.. . .
SPE 39487
Water Quality Requirements and Restoring the Infectivity of Waste Water Disposal
Wells
H.A.Nasr-El-Din, SPE, and A.A. A1-Taq, Saudi Aramco
Copydght 1998, Socie~ of Petroleum Enginwm, Inc,
This paper was prepared for presentation at the 1~ SPE International SymWsium
Formation Damage Control held in Lafayetie, Louisiana, 10-19 February 1%,
on
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Abstract
Water separatedin desaltersand other separationunits in a gas-
oil separation plant contained variable amounts of oil
mntaminan L suspended solids and chemieals. Two nearby wells
are used to dispose the produced water Mm the plant. Due to the
poor quaIity of the waste water and long shut-in peri@ one of the
two wells encountered a si~mt drop in well injtivity.
A thorough investigation was conducted to identify the
damaging mahanism, design a -tment progmrn to -ore the
well injtivity, and ~mmend guidelhes for water quali~
nded to minimize formation damage. The study included
chamcterization of the waste water, and conducting @reflood
experiments to determine the eff~ of total -nded solids, oil
eonten~ particle size, H2S and iron mntent on the permeability of
reservoir cores (sandstone formation). Finally, coreflood
experiments were performed to determine an acid formulation
which can be used to remove formation damage while
maintaining the integrity of the formation (sandstone).
Experimental Ats indicated that the waste water contained
significant amounts of suspended solids (mainly iron tide) and
oil (up to 250 mg/1). Coarse pmticles of more than 500 microns
were present in the waste water. CoreflM rdta indicated that
the waste water severely damaged reservoir mm. Formation of
an external ~ter cake was the damaging mechanism obseIved in
W mrefIood experiments. Iron tide played an important role in
the damage observed in the lab and field studies, The following
water quality requirements were recommended to minimize
loss of infectivity: total suspended material (solids and oil)
should not exceed 50 ppm, mean particle size should not
exceed 4 microns, hydrogen sulfide concentration should not
.
W .,
D
Society of Petroleum Engineers
exeeed 10 ppm, and total iron concentration should not
exceed 2 ppm. Also, to prevent formation damage due to
particle settling, it was recommended to continuously inject
the waste water into the two disposal wells. Shutting in
disposal wells for a long period of time will allow most of the
partictiate material to settle in the pore spaces, which will
of
cause formation darnage and loss of infectivity.
To restore the infectivity of the damaged well, an acid
formtiation was designed which took into account formation
mineralogy, presence of trapped oil, precipitation of iron, and
elemental s*. The treatment was applied in the field
where the acid was injeeted using a 1.5” coiled tubing. Ball
sealers were added to the acid to ensure better diversion. The
treatment was successful, and the well infectivity increased by
more than 400°/0.
Introduction
Water separated from ~e~nt desalters and other separation
units in a gas-oil sepamtion plant in Saudi Arabia contained
variable amounts of oil and suspended solids. Two wells are used
to dispose the plant waste water. Both wells, designated Wells
A and B, were drilled and completed as cased hole in a
sandstone formation. Well “A”, the well of interest in the
present study, was drilled and completed with a 7“ casing and
a total depth (TD) of 7,003 ft in December of 1983. It has 420
R of perforations. The well was put on service in March of
1993 with an estimated injeetion rate of 5,000 bbls/day at an
injection well head pressure (I-) of 900 psi. Then, it was
shut-in in October of 1994 while injection continued to Well
‘B”. After almost a year, injection of waste water into Well
“A” was resumed, however, IWHP was 2000 psi. This high
injeetion pressure indicated that this well was severely
damaged.
The damaging mwhanism which caused loss of infectivity
of Well “ A“ was not known. To treat the well, it was first
assumed that this well was damaged due to the presence of oil
in the injection water. The presence of oil in the injmion
water ean damage the well in several ways. Oil saturation will
increase in the wellbore area and, as a result, brine
permeability will decrease. Heavy hydrocarbons and
asphaltene can precipitate and block some of the pore throats.
