SPE

SPE 23817

A New Technique for the Evaluation of Acid Additive Packages

LR, Houchin, W,E, Foxenburg, M.J, Usie, and Jun Zhao, OSCA Inc,

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designed utilizing this laboratory procedure showed

The expanded use of sandstone matrix acidizing
techniques may have been the mmt significant trend of
the turbulent 1980s. (3ulf Coast operators have found
that remedial acid treatments cost a fraction of that
required for a comparable offshore completion.
Improved design and application techniques now
provide econwnic success rates greater than 80% with
most treatments paying out in less than 30 days,
However, one area that continues to frustrate designers
of acid treatments is the unpredictability of crude oil
reservoirs, Current testing procedures are inadequate,
failing to accurately replicat~ the interaction between
the treating fluid and acid sensitive crudes. Reliance on
these procedures can produce catastrophic facility
upsets, downhole emulsion blocks, reduced damage
removai efficiencyor result in a marginal treatment
re~ponse,
A new simplified laboratory testing procedure was
developed which more accurately simulates treatment
effects under reservoir conditions. This laboratory test
demonstrates the need for less reliance on surfactant
non+mulsifiers and an expanded use of mutual
solvents. Field data confirms more accurate prediction
of acid compatibility. In addition, acid treatments
Refarenoaa and Illuatrationa at em! of papar.
greater Mid production response and maintained the
incremental increase for a much longer time. Design
guidelines are presented which address concerns of
mutual solventkorrmion inhibitor incompatibility
y, high
temperature applications and treating volume
requirements,
XMWMWQN
Remedial sandstone matrix acidization of crude oii
reservoirs has become the primary tool of experienced
engineers to maximize profits at minimal cost. (3idlcy1
found that the stimulation response from acid
treatments of gas or water injection wells was
somewhat predictable. However, the high degree of
variability of crudes made the acidization of crude oil
reservoirs unpredictable, requiring extensive
pre-stimulation laboratory testing and evaluation of the
unique, site specific nature of individual oil wells. This
study focused on developing laboratory test procedures
and design criteria to more accurately predict acid
treatment responsein crude oil reservoirs,
The problems assodated with acid induced emulsion
formation upon stimulation of oil wells was addressed
by Mobil Oil in the mid 19S0s2. Suboptimized results
with operational complications such as emulsion blocks
and facility upWs were occurring far too often, Mobil
 . . .. . ----- . u.
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required its engineering staff to take samples of the
treating fluids being delivered to location and mix them
with a fresh crude sample from the well. If a 90%acid
breakout was not achieved in 10 minutes, the truck was
sent back to the yard, The service companies got the
message. The Mobil test became the first standard for
pre-stimulation testing. Most of the acid additives used
to pass this test were cationic surfactant
non-emulsifiers, This class of surfactants were found to
oil wet sandstone reservoirs,3 Anionic surfactants,
thougn compatible with the nettability characteristics
of sandstone reservoirs, were usually incompatible with
the cationic acid corrosion inhibitors. To avoid blending
difficulties and operational failures associated with
surfactant/formation incompatibility, there was a shift
toward the use of nonionic surfactants for emulsion
prevention. As a general rule, these ponionic
surfactants were a little slower acting, often requiring
more than the 10 minutes breakout required by the
current test,
In the late 1970s,API Bulletin, RP+24 attempted to
standardize pre-stimulation testing procedures. This
procedure recommended only the hydrochloric
hydrofluoric (HC1:HP)mud acid be tested for sandatone
reservoirs. This updated version of the Mobd Oil
Company test did not sat specific standards for acid
break out times, Nor was the I-ICIpreflush evaluated
for its emulsion potential. As a result, this procedure
never received widespread industry acceptance.
The industry test requirements have evolved to testing
all acid stages with a 5050 mix of live acid (plus
additives) to crude, requiring a 90% acid breakout in 15
minutes at approximately 150F (66C), or bottom hole
temperature, The major deficiency of this current
practice is that it assumes the live acid with all of its
associated additives represents the fluid that intermixes
with crude in the formation, This study has found that
these critical additives, through chemical masa transfer
effects, are initially adsorbed onto the formation
matrix, leaving the acid front untreated, Furthermore,
critical crude sensitivity to acid containing dissolved
iron and other acid reaction products must be evaluated
to ensure acid/crude compatibility,s
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WE 23817
