Mathematical Modeling of Secondary
Precipitation From Sandstone Acidizing
Y.-H. Li, SPE, J.D. Fambrough, SPE, and C.T. Montgomery, SPE, Arco E&P Technology
Summary
Field and laboratory experience clearly demonstrates that, besides
primary dissolution, precipitation from both secondary and tertiary
reactions with aluminosilicates adversely affects matrix acid treat-
ment success. In the secondary reaction, fluosilicic acid from the
primary dissolution will further react with aluminosilicates to form
hydrated silica on the matrix surface. In the tertiary reaction,
aluminum fluoride also extracts aluminum from aluminosilicates to
form silica gel by lowering the fluoride/aluminum (F/Al) ratio in
the solution. In the presence of a high concentration of metal ions,
metal fluorides and fluosilicates are also likely to precipitate.
An optimum acidizing design package can be derived for a
specific formation mineralogy and damage mechanism if this
complex reactive system can be modeled properly. A geochemical
model for acidizing has been developed for this purpose. The
numerical simulator is a reactive flow model that solves the reactive
system with both reaction kinetics and chemical equilibrium cal-
culations. All possible reactions among all species in the system are
solved simultaneously. As acid spends, the computer simulation
shows the progress of aluminosilicate dissolution and the formation
of different precipitates as the change of dissolved species along the
reaction path occurs. The evolution of the damage skin can be
evaluated as simulation continues. On the basis of simulation,
different pumping schedules with different types of acids can be
quickly evaluated to optimize treatment volume and minimize
precipitation of hydrated silica and other precipitates.
To validate the model, a series of laboratory coreflood tests has
been fully analyzed. The results indicate that the formation of silica
gel is significant, on the basis of hydrofluoric acid (HF) effluent
analysis. The same set of kinetic data derived from the laboratory
coreflood data adequately predicts and explains a sandstone acidiz-
ing field case.
Introduction
It is always difficult to describe a reactive system that contains
numerous species by several reaction equations without including
all other possible interactions among the species. Many simplifi-
cations to describe sandstone acidizing chemistry have been re-
ported, but a comprehensive solution or a systematic approach to
encounter all possible interactions in an acidizing environment
requires a geochemical model, especially if secondary and tertiary
reactions are to be accounted for in the system. The geochemical
model described here integrates both equilibrium and kinetically
controlled reactions into a comprehensive framework. The reactive
system is based on a Gibbs free energy minimization technique with
kinetically controlled mineral dissolution. The numerical simulator
has the following features: the model is an isothermal, aqueous-
phase, one-dimensional (1D) radial flow simulator; staging is
allowed for different injection fluids pumped in sequence; two sets
of mineralogy are allowed— one for the rock and one for the
damage; and porosity/permeability correlations are used to deter-
mine a changing skin factor with pump time and treatment volume.
Ten species are allowed in the input file. These include two acids
[hydrochloric acid (HCl) and HF] and eight minerals (quartz,
K-feldspar, Na-feldspar, kaolinite, smectite, illite, calcite, and si-
derite). Reaction kinetics are built in for the dissolution of all eight
Copyright 1998 Society of Petroleum Engineers
This paper (SPE 53001) was revised for publication from paper SPE 39420, first
presented at the 1998 SPE International Symposium on Formation Damage Control
held in Lafayette, Louisiana, 18–19 February. Original manuscript received for review
30 January 1998. Revised manuscript received 8 September 1998. Revised manu-
script approved 25 September 1998.
SPE Journal, December 1998
minerals. The acidizing equilibrium chemistry includes 11 elements
and 74 species, which embodies most of the dissolved or disasso-
ciated species and other possible precipitates formed from the
reactions of the above minerals.
Sandstone Acidizing Chemistry
The chemical reactions between sandstone minerals and HCl/HF
are complex but reasonably understood on an individual basis.1, 2
However, the number and variety of minerals commonly found in
sandstones, coupled with the complexity of the reactions involving
HF, HCl, silicates, and aluminosilicates, make a detailed acidizing
chemistry description very challenging.
Primary Reaction. A reasonable simplification of the primary
reaction in such a system is to lump minerals of similar reactivity.
Quartz reacts relatively slowly with HF, whereas aluminosilicates
(clay minerals, feldspars, and mica) react relatively rapidly.3-6
Hence, the HCl/HF/sandstone system can be approximated with
two dissolution reactions as
Quartz 1 HF 3 H2 SiF6 . . . . . . . . . . . . . . . . . . . . . . . . . . . . (1)
or SiO2 1 6HF 3 H2 SiF6 1 2H2 O . . . . . . . . . . . . . . . . . . . . (2)
and
