SPE 31082
4 SPE 86494

presented at the 1996 International Symposium on Formation
Damage Control, Lafayette, Louisiana, 14-15 February.
3. Todd, B.L. et al.: “Well Drilling and Servicing Fluids and
Methods of Removing Filter-cake Deposited Thereby,” U.S.
Patent No. 6,422,314, 2002.
4. Todd, B. and Murphy, R.: “Laboratory Device for Testing of
Delayed-Breaker Solutions on Horizontal Wellbore Filter
Cakes,” paper SPE 68968 presented at the 2001 SPE European
Formation Damage Conference, The Hague, The Netherlands,
21-22 May.
5. Whitfill, D.L. et al.: “Evaluation and Selection of Drill-In and
Completion Fluid Systems for Minimal Damage,” paper AADE-
02-DFWM-HO-08 presented at the AADE 2002 Drilling and
Completion Fluids and Waste Management Conference,
Houston, Texas, 2-3 April.

Table 1—Dissolution of Particulate Solid Bridging Agents with Ammonium Salt Solutions
Solubility
Bridging Agent Ammonium Salt Solution 3
(g/100 cm )
Magnesium Oxide 4 M Ammonium Chloride 1.6
Magnesium Oxide 8 M Ammonium Acetate 2.8
Magnesium Oxide 1.3 M Ammonium Chloride plus 1 M Sodium Citrate 2.8
Magnesium Carbonate 8 M Ammonium Acetate 2.2
4 M Ammonium Chloride
Magnesium Carbonate 2.9
plus 0.4 M Trisodium Salt of Nitrilotriacetic Acid (NTA)
Anhydrite (CaSO4) 4 M Ammonium Chloride 1.7
Anhydrite (CaSO4) 8 M Ammonium Acetate 2.9
Lime (CaOH) 1.3 M Ammonium Chloride 3
Zinc Oxide 4 M Ammonium Chloride 3
Zinc Oxide 1.3 M Ammonium Chloride plus 0.8 M Sodium Citrate 2.9
Zinc Carbonate 4 M Ammonium Chloride 2.4
0.36 M Diammonium Salt of
Lanthanum Oxide 2.2
Ethylenediaminetetraacetic Acid (EDTA)
Manganese Hydroxide 4 M Ammonium Chloride 1

Table 2—Drill-In Fluid Formulation Based Table 4—Rheological and Filtration Properties of the Drill-In
on Mag-Ox 10cr for Static Fluid-Loss Testing Fluid with Mag-Ox 10cr Used in the Radial Flow Test
Component Amount Date Before After
10% NaCl 336 mL Shear Applied Multimixer – 5 min. Multimixer – 5 min.
Xanthan Polymer 0.85 g Test Temp., °F 120 120
Stabilized Nonionic Plastic Viscosity, cP 11 11
7.4 g
Starch Derivative
Yield Point, lb/100 ft² 19 21
Mag-Ox 10cr 25 g
10-sec gel, lb/100 ft² 4 4
10-min gel, lb/100 ft² 6 9
Table 3—Drill-In Fluid Formulation for Dynamic
Fluid-Loss Testing pH 11.5 11.3

Component Amount 600 rev/min 41 43

9.2 lb/gal NaCl 350 mL 300 rev/min 30 32
Xanthan Polymer 1.1 g 200 rev/min 24 27
Stabilized Nonionic Starch Derivative 7.6 g 100 rev/min 18 20
6 rev/min 6 7
Mag-Ox 10cr 43.3 g
3 rev/min 5 5
Rev Dust 7.7 g
Disc, µm 35 35 10
Spurt, mL/30 sec 2.8 2.8 1.9
Total filtrate, mL/30 min 9 8.3 8
Corrected Filtrate, mL 15.2 13.8 14.1
SPE 86494 5

Table 5—Breaker Formulation

for Radial Flow Test
Component Amount
9.2 lb/gal NaCl 350 mL
Ammonium Citrate 20% wt/wt
Oxidizing Breaker OxB 2% vol/vol

DN004208
Fig. 1—Particle-size distribution of mag-ox 10cr.

DN004209

Fig. 2—7% ammonium chloride-break of mag-ox-based drill-in fluid.

6 SPE 86494

DN004210
Fig. 3—Filtrate leakoff during filter-cake deposition for radial flow test.

DN004211

Fig. 4—Filtrate leakoff during the breaker soak in the radial flow test.

DN004212

Fig. 5—Residual filter cake after cleanup in the radial flow test.
SPE 86494 7

DN004229
Fig. 6—Dynamic breaker test simulating radial flow test.

Fig. 7—Dynamic breaker test simulating lower radial flow test breaker concentrations. DN004230
8 SPE 86494
Appendix A
HPHT Cell. The HPHT cell is a hollow cylinder with end
caps, which inlcude one port and valve each. One end of the
HPHT cell is machined to allow a 2.5-in. diameter by 1/4-in.
thick aloxite disk to be installed. Drill-in fluid is poured into
the cell, and the cell is heated and pressurized. When the
temperature reaches the desired level, the bottom end-cap
valve (filter-disk end) is opened for a predetermined amount
of time to build the filter cake.
The following steps were performed for this study:
1. Install the appropriate aloxite disk into the cell.
2. Add drill-in fluid, and close the cell.
3. Apply pressure and heat until the cell is stable.
4. Open the filtrate valve for a predetermined time to
allow flow into the disk.
5. Pour off drill-in fluid, and load the cell with
breaker solution.
6. Allow the breaker to soak for a predetermined time.
7. Determine the extent of the filter-cake cleanup through
returned flow rate or visual inspection.
Dynamic Filtration System. A computer-controlled dynamic
filtration system4 (Fig. A-1) deposits a filter cake on the
internal surface of a cylindrical filter when a differential is
applied. The filter medium is a porous ceramic material
available in several pore sizes (permeability). A shear shaft is
centered within the filter and rotated to provide a uniform and
known amount of shear across the filter surface. The internal
pressure applied to the fluid, the differential pressure applied
across the filter, the shear rate, and the temperature are all
programmable.
Fig. A-1—Dynamic filtration system.
When the filter cake is formed, the excess drill-in fluid is
removed and the cell is loaded with the breaker solution. The
device is programmed with a sequence of timed steps in which
the internal pressure, differential pressure, shear, and
temperature are applied as required.
The following procedure was used:
1. Prepare the drill-in fluid to be tested and hot roll for
16 hours.
2. Assemble the filter core into the core holder with the
shear shaft guide.
3. Load the fluid into the device and program it for filter-
cake formation.
4. Run the filter-cake formation test.
5. When the filter-cake formation sequence is completed,
download and plot the data.
6. Remove the cell from the device and pour off the drill-
in fluid.
7. Rinse the cell and core holder carefully without
disturbing the filter.
8. Load the breaker solution to be tested. Re-install the
cell into the device.
9. Program the device with the breaker test sequence.
10. Run the breaker test.
11. When the test is concluded, download the data, and plot
the leakoff profile.
Radial Flow Model. The radial flow model (Fig. A-2) is used
to scale-up the volumes and to more accurately simulate the
mud placement, displacement, and cleanup in a radial flow
regime. The equipment allows the use of realistic flow rates
according to expected field conditions.
DN004213
SPE 86494 9

DN004214
Fig. A-2—Radial flow model.