A new test procedure for pre-stimulation evaluation o!
acid compatibilityy is provided. Labor&tory and field
data indicates this simple laboratory test procedure has
been effective in preventing those operational problems
such as rmulsion blocks and catastrophic facility upsets.
In addition, the resultant acid treatment not only
produced at a higher initial rate, but maintained the
incremental increase for a much longer time, While
the acid additives were selected in order to pass this new
test procedure, it became obvious during the course of
this study that numerous unanticipated benefits had
been derived. This paper includes these design factors
and field evaluation data utilized by the authors which
produced better, longer lasting results.
~
Several authors have reported severe surface emulsions
when acid returns are flowed back to central
facilitiesF7 Dunlap et.d. suggested that both facility
upsets and downhole emulsions occur as a consequence
of inadequate pre-pb compatibility y testing.7 Other
authors have demonstrated that surfactant
non+mulaifiers, used to prevent theea emulsification
tendencies, may preferentially adsorb onto mineral
surfaces.gg TM adsorption results in the aurfactant$
being unavailable in the acid fluid front where
formation damaging emulsions can form. The challenge
was to develop a test procedure that more accurately
replicated reservoir conditions.
The first step was to determine the Affect of nonionic
surfactant adsorption. Hallg had evaluated the
adsorption effect of anionic and cationic surfactants in
an acid solution after being flowed through a sand
pack. However, he did not look at the nonionic
surfactants that are currently in use. A 6 foot long
(1.83 m) by 2 inch diameter (50,8 mm) core test
apparatus was constructed according to specifications
established by King,10 This apparatus contained Berea
cores assembled in series, wrapped with a triple
thickness fiberglass mat and sealed with resin, Pluid
taps were lomted every 6 inches (lS2,4 mm) for
sampling purposes, Three widely used nonionic
surfactant non+mulsifiors were addad to a M% HCl
acid solution and flowed through the test apparatus,
Fluid samples were taken from each sample port and
mixed with ail acid aansitiv~crude, The acid front was
. .
PE23817 L.R. KKZilN, W.E. -
calculated at rate versus time, A 100 cc sample was
collected from each sample port as the aad front
passed. The sample was split and duplicate emulsion
trots were run, The results were averaged and are
reported in Tables 1 and 2. l%~re was no variation
greater than standard *5% experiment error. Ail
nonionic non-emulsifiers failed to eficctively function
after only 6 inches (152.4mm) of acid penetration into
the core (See Table 1). Acid solutions containing 10%
ethylene glycol rnonobutyl ether (EGMBE) in addhion
to the surfactant showed slightly better non-emulsion
performance even at 24 inches (609.6 mm) of
penetration. Tables 1 and 2 show only that data in
which the additive system provided functional
non-emulsion proprties, therefore, no data is reported
beyond a penetration of 24 inches(6(9.6 mm).
Obviously, a 6 foot (1.83 m) core test apparatus is not
practical for routine testing purposes. However, the
send pack approach used by Hallg .muld be easily
adapted to simulate these adsorption effects on aad
compatibility. A sand pack composition and step-wise
procedure was developed as shown in Appendix A. An
attempt was made to duplicate the effects observed in
the long core apparatus. Figure
1 shows a comparison
of the acid breakout of a typical Gulf Coast crude using
both the current testing procedure and the new sand
pack test. The current procedure showed a X3(YXacid
breakout in 1S minutes, but only a trace when the acid
solution was flowed through the sand pack,
The first step in validating the new Sand Pack Method
(SPM) was to add it to our existi!g test regimen. Test
results indicate that, as observed in the long core test,
the surfactant non-emulsification function was almost
always lost due to adsorption, When surfactant loading
was increased to compensate for adsorption in the SPM
test, an over-treat condition was created in the standard
live acid test+ The only acid treatment that consistently
passed both tests was the addition of mutual solvents or
alcohols with low levels of surfactants.
Figures 2 and 3 demonstrate the difference htween the
likely effect of an acid/surfactant front and one
containing acid/surfactant/mutual solvent, Figure 2
shows the advance of an untreated acid front (HC1
preflush) due to adsorption of the surfactant.
Eventhough some desorption will occur with later
467
tG, M.J. WIE, & J. ZWW .:
stagm the untreated front has displaced much of the
oil that was located in the near wellbore region. If
instantaneous emulsific~tion does not occur, it becomes
progressively less likely that there will be sufficient
energy applied to cause emulsification as the front
penetrates due to a reducing velocity with the radial
expansion. Therefore, a greater emphasis was placed on