565
2 H.A. NASR-EL-DIN AND A.A. AL-TAQ
Change of rock nettability due to organic deposit is also a
possibility. To remove potential damage due to oil invasion,
and restore the well infectivity, 2200 gals of xylene (5 gals/fi
of perforations) followed by 2000 gals of a solution
containing 10 VOlO/O mutual solvent and 0.2 WtO/O of a water
wetting surfactant were circulated in the wellbore. These
chemicals should remove heavy hydrocarbons and restore
rock nettability. The well was backtlowed to a nearby pit,
where large amounts of oil were recovered. However, the well
infectivity remained low where the injection rate was 3,000
bbls/day at 2,200 psi injection pressure. This result indicated
that Well” A“ was still damaged and further treatments were
required.
Two points of concerns arise from the analysis of the well
history. Well” A“ was partially damaged due to the presence
of large amounts of oil in the injection water, This is a serious
concern and the amount of oil should be carefilly monitored.
A second concern is related to shutting-in the well for a long
period of time. If the waste water contains suspended solids,
which is the case as will be discussed later, then these
particles will settle near the wellbore during this period and
will induce severe formation damage. Therefore, it is
recommended to continuously inject the waste water into
these wells.
The objecdves of this study are to: (1) assess the effect of oil
contamination and suspended solids on well infectivity, (2)
understand the mechanisms of formation plugging, (3) develop
remedial actions to restore the injdvity of damaged wells, and
(4) rammend @delines for the quality of injaed water in
terms of suspended oil and solids.
Effect of Water Quality on Well Infectivity
Produ~ water often mntains oil, -nded solids and other
water treatment chemids. The presence of suspended material
(oil and solids) can cause severe decline in well injecdvity,
especially if water is injected below the ficm p~e of the
formation or if the permeability of the fomtion is low (tess than
300 red). Some formations have high ~rmeability streaks
(permeability is higher than fw darcies). Such formations are
idd for injection of produced water where the presenw of solids
or oil will not si@cantly Mi well infectivity.
Seveml ~hers have examined various impairment
mechanisms due to the presence of particles and oil in water
injection and disposal wellsl-14. Amrding to Barkman and
Davidsonl, solid pmticles can impair well inj~vhy through the
following four mechanisms: wellbore narrowing (cake formatio~
invasion of particles deep into the -rvoir, wellbom fill up by
particle settling, and perforation plugging.
Recently, Nasr-El-Din]3 reviewed previous experimental and
theoretical studies done on flow of suspensions and oil-in-water
emtisions in porous media. Aarding to th~ studies, the
damage depends on particle size of the solids and oil present in
the injection water and the pom diameter of the formation. If the
particles are larger @ the average pore throat diameter of the
566
SPE 39407
formatio~ then the particles cannot penetmte the pres. As a
tit an external filter cake with a permeability lower than that
of the formation will fo~ Fig. l-a. This type of damage occurs
very fast and has great impact on well injectivi~. The degree of
plugging and the extent of infectivity dwline depend on (a) rock
characterisdcs, permeability and porosity, (b) oil mntent and drop
size distributio~ (c)flow velocity, and (d) total -nded Solidss.
Another type of injeetivity impairment occurs when the size of
the pardcles p=nt in the injection water is smaller than the
average pore throat diameter of the formation. These particles
will invade the formation and bridge at some pres, Fig. l-b. The
degree of damage is mntrolled by three factors: particle
characteristics, concentration and fluid flow. As solids
conmntration in the injection water is increased, the rate of
permeability decline ~mes higher.
Obviously,if the size of the particles is significantly smaller than
the average pore throat diameter of the forrnatio~ Fig. l-c, then
th= particles will flow through the formation without causing
any damage. As a -~ there will & no loss of infectivityfor a
long ~riod of time The presenm of solids in the injection water
can cause other types of darnage. For particles invasion
mec~su Barkman and Davidsonl and Vetter et al.3 reported
that particles in the injection fluid can k transported to great
distance horn the wellhre and will de~sit at a radial distance
where the p~ssure gradient is low, subsequently the rate of
permeability impairment will be negligible.
Several empirical models are used to determine the quality of
injecdon water which will minimize injeetivity impairment.
Among thew is the 1/3 - 1/7 tie. These rides relate particle size
in the injecdon water to the average pore size of the formation.