Aluminosilicates 1 HF 3 H2 SiF6 1 fluorides of Al, etc.
. . . . . . . . . . . . . . . . . . . . . . . . . . (3)
The reaction of K-feldspar with HF is given in Eq. 4 as an example;
however, the reaction of other aluminosilicates (feldspar or clay)
would form similar species.
KAlSi3 O8 1 ~n 1 3m!HF 1 ~16 2 n 2 3m!H1
3 K1 1 AlF~32n!
n 1 3SiF~42m!
m 1 8H2 O, . . . . . . . (4)
where index n may take any integer value in the range of 0 to 6,
and m 5 4 to 6. If n 5 1 and m 5 4, then three protons will be
needed to advance the reaction. If n 5 2 and m 5 6, then four
protons will be generated as the reaction proceeds to the right side.
SiF(42m) is shown as the general form of fluosilicic acid. SiF4 is an
m
intermediate compound and will convert to SiF22 as it is being
6
consumed in the reactive system. SiF2 5 will coexist in solutions, but
the majority of fluosilicic acid will be found as SiF22 6 or H2SiF6
because of equilibrium constraints. It is important to recognize that
AlF(32n) is also in equilibrium. From 19F nuclear magnetic reso-
n
nance spectroscopy studies, a distribution of the fluoride on the
aluminum has been reported.7–9 For example, at a F/Al ratio of 1.5,
Al31, AlF21, AlF1 21
and AlF1
2 , and AlF3 are all present, with AlF 2
each composing about 45% of the aluminum species and Al31 and
AlF3 each composing about 5%.
Examples of K-feldspar dissolution that illustrate the effect of the
forms of fluosilicate and fluoaluminate ions on HF and proton
consumption are
KAlSi3 O8 1 13HF 1 3H1 3 K1 1 AlF21 1 3SiF4 1 8H2 O,
. . . . . . . . . . . . . . . . . . . . . . . . . . (5)
KAlSi3 O8 1 18HF 3 K1 1 2H1 1 AlF21 1 3SiF22
6 1 8H2 O,
. . . . . . . . . . . . . . . . . . . . . . . . . . (6)
393
 KAlSi3 O8 1 20HF 3 K1 1 4H1 1 AlF1
2 1 3SiF6 1 8H2 O,
22
. . . . . . . . . . . . . . . . . . . . . . . . . . (7)
and KAlSi 3 O8 1 21HF 3 K1 1 5H1 1 AlF3 1 3SiF 22
6 1 8H2O.
. . . . . . . . . . . . . . . . . . . . . . . . . . (8)
Proton creation or consumption is dependent upon the available
forms of aluminum fluorides and fluosilicic acids from the reactions
of aluminosilicates with HF.
Secondary Reaction. The secondary reaction of HF with alumi-
nosilicates is the reaction of fluosilicic acid derived from the
primary reaction with an aluminosilicate to form hydrated sil-
ica.10, 11 Two examples with K-feldspar and illite are given as
1
6 1 6KAlSi3 O8 1 18H 1 10H2 O
SiF22
1
3 6K 1 6AlF 21
1 18H2 SiO3 1 H4 SiO4 , . . . . . . . . (9)
and SiF 22
6 1 KAl3 Si3 O10 ~OH!2 1 6H1 1 4H2 O
3 K1 1 3AlF1
2 1 4H4 SiO4 . . . . . . . . . . . . . . . . (10)
Dissolving the silicon in the aluminosilicate results in an amor-
phous silica gel film. In addition, the silica in SiF22
6 also precipitates
as silica gel.
Tertiary Reaction. The tertiary reaction of HF with alumosilicates
involves the further reduction of the F/Al ratio in dissolved alu-
minum fluoride species. The reaction extracts aluminum out of
aluminosilicates and leaves silica gel in the matrix.7, 8 An example
of the tertiary reaction with K-feldspar can be written as
AlF1 1
2 1 KAlSi3 O8 1 4H 1 4H2 O
3 K1 1 2AlF21 1 3H4 SiO2 . . . . . . . . . . . . . . . . . . (11)
This reaction continues to reduce the F/Al ratio in the spent HF until
the remaining HCl is consumed.
Precipitates. Although acidizing reactions result in precipitation
in some cases, some undesirable reactions can be avoided by
following proper procedures and taking precautions. The following
gives the possible precipitates in sandstone acidizing and their
origins.
Colloidal Silica. Amorphous silica comes from clay and silicate
dissolution in HF. H2SiF6 extracts aluminum from any alumino-
silicate mineral and simultaneously deposits amorphous silica.
Hydrated silica can be in the forms of H2SiO3 (or SiO2:H2O) and
H4SiO4 [or Si(OH)4 and SiO2:2H2O]. H2SiO3 has been identified as
amorphous silica in acidizing experiments.12 The difference be-
tween H2SiO3 and H4SiO4 is the degree of hydrolysis. Colloidal
silica precipitation occurs when the HF initially present is nearly
consumed and the solution contains a relatively high amount of
fluosilicate ions, SiF22
6 . When amorphous silica forms, it forms on
the surface of clay and silt, resulting in a retardation of further clay
acidization. This results partly from the greater affinity of fluorine
for aluminum than for silicon as
H2 SiF6 1 6Al31 1 4H2 O 3 6AlF21 1 6H1 1 H4 SiO4 .
. . . . . . . . . . . . . . . . . . . . . . . . . . (12)
This expression can be illustrated in two steps in Eqs. 13 and 14.
Fluosilicate ions are hydrolyzed, and amorphous silica is deposited at
the surface of the clay/fines. Simultaneously, HF is generated and
aluminum is preferentially removed from clay minerals, which results
in additional amorphous silica. Silica gel precipitation from the first
step increases with HCl concentration, as illustrated in Eq. 13.
1 Fe21 is not considered to be a problem because ferrous hydroxide
6 1 2H 1 4H2 O 7 H4 SiO4 1 6HF, . . . . . . . . . . . . . (13)
SiF22
and 6Al31 1 6HF 7 AlF21 1 6H1. . . . . . . . . . . . . . . . . . . (14)
394
Aluminum and aluminum fluorides in solution can also react with