the additive package in the acid preflush, particularly
since the field being considered in the field trial had a
history of facility upsets and difficulty unloading after
acid stimulation.
The most common acid system utilized in the Gulf
Coast is shown in Table 3.11U This system evolved
because of three primary features which include: low
acid strengthkoncentration. lower volumes ~d a
brine/mutual solvent post flush. The logic behind this
system is that while it may be sub-optimised, it is less
likely to induce damage from incompatible mineral acid
reactions, weakening of the matrix binder by over
The
stimvletion or cause excesive corrosion.
brine/mutual solvent postflush would not interfere with
the add corroeion inhibitor and would remove excess
inhibitor from the formation face, thereby, l-fig the
formation water wet.
The initial field trial involved 11 acid jobs from one
single structure in the offshore eastern Gulf of Mexico.
The first two treatments used the current standard acid
design and resulted in platform shut down due to
facility upsets during the acid flow back. Tables 4 and
5 show the alternative acid systems that were
subsequently applied. System A (Table 4) had EGMBE
added to the acid preflush and the brine postflush. Our
concern was the untreated acid front causing an
emulsion and the benefits of EGMBE in the postflush
were still valid. System B (Table 5) provided EGMBE
in all aqueous stages. This system was first attempted
because the SPM test indicated inadequate acid
breakout in the mud acid (HCLHF) test. Acid volumes
were reduced to accommodate pre-approved AFE limits
on both treatment designs. There was no technical basis
for this decisionwhen it was originr.ily made.
The performance of all three acid designs for the 11
wells in the field trial are shown in Table 6. All of the
wells are geologically similar with near identical
.-.
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reservoir properties inck~dinginterval length. Build up
data was not available, therefore, 6 month cumulative
production was provided.
Both systems A and B were flowed back to the central
facility without causing an upset. They also provided a
20% improvement over the production increase
ex~rienced with the initial two treatments, System A
produced almost double the cumulative production,
when compared toresults obtained through the current
standard acid design, while the production from System
B virtually tripled.
The value of Acid Flow Back anal sis has teen
previously documented in the literature. 1L4 Acid Flow
Back analyses were conducted on each treatment. An
average of 10 samples were collected during the acid
return. Sample collection was initiated when pH began
to drop and was continued until a consistent pH of #
was reached. Microscopicanalysis of the crude ahowed
a prewnce of rigid film ermdsion on the wells where
the current standard acid design was used (Table 7).
The results of ICP (Inductively Coupled Plasma
Emission Spectroscopy) ion analysis on acid returns are
presented in Table 7. Although the focus of this paper
does not include an indepth analysis of Acid Flow Back
results, a general overvi~w may help explain some field
results, For example, the siliconaluminum (SiAl)
raties are almost identical on the three treatments, but
the total ion concentrations of Si and Al increased in
proportion to the increased usage of EGMBE. Tine
higher the total ion concentration of Si plus Al, the
higher the cumulative production increase, More
importantly, all five wells treated with System B
maintained at least some incremental increase for 6
months. No well treated with either of the other two
systems maintained their incremental increase for this
length of time,
A search of the literature provides an interesting
confirmation as to the outcome of this field trial, Just
as in this field trial, Clidley15 had shown that the
successrate of acid treatments more than doubled when
E(IMBE was added to the treatment solution, His study
used a larger sample of wells treated, and yet, the
results of average production increases were more
dramatic. He found that adding EGMBE to the HC1
acid prefhsh more than doubled his average production
increase. This was exactly the same results as reported
in this study. The most important finding was that this
study showed a three fold production increase end
C3idleyexperienced five fold increases when E(3MBE
was added to the HCIMF mud acid. He concluded that
one of the most common mistakes made in the
application of acid treatments was no mutual solvent in
the mud acid treatment.
There. are several plausible explanations for why
E(3MBE or other similar mutual solvents are so
effective when added to the mud acid stage. One likely
explanation is that the most common inorganic
component of formation damage is comprised of clays
and silts that have become oil wet or are part of a
. 16,17,18 ~ d~ge
complex organic/inorganic depomt.
can only be removed by a mud acid solution with
sufficient solvent volubility to simultanwusiy remove