Average Pre throat diameter can be measured using the mercury
capillary method. It can be roughly estimated (in micron) by
taking the square rmt of the formation permeability in (red).
Once the avemge pore throat is know the maximum particle
size in the injection water should be less than 1/3 of the average
pore throat diameter of the formation.
In mnclusio~ care must be taken to prevent formation damage
due to invasion of foreign solids and oil. The quali~ of water in
terms of its -nded solids and oil shotid be ma and
related to the pore size of the formation. These measurements are
important parameters which can & used to aid in the design of
proper filtration system that will prevent formation damagez7.
Experimental Studies
A thorough experimental program was conducted to
determine the damaging mechanism and quality of injection
water which will minimize formation damage. The
experimental program include: characterization of bailer
samples, the plant waste water and conducting coreflood
experiments.
Two bailer samples were collected from Well “ A“. Solids
present in these samples were separated and analyzed using
Thermal Gravimetric Analysis (TGA), X-Ray Diffraction
(XRD), X-Ray Fluorescence (xRF) and Scanning Electron
SPE 39&7 QUALITY REQUIREMENTS AND RESTORING THE INFECTIVITY OF WASTE WATER DISPOSAL WELLS
Microscope (SE~ techniques. Also, volubility tests were
conducted on the separated solids.. All volubility tests were
conducted at reservoir temperature (180 “F).
To determine current water quality and conduct coreflood
experiments, several field samples were collected from the
plant and the two wells. Because the waste water contain
suspended solids and oil, it was necessary to collect samples
from horizontal, vertical and bottom orientations. Several lab
arudyses were conducted on the colleeted samples including:
particle size distribution, total suspended solids (TSS), total
dissolved solids (TDS), sulfate, sulfide, pH, Cl, Na, Si, Q
Mg, K, Al, C03, total iron and HC03.
Coreflood experiments
Coreflood experiments were conducted to determine the
infectivity of the plant waste water. The restits from these
tests were used to determine the damaging mechanisms. and
evaluate various methods to remove the damage and restore
well injectivi~. Several core plugs with an air permeability
ranging from 20 to 7,000 md were used. The core plugs were
obtained from ofiset wells and were leached with toluene
using the Dean and Stark method.
Water samples were collected from the common line going
to Wells A and B. A portion of this water was first filtered
using a 0.45 ~m filter, then through a 0.2 pm filter. This step
was conducted to remove most of the suspended materials
(solids and oil) from the plant waste water. The filtered water
was used to determine the base permeability of undamaged
cores.
Coretlood experiments were performed in a linear mode at
resemoir temperam and pressure. Fig. 2 shows a schematic
diagram of the mreflood set-up which mnsisted of transfer
vessels for the injected fluids, a syringe pump, a constant
temperature ove~ a core-holder, a chart mrder and an
automatic fiction eolleetor. The procedure used to conduct
coreflti experiments was as foliows:
1. The core plug was placed in the core-holder, and an
overburden pressure of 3000 psi was applied to the plug via a
special pump. The core-holder was placed in an oven at a
temperature 180 T (reservoir temperature).
2. Filtered (0.2 ~) waste water was injected into the core
plug at a constant flow rate (4 cm3/s) until the pressure drop
across the core stabilized.
3. Utilltered waste water with a known total suspended
material (TSM) was injected into the core. Because this water
contained suspended solids and oil, it was very important to
keep solids suspended otherwise, the solids would settle in the
transfer vessel and the resdts wodd be incorrect. To keep the
oil droplets and solid particles suspended in the ufiltered
water, the transfer vessel was placed in a reeker as shown in
567
3
Fig. 3. The reeker was operated continuously during the
experiment.
4. After obtaining a stable pressure drop across the core,
injection of filtered water was resumed. The core permeability
was determined using Darcy’s law for linear flow.
5. The core effluent was collected using an automatic fraction
collector and analyzed for key ions.
6. The particle size distribution of the solids present in the
waste water and core effluent was measured.
Analytical Techniques
Particle size distribution for the solids present in the waste
water was measured using MALVERN instrument which
finctions using a laser beam. Total suspended material
(TSM) was measured as dry weight of the solids retained on a
0.45 w Millipore type HA membrane. Total dissolved solids
(TDS) was measured using a conductivity method.