fluosilicic acid if the species with fewer fluorides are more reactive
toward fluosilicic acid. This will convert more fluosilicic acid to
silica gel. One can write a balanced reaction for this process as
1 1
6AlF21 1 SiF22
6 1 4H2 O 3 6AlF2 1 H4 SiO4 1 4H .
. . . . . . . . . . . . . . . . . . . . . . . . . . (15)
The reaction is, in fact, in equilibrium because, once the fluoride
is associated with aluminum, it will be distributed among the
various aluminum fluoride species in accordance with its equilib-
rium behavior. A high proton concentration can also force hydrated
silica to dissolve and rebalance the Al/F ratio in solution.
Silica gel is a hydrated silica, so a high concentration of HF will
force silica gel to dissolve following the same dissolution of silica
as known in the primary reaction,
1
H4 SiO4 1 6HF 7 SiF22
6 1 2H 1 4H2 O. . . . . . . . . . . . . . (16)
Aluminum Salts. The dissolved aluminum can form six com-
plexes with fluorine: AlF21, AlF1 2 22 32
2 , AlF3, AlF4 , AlF5 , and AlF6 .
(32n)
AlFn is a general form of fluoaluminic acid with n from 1 to 6.
All can coexist and are controlled by equilibrium relationships in
the solution. AlOH21, Al(OH)1 2
2 , Al(OH)3, and Al(OH)4 can also
form. Walsh et al.13 showed that AlF3 and Al(OH)3 precipitates can
form during sandstone acidizing. AlF3 can precipitate if the HF
concentration is still high but the ratio HCl/HF is low. Al(OH)3 can
precipitate if both HF and HCl concentrations are low (i.e., toward
the end of the reaction from an initially strong HCl/HF acid
formulation).
Calcium Fluoride. Calcite reacts very quickly and completely
with HCl acid, but, in the presence of HF, the reaction proceeds.
CaCO3 1 2HF 3 CaF2 1 H2 O 1 CO2 . . . . . . . . . . . . . . (17)
CaF2 has a very low solubility. However, preflushing with HCl acid
can minimize this reaction. An adequate preflush has to be injected
to remove all the carbonate material from the near-wellbore region
before an HF treatment. Calcium fluoride also forms from the
reaction of calcium chloride completion fluid with HF.
Sodium and Potassium Fluosilicates and Fluoaluminates. The
reaction products, fluosilicic acid and fluoaluminic acid, are readily
soluble in water, but their potassium, sodium, and calcium salts are
partially insoluble. The salts are formed by the following reactions.
1
6 1 2K
SiF22 3 K2 SiF6 , . . . . . . . . . . . . . . . . . . . . . . . . . (18)
1
6 1 2Na
SiF22 3 Na2 SiF6 , . . . . . . . . . . . . . . . . . . . . . . . (19)
1
and 6 1 Ca
SiF22 3 CaSiF6 . . . . . . . . . . . . . . . . . . . . . . . . (20)
Sodium and potassium fluosilicates precipitate from feldspar or
illite clay dissolving in HF or by seawater/brine mixing with spent
HF. These fluosilicate precipitates are more likely to form during
the initial phases of the dissolution because high concentrations of
HF enhances the process. Additionally, fluosilicate can react with
calcite in the formation to form calcium fluosilicate. Dissolving
calcite around the wellbore with a preflush minimizes damage from
this precipitate. Formation of K3AlF6, Na3AlF6, and Ca3(AlF6)2 has
also been reported.14 Thus calcium, potassium, and sodium ions
should not be mixed with either spent or unspent HF. Formation
water, which contains calcium chloride, sodium chloride, and
potassium chloride, should be avoided. The only compatible salt
solution with HF is ammonium chloride.
Iron Precipitates. Ferric hydroxide forms when acid spends and
pH rises. Sources of ferric iron include some minerals, such as
chlorite, siderite, and hematite, and tubing rust. These HCl-soluble
minerals begin to precipitate gelatinous ferric hydroxide as the pH
rises above 2.2. A preflush of HCl is used to remove most of the
soluble iron. Ferrous hydroxide forms if the pH rises above 7.0. The
precipitates at pH between 7.7 and 9, which is normally above the
pH of spent acid.
SPE Journal, December 1998
Model Description
Chemical reactions between sandstone minerals and HCl/HF are
complex. The intricacy of the various species interactions make
quantifying the impact on specific species formation from a single
process variable change almost impossible as reservoir and treat-
ment conditions vary. Computer simulation can be helpful in
resolving this and can be used in diagnosing the potential of
precipitates and maximizing treating efficiency.
The simulator is an isothermal, aqueous-phase, 1D radial flow
model. This is a reactive flow model simulating acid/mineral
reactions within a formation matrix. To mimic field operations, the
re-form. However, the model is set to prevent dissolution from
exceeding its equilibrium limitation. The initial acidizing kinetics
data were derived from internal laboratory data and the litera-
ture.23-25 There may be several chemical formulas for each mineral.
The exact formulas used in the simulator are SiO2 for quartz, KAlSi3O8
for K-feldspar, NaAlSi3O8 for Na-feldspar, Al2Si2O5(OH)4 for kaolin-
ite, Al2Si4O10(OH)2 for smectite, KAl3Si3O10(OH)2 for illite, CaCO3 for
calcite, and FeCO3 for siderite. The exact dissolution equations used
in the model are summarized as
SiO2 1 6HF 3 2H1 1 SiF2
6 1 2H2 O, . . . . . . . . . . . . . . . (21)