oil barriers while dissolving clays and silts.16 we
this may explain the higher production increase, it is
difficult to explain the longevity of the treatment
response. Perhaps, by more completely removing tlww
complex deposits, it takea more time for the damage to
re-ur.
The authors considered two other pxwible explanations.
Short term production responws appear to be associated
with post-stimulation fines migration, The source of
these fines can be acid reaction products such es
colloidal silica, or fines liberated by excessive acid
volumes weakening the matrix binder.
This field study showed higher recovery of potential
acid reaction products (Table 7) when EOMBE was
added to the acid solution; The E(3MBE may be
preventing the acid corrosion inhibitor from oil wetting
particles such as hydrated silica and causing them to
flocculate, The tendency of EGMBE to water wet
particles and keep them dispersed, should allow them to
flow out of the reservoir instead of plugging it, The
efficiency of E(JMBE and other associated mutual
mlvents to strip oil wet films from surfaces raises some
interesting corrosion inhibitor performance questiona
which are addressed in the next section,
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Another factor likely to produce short term results is
the release of fines due to excessive acid volumes
weakening the matrix binder. It has long been
established that, with sandstone matrix acidizing, once
near wellbore damage is removed, the maximum
treatment response has been reached.~9n Additional
live mud acid penetration usually starts to produce
fines and induce damage. The volumes of acid were
reduced in this field trial In order to compensate for
the added cost of the mutual solvent. These lower
volumes may have been sufficient to remove most, if
not all, of the near wellbore damage without excess live
mud acid producing fines.
Several investigators have raised questions about
mutual solvent compatibtity with acid corrosion
iIdlibitOl$.921a The authors f~l that acid corroei~
inhibitors are available that can be used with mutual
solvents up to 20@F (93C), sea Table 8, The use of
mutual solvents in acid solutions will usually require a
higher loading of corrosion inhibitor. Flocculated solids
found in the presence of high corrosion inhibitor
concentration and EC3MBE have been reported.~
However, these reports have involved a limited group
of inhibitors at very high loadings of 2%, A good
practice is to require corrosion test data with the
specific inhibitor and mutual solvent selected for the
acid tretitment. In addition, inhibitor loss due to
filtration should be evaluated if acid solutions
containing corrosion inhibitors are to be filtered,n
If a well with a bottom hole temperature above 200F
(93C) must bS acid stimulated to bS ~mnomi~l,
consider some of the following design options:
1) Run a compatible brine (3% NH4C!1)preflush
containing mutual solvent instead of adding the
mutual solvent to the HC1preflush.
2) Substitute organic acids for mineral acids such as
10%acetic acid for 7S% HC1 or 102% acetic:HF
for 7.5:1.5%HC1:HF. Organic acids are much
less corrosive than mineral acids,
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3) Minimii acid contact with tubulars.
a. The mud acid stage spends so quickly at these
temperatures that it can only remove very
near wellbore damage. Reduce volumes by
75% and test results, Then, additioml
stages can be run if needed.
b. Increase pump rates. This not only
minimizes contact time, but will enhance
diverters that perform marginally at higher
temperatures.
4) Reduce concentration of mutual solvent.
Emulsions are leas stable at high temperatures
and require less chemicals to prevent, The use
of organic acids and improved iron control can
help prevent rigid film emulsions at elevated
temperatures. One of the most important
fulictiona of mutual solvent is to prevent the oil
wetting effect of acid corrosion inhibitors. If the
mutual solvent concentration ia reduced, it is a
good practi~ to incorporate design tachrdques
that also Iowers the inhibitor loading.
These guidelines should help when high temperature
reservoirs are encountered. The best hurance when
designing acid treatments is to assure they are
completely tested. Testing procedures should accurately
simulate reservoir conditions. Standardized test
procedures should not be used as the sole criteria for
acid/crude compatibility. Flexibility in test procedures
are required to simulate the wide range of variables
encountered in sandstone matrix acid treating of crude
oil reservoirs,
~) The current industry accepted acid compatibility
testing prcxedures were found to inadequately
simulate the downhole performance of acid
additive packages.
~,
A new test procedure has been provided that
more accurately replicates the actual treatment
performance in the field, Acid treatments
developed by utilizkg this procedure have been
effective in preventing facility upsets, and more
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importantly, the treated wells have produced at