The sulfate ion concentration in the aqueous phase was
measured turbidimetncally following precipitation with a
barium chloride solution. The chloride ion was measured by
titration using a 0.1 N silver nitrate solution. Potassium
chromate was added as an indicator. The concentration of
hydrochloric acid was measured by acid/base titration using a
O.lN NaOH solution.
The concentrations of various cations present in the waste
water, e.g., calcium, magnesium, sodium, potassium,
aluminum total iron, silicon and barium were measured by
Inductively Coupled Plasma Emission Spectroscopy (ICP).
Results and Discussion
Characterization of the Plant Waste Water
The first step in this study was to characterize the plant waste
water. Samples of the waste water were collected just before
the wellhead. Total suspended solids, oil, hydrogen su~de,
total iron and pH were monitored over a long period of time.
The analysis of these samples indicated that the composition
of the plant waste water varied with time. The plant waste
water was acidic, where the pH values averaged 4.5. The total
suspended solids (TSS) ranged from 3 to 250 mg/L. Although
the average TSS value was 37 mm, there were several TSS
spikes which exceeded 100 mg/L. These high TSS values
were of major concern kause high concentrations of
suspended solids could cause severe formation damage,
especially in low permeability zones13.
The same type of variation was also noted for the oil
content in the waste water. Oil content was relatively low
most of the time. However, there were several readings of 140
mg/L. Similar to suspended solids, oil can cause formation
damage by blocking some of the pores, forming filter cake
with the solids and by reducing rock permeability to water
4 H.A. NASR-EL-DIN AND A.A. AL-TAQ
(relative permeability effwts), Total iron concentration was
relatively high most of the time and had an average value of
2.8 mg/L. The source of iron in the waste water was the
corrosion products.
Hydrogen su~lde concentration in the collected samples
ranged between 21 to 107 ppm. High levels of hydrogen
stilde in the waste water were of a concern. Hydrogen stilde
reacts with iron and produces iron sulfide which will
precipitate at pH values grat than 2. This means that iron
tide will precipitate before it reaches the target zone in the
NO wells. The presence of iron su~lde in the waste water can
plug tight zones and causes loss of infectivity. Therefore, it is
strongly recommended to monitor the concentration of
hydrogen suMde in the waste water before injection into
disposal wells.
Measuring Pore Throat Distribution
Well “A”was not cored. Therefore, core plugs from an offset
well were used to determine ~re throat distribution. Pore
throat distribution was determined using mercury injection
method. Fig. 4 shows the incremental saturation as a function
of pore throat radius. The distribution indicated that the
matimum pore size is nearly 20 microns and the mean pore
size is 2.8 microns. These resdts indicated that this
formation is susceptible to formation damage if the injection
water contains coarse particles.
Factors Affecting Permeability Impairment
Several coreflood experiments were conducted to
determine the effect of waste water on core
permeability. Fig. 5 shows the variation of permeability
ratio as a function of the cumulative core effluent.
Permeability ratio is defined as the brine permeability at
any time divided by the initial core brine permeability.
The core had an initial brine permeability of 251 md.
The permeability ratio was unity during the injection of
filtered waste water. The waste water had high salinity
and did not cause formation damage due to fines
migration or clay swelling. A significant drop in the
permeability ratio was observed when the waste water
was injected to the core. The waste water contained
TSM (oil and solids) of 89 mg/1. The permeability ratio
increased to almost its initial value when the flow
direction was reversed. These results indicated that the
waste water damaged the core and the damaging
mechanism was the formation of an external filter cake.
Fig. 6 depicts the variation of the permeability ratio
with the core effluent for a core plug with an initial
permeability of 77 md. Similar to the results shown in
Fig. 5, the waste water caused severe damage to the
core. The rate of decline in the permeability ratio was
faster than that noted in Fig 5. This was mainly due to
the lower initial permeability of this core.
Fig. 7 depicts the permeability ratio as a function of
core effluent for a core with an initial permeability of 65
568
SPE 394S7
md. Injection of waste water with TSM of 15 caused
gradual drop in the relative permeability. The decrease
in core permeability was less than that observed in Figs
5 and 6. Waste water with TSM of 15 mg/1 still
damaged the reservoir cores.