input file allows users to stage treatments with different injection

KAlSi3 O8 1 20HF 3 K1 1 4H1 1 AlF1
2 1 3SiF6 1 8H2 O,
22
fluids in sequence. One can specify two different sets of miner-
alogies, one for the formation matrix and one for the damage . . . . . . . . . . . . . . . . . . . . . . . . . . (22)
material. This allows the composition of the invading solids to be
different from the matrix mineralogy. Given a single mineral, the NaAlSi3 O8 1 20HF
native mineral and invading solid mineral can also have unique
properties in terms of reaction rates and the effect of the porosity 3 Na1 1 4H1 1 AlF1
2 1 3SiF6 1 8H2 O,
22

change on permeability.
The mass transfer equations for reactive species transport include . . . . . . . . . . . . . . . . . (23)
both convection and diffusion processes. The reaction calculations
use equilibrium reactions with options to include rate-controlled Al2 Si2 O5 ~OH!4 1 16HF 3 2H1 1 2AlF1
2 1 2SiF6 1 9H2 O,
22

reactions. Some of the chemical reactions are assumed to be in

equilibrium (modeled with Gibbs free energy minimization), . . . . . . . . . . . . . . . . . . . . . . . . . . (24)
whereas others are rate-limited (modeled with empirically deter-
mined kinetic rate equations).13, 15-18 The simulator allows an ar- Al2 Si4 O10 ~OH!2 1 28HF
bitrary combination of kinetic and equilibrium reactions as long as
it involves a sufficient number of chemical species. In general, if 3 6H1 1 2AlF1
2 1 4SiF6 1 12H2 O,
22

the reactions in a system are limited by the time domain of interest, . . . . . . . . . . . . . (25)
users have to provide reaction rates. The algorithm for equilibrium
calculations is based on a Gibbs free energy minimization routine KAl3 Si3 O10 ~OH!2 1 24HF
developed by Smith and Missen,19 thus freeing the system reaction
specifications with equilibrium constants. 3 K1 1 2H1 1 3AlF1
2 1 3SiF6 1 12H2 O,
22

Because mineral dissolution during an acidizing treatment is

dominated by the kinetically controlled process, all initial minerals . . . . . . . . . . . . (26)
in the system have their own kinetic expressions. After dissolution,
interactions of dissolved species and reprecipitation continue. Both CaCO3 1 H1 3 Ca21 1 HCO2
3, . . . . . . . . . . . . . . . . . . . (27)
dissolved species and reoccurring secondary precipitates are de-
rived from the equilibrium calculations. Nonuniform grid spacing and FeCO3 1 H1 3 Fe21 1 HCO2
3 . . . . . . . . . . . . . . . . . . (28)
along the radial direction is used to obtain better resolution around
the wellbore region where damage is the highest. A detailed chemical Although the actual reactions may be different from these expres-
description of all reactants and subsequent species can be obtained near sions, the sequential equilibrium calculations will convert the
the wellbore or at any location from the wellbore to a defined boundary reaction products to other species in the aqueous phase according
during the entire acidizing treatment. The sequential steps used in the to chemical equilibrium. Eqs. 29 and 30 illustrate two examples of
simulation calculations are flashing the initial composition, mass the secondary reaction in which fluosilicic acid reacts with alumi-
transfer calculation, kinetic calculation, equilibrium calculation, po- nosilicates to form hydrated silica,
rosity calculation, permeability calculation, and pressure profile cal- 1
culation. Separating the kinetically controlled mineral dissolution from 6 1 3NaAlSi3 O8 1 8H 1 16H2 O
SiF22
the equilibrium calculations and using minimum grid spacing without
altering chemical equilibrium speed up the simulations and allow the 3 3Na1 1 3AlF1
2 1 10H4 SiO4 , . . . . . . . . . . . . . . . (29)

model to run on a Pentium 133 PC in 5 to 10 minutes. 1

Database for Chemical Equilibrium Calculations. The database
for the sandstone acid reactive system contains 11 elements and 74
species. These 74 aqueous and mineral species are mainly derived
from 11 elements: H, Cl, F, Si, Al, K, Na, Ca, Fe, C, and O. The
required thermodynamic data for each species includes enthalpy
and Gibbs free energy at the standard state and a temperature
function of the species’ heat capacity.20-22 Three main groups of
soluble species in the database are aluminum fluorides (Al31,
AlF21, AlF1 2 22 32
2 , AlF4 , AlF5 , and AlF6 ), aluminum hydroxides
(AlOH21, Al(OH)1 2
2 , and Al(OH)4 ), and silica fluorides (SiF4 and
SiF22
6 ). The precipitates from the aqueous-phase reactions are CaF2,
AlF3, Na2SiF6, K2SiF6, CaSiF6, and H4SiO4.
6 1 KAl3 Si3 O10 ~OH!2 1 6H 1 4H2 O
SiF22
3 K1 1 3AlF1
2 1 4H4 SiO4 . . . . . . . . . . . . . . . . . . . (30)
Similar expressions can be given to the tertiary reaction. Note that
all aluminum fluorides are expressed as AlF1 2 and silica fluorides
are in the form of SiF22
6 . The chemical equilibrium calculations will
redistribute the species from both secondary and tertiary reactions
with the appropriate concentrations in the system as explained in
the primary dissolution.
For an unknown kinetic expression, dissolution reactions are
assumed to be first order with respect to the concentrations of
solvent and the minerals. Quartz is minutely soluble in HCl but will
readily dissolve in HF. A simple expression is