higher initial rates and maintained these rates
for a much longer time period. The authors would like to thank the management of
OSCA, INC. and GREAT LAKES CHEMICAL
3) Laboratory tests and field results indicate that CORPORATIONfor permission to publish this paper.
the current practice of relying exclusively on
surfactant/non-emulsifiers to achieve acid
y usually provides unpredictable
compatibility
results which have typically produced 1) Gidley, J.L.: Acidizingsandstone Formation* A
suboptimized treatments and/or emulsion related Detailed Examination of Recent Experience,
upsets. pqx!r SPE 14164presented at the 19S5SPE Ann,
Tech,Conf,, Les Vegas,Nevada, Sept. 22-2S.
4) An expanded use of mutual solvents was
required to meet acid compatibly objectives.
2) Producl Data Bulletin Manuak Aquaness
The addition of mutual solvent to the aqueous
Chemical Company; Houston, TX, 19S9.
preflush and the HCkHF mud acid stage is more

I
important than the current practice of adding it
3) McLeod, H.O.: Stimulation;SPE Short Course
only tc the brine poatflush, Extending the
production increase beyond 6 months only
4) API Recommended Practices For Laboratory
occurred from treatments in which mutual
Testing of Surface Active Agents for Well
solvents were added to the HCkHF mud acid
Stimulation, API RP-42, Second Edition,
stage, Guidelines are provided to address
January, 1977.
concerns of mutual solventkorrosion inhibitor
incompatibility.
I 5) Houchin, L.R., Dunlap, D.D., and Domike, K.M.:
The Occurence and Control of Acid - Induced
s) The organic component of formation damage and
Asphaltene Sludge paper 19410presented at the
acid compatibility may be the most critical
1990 SPE Formation Damage Controi
factors affecting treatment optimization. This
Symposium,Lafayette, LA Feb. 22-23.
:Itudy shows that preventing acid induced
emulsions and sludges, ensuring adequate solvent
6) Coppel, C,P.: Factors Causing Emulsions Upeets
volubility of aqueous acid systems, and
in Surface Facilities Following Acid
incorporating maximum nettability features are
Stimulation, J. Pet. Tech.(Sept. 1975)1060-6S.
paramount to successful matrix acidization of
crude oil reservoirs, These featurez will allow 7) Dunlap, D.D, and Houchin, L,R.: Evaluation of
for the removal of oil coated complex Acid System Design and Formation Damage
organic/inorganic deposits, the dispersibility and Using Polarized Microscopy paper 1942S
recoverability of acid reaction products and presented at the 1990, SPE Formation Damage
minimization of acid induced damage, Control Symposium, Lafayette, LA Feb. 22-23,