The most important aspects of the results shown in
Figs. 5 to 7 were: waste water was damaging to the
cores and the damage increased at higher
concentrations of suspended material, especially in low
permeability cores. Also, the mechanism of forma~on
damage observed in all coreflood experiments was the
formation of an external filter cake.
To identify the damaging material, the waste water
was filtered using a 0.45 micron filter. The solids were
analyzed using XRD method. The results indicated that
mackinawite (FeS) was the main mineral present in the
collected solids. The presence of iron sulfide was not
surprising because the waste water contained hydrogen
sulfide. It is clear from these results that the
concentration of hydrogen sulfide should be measured
in waste water. Hydrogen sulfide should be treated as a
damaging material, i.e., solids and oil, and its
concentration in the plant waste water should be
reduced.
To determine water quality requirements, several
coreflood experiments were conducted. Particle size
distribution was measured for the injected waste water
and the core effluent. Fig. 8 shows that the mean
particle size in the injected water was nearly 40 microns.
The mean particle size of the solids in the core effluent
was nearly 4 microns. These results indicated that all
particles with diameters greater than 4 microns were
retained in the core and obviously caused loss of the
core permeability.
To restore the permeability of the damaged cores, 15
wt% HCI was used. Fig. 9 shows the concentration of
HCI in the core effluent. The acid concentration
increased to 15 wtVO during the first acid injection. The
objective of the first acid injection was to remove
formation damage due to the injection of plant waste
water and leach iron from mineral containing iron, e.g.,
chlorite. Unfiltered waste water was injected into the
core. Similar to previous results, the core was damaged.
A second acid injection was performed to confirm the
nature of damaging material. The concentration of the
acid in the core effluent reached 13 wtYo. Acid
concentration reached zero during the injection of
filtered plant waste water.
Fig. 10 shows the concentration of total iron in the
core effluent. Several spikes of high iron concentration
were noted. The first spike was noted during the
injection of waste water. The second spike occurred
during the injection of the first acid injection. The source
of this iron was the damaging material and iron
containing minerals present in the core. The third spike
was lower than the second one, but the concentration of
 SPE 394S7 QUALITY REQUIREMENTS AND RESTORING THE INFECTIVITY OF WASTE WATER DISPOSAL WELLS
iron was still high. The main source of iron in the third
spike was the damaging material. The results shown in
Fig. 10 confirmed that the damaging material contained
iron and the core permeability could be restored using
15 wt% HCI.
Field Application
Based on extensive lab studies, Well “N’ was aeidized. The
treatment consisted of two stages designed to remove
organidinorganic material which might plug the petiorations and
titimately restore the well infectivity.
To remove the organic material and provide good contact
beween the inorganic de and acit the ~ stage started with
the injdon of 107.5 bbls (10.75 galdft of perforations) of 90
wt~. xylene and 10 wt~. mutual solvent using a 1..5”coiled
tubing (~. The mi.~e was left to soak for 30 minutes, then
the well was flowed back to a nearby pit for nearly 14 hours. The
color of the colleeted samples was black to brownish with xylene
smell. Some of these samples bd a H2S smell, contained
-nded solids and oil.
The second stage of the treatment included injection of 400
bbls (40 gals/ft) of 15 wt% HC1 acid. The objective of this
stage was to remove the remaining inorganic scale, such as
iron su~lde and iron oxides. The well was flowed back to the
pit and 22 samples from the acid return were collected. The
color of the initial samples was black. The samples collected
during acid returns had a greenish color and a strong HZS
smell. These obsemations indicated the presence of iron
su~de.
A posttlush of 600 bbls of 1 wtYo ammonium chloride
followed the acid treatment. An infectivity test was conducted
using the ammonium chloride solution and showed a
significant improvement in the well infectivity. The injection
rate increased from 3,000 bbls/day at 2200 psig to 15,000 bbls
1,700 psig.
To assess the treatment, a geochemical analysis was
conducted on the aqueous phase of the collected samples. Fig.