Kinetic Expressions. The input data include two acids (HCl and
HF) and eight different minerals (quartz, Na-feldspar, K-feldspar,
kaolinite, smectite, illite, calcite, and siderite). All eight minerals
have their own irreversible dissolution expressions. The justifica-
tion for an irreversible setup is that, in the acidizing treatment
domain, there is not sufficient time for the dissolved minerals to
dCq
2 5 kq ~HF!a ~Cq !, . . . . . . . . . . . . . . . . . . . . . . . . . . . . (31)
dt
where C q 5 silica concentration. Aluminosilicates dissolve in HF
but also slightly dissolve in HCl. Aluminosilicate can further react
with fluosilicic acid in the secondary reaction and with aluminum

SPE Journal, December 1998 395

fluoride in the tertiary reaction. To account for all these, the rate
equation is expressed as a function of multivariables as and ki 5 ko SD
fi n
fo
. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . (41)

dCa 1 1 The final skin can be calculated as

2 5 f ~HF, SiF21
6 , AlF2 , H , Ca !, . . . . . . . . . . . . . . . . (32)
dt

OFS D G S D
N
fi n
ri
where C a 5 aluminosilicate concentration. There are many com- S5 2 1 ln . . . . . . . . . . . . . . . . . . . . . . . (42)
binations that can furnish the above expression. In the model, fo ri21
i51

dCa The porosity/permeability correlation illustrated previously is a

2 5 ~ka1 ~H1!a 1 ka2 ~HF!b ~H1!c
dt general and simple expression. The proposed correlation for this
work is
1 e 1 f 1 g
1 ka3 ~SiF21
6 ! ~H ! 1 ka4 ~AlF2 ! ~H ! )Ca . . . . . . . . . (33)

d
is suggested. A precise expression requires laboratory experiments
on a given mineral to determine the form of the rate equation and
the coefficient and power index on the concentration terms.
A true kinetic rate expression should also include mass transfer
constraints, such as surface area. The rate expression as a function
of mineral concentrations is a self-imposed rate limitation. In
addition to the concentration term, two multipliers to the rate
expression, which corrects for mineral surfaces not exposed to pore
fluid in the acidizing system, are given. For inaccessible minerals,
this multiplier is
~C 2 Cmin!
, . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . (34)
~Co 2 Cmin!
where C o is the mineral initial concentration and C min 5 an
empirical number; and, for silica gel coatings, the multiplier is
CH4SiO4
~1 2 u ! where u 5 . . . . . . . . . . . . . . . . . . . . . (35)
CH4SiO4 , o
u 5 the fraction of mineral coated by silica gel, and the denominator
is an empirical number. Both terms can be used to multiply the rate
expression to incorporate the mass transfer effect into the mineral
dissolution.
Definition of Skin and Porosity/Permeability Correlations.
Skin is a common name used in describing wellbore damage. It is
a parameter to accommodate a Darcy’s flow calculation for a
damaged wellbore. It is a dimensionless number and does not
provide any information about how far damage penetrates into the
formation or how the damaging material is distributed in the pore
space. The definition of skin can be described as
PS D
k fi21 2 ~Vi, o 2 Vi ! ni
5 , . . . . . . . . . . . . . . . . . . . . (43)
ko fi21
i51, N
where N 5 the number of solid species, and V 5 the volume of a
specific mineral. This gives each individual mineral its own cor-
relation on the effect of a porosity change on permeability.
Laboratory Data Validation
The objective is to validate the acidizing geochemical model with
a comprehensive laboratory acidizing experimental program.
Laboratory Program. Lindsay26 carried out a series of acidizing
experiments in Berea sandstone. A high strength acid (12% HCl/3%
HF; no preflush) was injected through Berea plugs at five different
flow rates at both 77°F and 125°F. A total of 10 complete tests
(Runs 3 to 12) have been reported and provide details on HF
effluent concentrations vs. pore volumes (PV’s) of the acid injected,
along with porosity and permeability data of the tested cores. The
core plugs used were 1 in. in diameter and 4 in. long with initial
porosity about 18.6% and initial permeability around 100 md. The
mineral composition includes quartz, feldspar, chlorite, illite, do-
lomite, calcite, and siderite. Table 1 provides the flow rate and PV
injected during each experiment. The cores were injected with the
HCl/HF acid up to more than 80 PV. This experimental program
is similar to acidizing in the very near wellbore region (i.e., 4 in.
from the wellbore).
Data Interpretations by Others. Lindsay’s data have been ex-
tensively analyzed in several sandstone acid two-component, four-
component, and geochemical models.3-5, 16, 27 Three of these ex-
periments (Runs 8, 9, and 12) have been well interpreted with a
four-component model that includes HF, two lumped minerals, and

SD SD
silica gel from a secondary reaction.27 Neither the two-component
ra kR ra nor the four-component model accounts for the room temperature
S 1 ln 5 ln . . . . . . . . . . . . . . . . . . . . . . . . . . . . (36) data. The U. of Texas KGEOFLOW geochemical model gives a
ro ka ro
better interpretation of six experiments at both temperatures.16 The
or S5 S DSD
kR
ka
2 1 ln
ra
ro
, . . . . . . . . . . . . . . . . . . . . . . . . . . . (37)
reported precipitates were K2SiF6, and AlF3. Silica gel was only
observed in Run 12. No reports were given on the final porosity and
permeability. This could be because the experiments assumed that
where S 5 skin, a dimensionless number; r a 5 damaged radius; the carbonates were completely dissolved after injecting about 2 PV
r o 5 wellbore radius; k a 5 damaged zone permeability; and k R 5 12/3 HCl/HF, and therefore, carbonates were not included in the
reservoir permeability. This leads to the expression for calculating KGEOFLOW simulation.
the flow rate in a damaged wellbore,
kR hDp
q5 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . (38) TABLE 1—EXPERIMENTAL PROGRAM CONDUCTED BY
m~S 1 ln~ra /ro !! LINDSAY
Skin is also a summation of individual skins as defined by
125°F 77°F