6) Optimizing the acid additive package while
lowering the total volume of treating fluids
resulted in both a lower initial cost and the
highest level of incremental increase in oil
production,
8) Sutton, G,D, and I-mater, R.M,: *Aspectsof Acid
Additive Selection in Sandstone Acidizing,paper
SPE 4114 presented at the SPE-AIME 47th
Annual Fall Meeting, San Antonio, TX Oct. 8-11,
1972.

9) Hall, B.E.: The Role of Mutual Solvents in

Sandstone Acidizing, J, Pet. Tech. (Dec. 197S),
1439-42,
* .

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93917
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- -. ---- 7

10) King, G.E., and Lee, R.M,: Adsorption and
Chlorination of Mutual Solvents Used in
Acidizingpaper SPE 14432presented at the 198S
SPE Annual Technical Conference, Las Vegas,
Nevada, Sept. 22-25.
11) McLeod, H,O.: Matrix Acidizing,J, Pet, Tech,
(December1984),2055-69.
12) Brannon, D.H., Netters, C.K. and Grimmer, P.J.:
Matrix Acidizing Design and Quality Control
Techniques Prove Successful in Main Pass Area
Sandstone,JPT (Aug.1987),931-942.
13) Almond, S.W,, Brady, J,L., and Underdown,
D,R.: Prudhoe Bay Field Study - Return Fluid
Analysis,JPT (April 1990),46&472.
14) Fambrough, J.D., Brady, J.L., and Almond,
S.w.; Return Fluid Analysis From the
Sadlerochit Formdion, Prudhoe Bay, Alaskw A
Laboratory Study - Part II, SPE 22079
20) Paccaloni, G.: Field History VerWles Control,
Evaluation O(JJ, Nov. 26,1979,61-6S,
21) Woodroof, R.A, Jr,, Baker, J,R,, and Jenkins,
R.A, Jr.: Corrosion Inhibition of
Hydrochloric-Hydrofluroic Acid/Mutual Solvent
Mixtures at Elevated Temperatures, SPE 5645
presented at the 197S SPE Annual Tech. Conf.
and Exhibition, Dallas, Sept. 28- Oct. 1.
22) Davies, D.R., Lievaart, L, and Nitters, G,: The
Effects of Corrosion Inhibitors end Mutual
Solvents on Matrix Acidizing Treatments, SPE
171S3 presented at the 8th SPE Symp. cm
Formation Damage Control, 1988, Bakersfield,
CA.
23) Houchin, L,R., Dunlap, D.D., and Hudson, L.M.:
Field Mixing and Filtration of Acid Stimulation
Fluids, OTC 5244, presented at the 18th Annual
OTC Conf. in Houston, TX, May S-8,1986.

15) Gidley, J.L.: Stimulation of Sandstone

CRUDE OIL - ACIDCOMPATIBILITY
Formations with the Acidizing Mutual Solvent
Method, JPT (May 1971),SS1-558.

Overview
16) Houchin, L,R., and Hudson, L.M.: The
Prediction, Evaluation and Treatment of
Compatibility of the crude oil with the acid system is
Formation Damage Caused by Organic
determined by first running standard non-emulsion
Deposition, SPE 14818, Proc, ?th Formation
tests on the live acid (with and without additives) and
DamageControl Symp., Lafayette, (1986)83-90.
then filtering the optimized acid package tnrough a
sand/clay pack filter bed, The initial non-emulsion tests
17) Efthim, F,P., et,al,, Evaluation and Treatment
are designed to determine the optimum live acid
of Organic and Inorganic Damage in an
package as well as the crudes sensitivity to variables
Unconsolidated Aaphaltic Crude Reservoir SPE
such as acid strength, a?id type, and presence of soluble
19412presented at the SPE Formation Damage
ferric (+3) iron. The iron is added to the acid (2000
Symp. in Lafayette, Feb. 22-23,1990.
mg/1) to check for sludge sensitivity y or rigid film
emulsion formation, This iron sensitivity testing is
18) Bilden, D.M., et.al., Evaluation and Treatment
especially relevant for asphaltic crudes rmd many times
of Organic and Inorganic Deposition in the
results of compatibility testing may dictate a preflush
Midway Sunset Field, Kern County, CA, SPE
treatment prior to the introduction of the acid,
20073presented at the 60th CA Regional Meeting
held in Ventura, CA, April 4+, 1990.
Once the live acid system is formulated and optimised,
it is fiitered through a sand/clay peck and the
19) Paccaloni, (3: New Method Proves Value of
non-emulsion tests (compatibility) are re-run, III this
Stimulation Planning OGJ, Nov. 19, 1979,
way, the aurfactant adsorption ia simulated and the
155-160,