11 depicts the hydrochloric acid concentration in the collected
samples as a function of time. The acid concentration
increased and reached a maximum value of 11 wtOA.Then, it
gradually decreased and became constant at 2 wt% at the end
of the nitrogen lifi. It is important to note that the injected
acid had a concentration of 15 WtO/O whereas the maximum
concentration reached in the backflow was 11 wtYo. This
difference in acid concentration was due to dilution of the
injected acid with the formation water and acid reactions with
the formation minerals, casing and corrosion products. It is
also important to note that acid concentration at the end of
the nitrogen lift was 2 wtYo, This value was too high and
raised great concern because this acid could cause corrosion
of the well casing, Also, it would precipitate iron compounds
once the acid was consumed. Iron precipitates could further
damage the well. Therefore, it is strongly recommended to
backflow the well until acid concentration in the returns is
569
5
nearly zero or the pH of the returns reaches 4.
Fig. 12 shows that the concentration of total iron before the
injected acid contacted tie target zone was nearly 20 ppm.
Once acid contacted the target zone, the concentration of total
iron increased to 2,500 ppm. Iron concentration then
gradually decreased and remained constant at 200 ppm in the
samples collected during the last three hours. The results
shown in Fig. 12 indicated that the acid dissolved significant
amounts of iron. The most likely sources of iron were the iron
sulfide present in the injection water, formation minerals
(e.g., chlorite, pyrite and ankerite) and well casing.
Conclusions
1. The plant waste water was corrosive and contained high
concentration of hydrogen su~lde which reacted with iron
resulting in iron s~]de precipitation, tier damaging the
formation.
2. This water contained coarse particles which caused
formation damage by forming an external filter cake.
3. The plant waste water caused severe damage to reservoir
core plugs.
4. Corefloed tests as well as field results indicated that the
damaging material contained significant amounts of iron
compounds.
5. To restore the infectivity of damaged wells, the following
acid formula was reeomxnended: 15 WtO/O HC1, 10 VOlO/O
mutual solvent, 0.2 WtO/O corrosion inhibitor, 0.4 WtO/O iron
control agent, and 0.4 WtO/O HzS scavenger. Acid volume
should be 100 gals/ft. Ball sealers should be used for better
acid diversion. The recommended acid formula was very
effective in improving the infectivity of Well “A”.
6. To prevent any further damage to the disposal wells, the
quality of tie waste water should be improved as follows:
TSM should not exceed 50 ppm, mean particle size should
not exceed 4 microns, hydrogen tifide concentration should
not exceed 10 ppm, toti iron concentration should not exceed
2 ppm and pH value should be beween 6 to 7.
Finally, it is dso recommended to continuously inject the
plant waste water into the two disposal wells. Shutting
disposal wells for any period of time will allow all particulate
materiat to settIe, which wilI cause formation damage and
loss of well infectivity.
Acknowledgments
The authors wodd like to thank the Ministry of Petroleum
and Mineral Resources for petission to publish this work.
A. Bin Hassrm and T. A1-Shafie assisted with the
experiential work. The Chemistry and the Advanti
6 H.A, NASR-EL-DIN AND A.A, AL-TAQ SPE 39467

Instnunents Units of the Lab R&D Center m apptiated
for performing chemid and mineralogid analyses of the
acid returns.
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7. Pautz, J.F., Crocker, M.E. and Walton, C.G., ‘Relating

Water Quality and Formation Permeability Damage to
Loss of Infectivity’~ SPE 18888 presented at the SPE
Production Operations Symposium, Oklahoma City, OK,
March 13-14, 1989.

8. Zhang, N. S,, Somerville, J.M. and Todd, A.C., “An

Experimental Investigation of the Formation Damage
Caused by Produced Oily Water Injection” SPE 26702
presented at the Offshore European Conference held in
Aberdeen, UK, Sept. 7-10, 1993.

9. Khatib, Z.I., ‘Prediction of Formation Damage Due to

Suspended Solids: Modeling Approach of Filter Cake
Buildup in Injectors” SPE 28488 presented at the SPE
69th Annual Technical Conference and Exhibition, held
in New Orleans, LA, Sept. 25-26, 1994.

570
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