O OS DS D
N N
kR ri Run Flow Rate PV Run Flow Rate PV
S5 Si 5 2 1 ln . . . . . . . . . . . . . . . . . . . . (39) Number (mL/sec) Injected Number (mL/sec) Injected
ki ri21
i51 i51

10 0.327 25 4 0.342 88
In the damaged zone, the permeability increases inward into the
9 0.248 80 5 0.250 86
reservoir as the porosity increases with the radius. From the
assumption of a linear variation of porosity and a simple porosity 11 0.175 26 6 0.130 88
vs. permeability relationship,2 such as 8 0.128 81 7 0.063 83
12 0.063 30 3 0.062 87
fi 5 fo 2 a~D 2 ri ! . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . (40)

396 SPE Journal, December 1998

Experimental Results vs. Simulations From This Work. To
conduct coreflood simulations, the model was modified for a linear
flow. Table 2 gives the sandstone mineralogy used in the simula-
tion. These include quartz, K-feldspar, Na-feldspar, illite, calcite,
and siderite. Because dolomite and chlorite are not included in the
model, dolomite was replaced with calcite and chlorite was re-
placed with additional illite. These 10 tests are analyzed and
simulated in the model; the data fitting includes HF effluent,
porosity, and final permeability in the cores.
Figs. 1 and 2 (for 125°F) and Figs. 3 and 4 (for 77°F) present
both experimental and simulation results of HF effluent concen-
trations vs. PV of the acid injected for various injection flow rates.
Table 3 gives both measured and predicted porosity data for two
tests (Runs 10 and 11). Fig. 5 (for 125°F) and Fig. 6 (for 77°F) plot
the final data for all the tests from both experimental and predicted
permeabilities. The purpose is to illustrate that the model can do a
comprehensive interpretation rather than just fit several experi-
ments or several parameters. Table 4 furnishes the kinetic data used
in this exercise.
HF Consumption. Consumption of HF is an indication of the
degree of acidizing or silicate and aluminosilicate dissolution. The Fig. 1—HF effluent concentration from corefloods at 125°F.
conversions of aluminum to aluminum fluorides and silica to silica
fluorides are the main usage of fluoride. On the basis of HF
consumption (experimental vs. predicted), the model appears to
overpredict the flow rate effect, especially for the corefloods
conducted at 125°F. The reason is that the HF consumption does
not increase as much as the predictions with a decrease of flow rate
(or the consumption of HF in the experimental work does not
decrease as much as the model predictions with an increase of flow
rate). In the secondary reaction, fluosilicic acid (SiF226 ) is converted
to hydrated silica (H4SiO4). The filming effect from hydrated silica
gel reduces the reactive surface area and slows down the reaction.
The model may not impose the filming effect as severely as it
should. A severe filming effect will make the HF consumption less
sensitive to a flow rate change. The other reason is that, in the
secondary reaction, the conversion of fluosilicic acid to hydrated
silica reduces the total fluoride consumption from a total material
balance viewpoint. This also results in a smaller change in the net
HF consumption with respect to the flow rate changes. The con-
sumption of HF can serve as an indicator of the severity of the
hydrated silica formation. In other words, this also might indicate Fig. 2—Predicted HF effluent concentration for corefloods con-
that the real damage in the corefloods could be greater than that ducted at 125°F.
predicted by the model. These results support the recommendations
made by Paccaloni et al.28 of injecting acids at the highest rate
possible to minimize precipitation. This also supports the point that
the time that spent acid remains in the formation should be min-
imized.24, 29
Colloidal Silica. H4SiO4, or Si(OH)4, is perhaps the most im-
portant precipitating mineral in sandstone acidizing. Field experi-
ence and laboratory coreflood experiments have produced evidence
of the precipitation of Si(OH)4.2, 29-31 As reservoir minerals are
dissolved, aluminum and silica compete for the available fluorine.
Aluminum has the greater affinity for fluorine; so when the level
of free fluorine is reduced, silica precipitates in the form of Si(OH)4.
Fig. 7 and Table 5 show the sensitivity of silica gel precipitation.
In Fig. 7, the predicted upper curve was derived from a very high
conversion of SiF22 6 to H4SiO4. This results in a low consumption
of HF. This can also result in a low porosity in the core, as indicated

TABLE 2—MINERAL CONTENT USED IN SIMULATION

Mineral wt%

Quartz 70.0 Fig. 3—HF effluent concentrations for corefloods conducted at

K-feldspar 2.5 77°F.
Na-feldspar 2.5
Illite 15.0 in Table 5. The lower curve shows that, if H4SiO4 does not form and
Calcite 5.0 all dissolved silica remains as SiF22
6 , the consumption of HF will

Siderite 5.0 be very high and the HF effluent curve will be very low. This also
results in a high porosity in the core because no silica gel deposits

SPE Journal, December 1998 397

 Fig. 6 —Experimental vs. predicted permeabilities of corefloods
conducted at 77°F (initial permeability about 100 md).