I ANWTEUINIUEFUR=51AUWI~
downhole compatibility assured. If the previosly
obtained W% breakout and associated good wettability
characteristics are not maintained, mutual solvent(s) are
added to the system (and/or additional surfactant) until
post-filtration compatibility is achieved. The mud acid
stage is filtered through the same pack as the HCL
*Standard non-emulsion testing involves mixing 5050
ratios of acid system:crude oil under low shear, placing
mixture in 100 cc graduated cylinders and into a water
bath at bottom hole temperature,or 150F, whichever is
lower, The percent acid breakout is monitored every 5
minutes and observations made of the wettability
characteristics.
A compatible mix is defined as having greater than 90%
breakout within 15 minutes and displacing good
wettatility characteristics.
Outline
Step 1: Determine acid type and strength to be
tested based on mineralogy, suspected
formation damage, field operations, etc.
Step 2 Determine compatibility of crude with
chosen live acid prior to addition of
additives,
Step 3 Determine compatibility of crude with live
acid plus corrosion inhibitor,
S!cp 4: Determine compatibility of crude with live
acid plus corrosion inhibitor and additives
(non-emulsifiers, afiii-sludge surfactsmts,
iron control agents, etc.)
Optimize additive package to provide
290% acid breakout within 15
minutes,
Step 5: Filter optimum live acid package (acid +
additives) through sand/clay pack and
determine compatibility with crude oil,
9
WMID-ITIVEP~ SPE 23817
Step 6: Add mutual solvent to acid package, if
necessary, and filter through sandklay
pack, Determine compatibility with crude
oil.
Optimize treatment to provide 290%
acid breakout within 15minutes
SA.NINCLAYPACK FILTRATIONPROCEDUREFOR
G
Equipment/Apparatus/Rea2ents
* 1-9 cm ID Plastic Buchner Filter Funnel
* 1-9 cm OK)Whatman No, 4 Filter Paper
* 1- Sidearm Filter Flask
* Standard Pack Materiala: 101080 Wt%
Wyoming bentonite clay:fine silica flour:ltM
mesh sand
Stock solution of 3%NH4C1
100cc graduated cylinders
Vacuum pump or aspirator set up
Waring Blender and jars
Rheostat
a - If mineralogy indicates much higher percentages of
clay, the pack formula may be adjusted accordingly.
1) Mix 100cc of C.e acid system to be tested,
2) Prepare filter pack by mixing 200 g of the
blended pack material with 250 cc of 3% NH4C1
solution to make a slurry,
3) Filter slurry in Buchner funnel using a Number
4 Whatman filter paper to form the sand pack,
Collect A220 cc of brine effluent and discard,
This volume assures the pack will not exaggerate
dilution of the acid with excessNH4C1brine,
4) Filter the acid system, Collect the first 20 co of
effluent and discard,
5) Collect the remainder of the filtered acid and
trander SO cc to the blender, Add 50 cc of oil
sample and mix on low shear for 1 minute,
~
----, . . . . . .w. , .&!. SW-, Ca, v. WUi, a u. Mtuw 1

6) Place the mixture into a hot water bath at the

wells bottom hole temperatule or 150F, ~~
whichever is lower. OF x (OF- 32)/1.8 mOc
ft x 3048 E-01 =m
7) Measure volum, % acid drop-out at 5 minute
gal x 3,78S412E-03 =m 3
intervals.

8) Evaluate at 15 minutes to determine if industry

accepted standard of 90% by volume acid
drop-out has been achieved, In addition, the
overall fluid quality should be observed (oil
quality, water quality, presence and rigidity of
interracial layer, wettability, and sludge
sensitivity).

TABLE 1
Adsorption Effect of Men-Sonic 8urfeatmt8
Flowing Through 6 root Long Coro Apparatus
Percent Acid Droakout (1S nin./150? (66C)
Non-ionic Sa:p:; +1 Sa~ l:n!2
Surfactant Initial . (! m
15t HC3 only trace
surf. #1 94 ii ii j:
surf. #2 92 75 39
Surf. #3 92 71 32 11

TABLE 2
Adsorption Effect of Non-ionic 8urfactant8/
Mutual solvent Flowing through 6 Foot Long Core Apparatus

Percent Acid Breakout (15 Iain./150F (66C)

Non-ionic Sa~~l;n~2 Sample *4 s~:~l:n!;
$UrfaCtant/t3GM3E Initial (24 in,)
Surf, #1,/5t EGt4BE 100 96 89 70
SUrf. #1/10# E6MBE 1;: 90 90
Surf. #2/5t EGMBE 94 84 :;
Surf, #2/10& ZGMBS 97 94 86 68
Surf, #3/5t EGMBE 95 91 39
Surf. #3/::%E::::E 95 92 U 50
90 90 74 36
IO* EBMBE 92 91 79 48

---
 currant Typical Oulf Commc Mid mcoatBoat

2s Solvent Proflush (xyl@no)

7.59 35C1 + Burfoetont + c: + ICA
1:: 7.5 i i.St RC1112F + Surhotmt + c1 + ICA
150 3b ?n3,cl + 10$ CGMDC+ C8

CI rn corrosion inhibitor
tCA - iron control ~ant
CS - clay otabilixcr

TABLE 4

20 solvant prof lush (Xylanc )

7,S\ Wci + Surfcctmt + CI + ICA + 10$ EQNBE
% 7,5 : 1,5* UCIIIW + Surfactont + CI + XCA
75 3* NH4C1 + 10t 8GMB8 + CS

TAXL8 S

AaLd Syutos B

Troatmont VOIUBOS
Gallon. Per toot ~rostmcnt SY tom
20 tolvont prsf lush (xylono )
7.St 33C1 + Surfactmt + CI + MA + 10t 8GIIBC
% 7.S t 1,59 13C1:13? + Surtactant + C! + ICA + 10t CBRSB
75 3* Nit,cl + lot COI!B8 + Cs

TABLR 6

?roduction Uaspwso to Varloum Aoid Systems

&-rag. Production xncrosos

WJ:~{,of Troatmwrt Initial 6 Month Total 6 Month

TYRm 310?0 Cirmullltiv, Incrsam

2 Currmt 8tmndnrd 408* M::z; (sp) 32,240 (8:s)

4 Sy,toN A 488** 119,228
5 System B 504** 45,366 W 226,830

R@adin~ takm 15 days ttor troatmnt duo to ~mrlodia shut-in ( 10 days)

from downholo ond curfaco aulnion probhrns,
**S day r~~ding - bmsod on prrtraatnont ohokc aim, No upsotm reportod.

TABLE 7

Aoid F1OW aaCk Analymlm

y Troatmont TYW
No. TrMtmont 811A1
walls TYDt L!!ib&U Ratio Romsrk8

2 currmt std. 107 2497 ,04311 Rigid film smulolon

4 Ryotom A 134 312s ,04311 ..
5 lyotm B 216 40: ,05311 colloidal IiliC~ dctaat~d
in aolidc mralysia

406
 * Inhibitor Ot mmt 5* EGMBZ 10* EGmw

o .574 N.T, N,T.

2 ,011 .021 .032

,5 .000 , Ola .030

.8 .008 .011 *O1O

1,6 N.T. ,005 .009

7.!5 ~ lost Hcl w

t Inhibitor 08 BGHBE 5* WMBE 104 EGMBE

o ,235 N,T. N.T,

.2 .066 ,011 .025

,5 .016 .015 .019

.0 .009 .009 ,008

2,6 NoTo .005 .006

N.T. - not twstod

-,

M.1+A)7JWHCI tutRu!hod,(D)7s*nol ~*@ In@hod*

end (0) 7omt%mwELd pa msthod.

m
=
.-.
-. .

408