TABLE 4—KINETIC DATA

Activation Surface
Frequency Energy Area
Fig. 4 —Predicted HF effluent concentrations for corefloods Name Factor (Kcal/g mol) (m2/g)
conducted at 77°F.
Quartz 0.136E207 5.0 0.005
K-feldspar 0.135E205 8.0 1
TABLE 3—SECTIONAL POROSITIES DETERMINED BY Na-feldspar 0.760E206 8.0 1
CORE LABORATORIES vs. PREDICTED FOR TWO
ACIDIZING CORES Kaolinite 0.174E204 10.0 23
(INITIAL POROSITY: 18.6%) Smectite 0.361E205 9.5 82
Illite 0.776E205 10.0 113
Porosity
(%)
Run
Number Core Section Measured Predicted

10 Front 30.5 32.0

10 Middle 27.5 25.4
10 Back 24.9 19.4
11 Front 31.9 35.4
11 Middle 27.4 22.9
11 Back 25.2 20.1

Fig. 7—Effects of silica gel formation on HF consumption for the

coreflood conducted at 0.128 mL/sec and 125°F.

Fig. 5—Experimental vs. predicted permeabilities for corefloods

conducted at 125°F (initial permeability about 100 md).
in the matrix. The sensitivity study related to HF consumption and
porosity provides a confirmation of the degree of silica gel forming
in the matrix during the coreflood. Fig. 8 shows a simulation of the
formation and dissolution of silica gel in the core as a function of
time or the PV’s of the acid injected. After 80 PV 12/3 HCl/HF
pumped through the core, silica gel formed from the secondary
reaction is completely dissolved. Dissolving silica gel is similar to
dissolving quartz or silica. After most aluminosilicates have been
dissolved, the silica gel from the secondary reaction begins to
dissolve as HF/HCl continues to be pumped through the core. The
predicted pore space occupied by silica gel during an acidizing
experiment can be as high as 30%.
AlF3(s) Precipitate. AlF3(s) is observed in the simulation, as
illustrated in Fig. 9 for Run 9. Its formation in the pore space is on
the same order of magnitude as silica gel. After forming, it dissolves
slightly and slowly relative to silica gel formation. A duplicate of
the Run 9 simulation at 200°F shows that silica gel exists in the
same order of magnitude as that at 125°F, but AlF3(s) completely
disappears. This might explain why most flowback fluid analyses
show a high ratio of Al/Si. This ratio can be one to two orders of
magnitude greater than the Al/Si ratio present in the minerals
because dissolved aluminum is in solution and silica precipitates are
in the formation.23-25, 30

398 SPE Journal, December 1998

 TABLE 5—SECTIONAL POROSITIES IN PERCENT

Degree Location in the Core

of Silica
Gel
Formation Front Middle Back

Low 30.9 31.8 31.5

Moderate 33.4 21.3 21.7
High 24.6 19.6 20.4

Fig. 10 —Simulated calcium fluoride formation during coreflood

at 0.248 mL/sec and 125°F.

Fig. 8 —Simulated silica gel formation and dissolution during

coreflood at 0.248 mL/s and 125°F.

Fig. 11—Simulated calcium fluosilicate formation during core-

flood at 0.248 mL/sec and 125°F.

Iron compounds can become a real possibility in carbonates, where

Fig. 9 —Simulated aluminum fluoride formation during coreflood
at 0.248 mL/sec and 125°F.
CaF2 and CaSiF6 Precipitates. CaF2 and CaSiF6 will form, but
at lower magnitudes in comparison with silica gel or AlF3(s). Figs.
10 and 11 show the simulated results of CaF2 and CaSiF6 formation
at Run 9 conditions, respectively. An interesting observation is that
the formation of CaF2 is ahead of the formation of CaSiF6. It
appears that CaF2 has been displaced by CaSiF6. Because the
thermodynamic data for CaSiF6 were created from the mixing
values of other species, the magnitude of both CaF2 and CaSiF6
formation might not be accurate. However, this shows that calcite
reacted with HF in the formation can form calcium precipitates. In
the presence of a high strength HCl, the problem should be much
less severe. K2SiF6, is a potential precipitate from K-feldspar, illite,
and spent HF, but was not observed in the simulations. A strong
presence of calcium may suppress K2SiF6 formation. Thomas32
indicates that metal salt precipitation occurs at HF concentrations
of 3 wt% and above and that it can be reduced, but not eliminated,
by high HCl concentrations.
Iron Precipitates. Although siderite existed in the Berea core,
iron compounds are unlikely to precipitate in the presence of HCl.
there is enough carbonate material present to cause the HCl acid to
spend completely. This condition is rarely found in sandstones and,
therefore, does not pose much of a problem in sandstone acidizing.
No iron precipitates were observed from the model simulation.
Calcite and Siderite Dissolution. Calcite reacts very quickly
and completely with HCl acid. In fact, the reaction rate is so fast
that kinetic data cannot be measured at room temperature. In simu-
lation, if the dissolution of calcite occurs instantaneously, a disconti-
nuity in the HF consumption will occur, which affects the other species
balance. To prevent this, a mass transfer limitation is imposed on the
calcite dissolution to obtain a smooth HF effluent concentration curve.
A mass transfer constraint is also needed for siderite.
Field Data Validation
The field case analyzed in this paper also comes from the litera-
ture.33 It involves a sandstone acidizing treatment in an offshore
Louisiana oil well. The well produces from a 40-ft gravel-packed
zone in an unconsolidated, sandstone reservoir. A rate of only 1,222
BOPD was achieved from the expected 5,000 BOPD. An analysis
concluded that the formation damage affecting this completion was
the result of formation clays swelling when they were contacted by
completion fluids and by fines migrating toward the wellbore
during production.
The original literature33 gives details of the formation matrix and
damage mineralogy of this well and the pumping schedule. For
simulation purposes, the kinetic data generated from the laboratory
corefloods discussed in the above section were extrapolated to
218°F with the Arrhenius expression. The simulation results indi-
cated that the constraints may be because of the material balance

SPE Journal, December 1998 399

or the amount of acids needed to dissolve the damage. The damage
TABLE 6—FINAL SKINS FROM VARIOUS DAMAGE
skin was shown to be 204 initially and was reduced to 15.4 after DEFINITIONS
treatment. The simulated skins vary from 30 to 20.4, depending
upon how the damage is defined and how the damage material is 1-ft Damage Radius 1.5-ft Damage Radius
distributed in the void space of the matrix out to 1-ft radius.
Fig. 12 shows four examples of how the damage may be Damage Final Damage Final
deposited in a 1-ft radius away from the wellbore with an initial skin Definition* Skin Definition* Skin
of 204. Table 6 summarizes the simulated final skins with the
various definitions of the skin regarding invading solids distributed Uniform 20.44 Uniform 0.95
at both 1- and 1.5-ft radii. On the basis of the field results of a final Two-step 20.19 Two-step 3.02
skin of 15, the model provides a reasonable interpretation for the Three-step 2.57 Three-step 13.43
final skin in the range of 30 to 20.4 with 1-ft damage radius. There
Four-step 30.02 Four-step 77.82
is no reason to adjust the model for a perfect match. The issue is
how the damage can be better defined for a job design. The 20% * Illustrated in Fig. 12.
difference in the damage material packed in void space causes the
final skin to change from 30 to 20.4. This leads to the conclusion
that an increase in the treatment volume will eventually reduce the
skin from the treatment final skin of 15.4 to zero for this field case
if additional costs can be justified. essential to verify all thermodynamic and kinetic data used in the
model.
Conclusions 6. Methods for defining the damage mechanism and its distri-
bution remain an issue for sizing a treatment. A skin number is not
The geochemical model developed here is designed for routine sufficient to define the damage radius or damage profile. Appli-
matrix and treatment design to predict the interaction of fluids and cation of the geochemical model for engineering design remains a
minerals. It can be helpful in maximizing treating efficiency and challenge.
diagnosing the potential for precipitates to form. To a certain extent,
damaging precipitates can be avoided if the HCl/HF formulation is Nomenclature
properly matched to the formation mineralogy with the help of mod-
eling. This program furnishes a framework for this purpose. It still a, b, . . . , g 5 reaction order indices
needs refinement of the thermodynamic database for all species in- C a 5 aluminosilicate concentration per void vol-
cluded in the reactive system and more detailed specifications of the ume, g mol/ft3
kinetic equations. The general conclusions derived from this work C H4SiO4 5 silica gel concentration per void volume, g
follow. mol/ft3
1. Laboratory data validation and a field case prediction give C H4SiO4,o 5 an empirical number for silica gel concentra-
confidence in the model. tion per void volume, g mol/ft3
2. Decoupling dissolution kinetics of various minerals from C min 5 an empirical number of mineral concentration
equilibrium flash calculations and using minimum grid spacing per void volume, g mol/ft3
without altering chemical equilibrium speed up the calculations and C o 5 mineral initial concentration per void volume,
allow the simulation to be performed on a PC. g mol/ft3
3. Precipitation of colloidal silica appears inevitable and sub- C q 5 quartz concentration per void volume, g mol/
stantial. Colloidal silica occurs beyond the dissolution front and can ft3
extend into the reservoir. There is a balance between the primary D 5 distance from the wellbore to the boundary of
dissolution and secondary precipitation of colloidal silica. Higher the simulation domain, ft
flow rates correspond to less damage induced by acid. When h 5 formation height, ft
designing a job, there needs to be a compromise made in the k o 5 initial permeability, md
injection rate between efficient removal of damage and minimiza- k a 5 damaged zone permeability, md
tion of new damage by precipitation. k q 5 dissolution rate constant for quartz
4. AlF3(s) tends to disappear with an increase in reservoir tem- k a1, . . . , a4 5 dissolution rate constant for different mecha-
perature. In some cases, fluoride and fluosilicate salts, such as CaF2, nisms from 1 to 4
K3SiF6, Na2SiF6, and CaSiF6, occur within the dissolution of spent k R 5 reservoir permeability, md
HF and can be avoided with a preflush of HCl. k i 5 permeability at Location i, md
5. Key equilibrium data have to be carefully examined and n 5 power index for permeability/porosity corre-
detailed kinetic expressions have to be developed for a given lation
mineral. Validation of the model with flowback analysis of all dis- n i 5 power index of Species i for permeability/
solved species either from laboratory experiments or field samples is porosity correlation
Dp 5 pressure difference between the external
drainage radius and the well, psi
q 5 volumetric rate, B/D
r a 5 damaged radius, ft
r i 5 radius at Location i
r o 5 wellbore radius, ft
S 5 skin
S i 5 skin at Location i
t 5 time, seconds
V i 5 volume fraction of Species i, ft3
V i,o 5 initial volume fraction of Species i, ft3
a 5 regression constant for porosities at various
locations according to a given skin
u 5 fraction of surface covered by H4SiO4
m 5 fluid viscosity, cp
f i 5 porosity in the rock matrix at Location i
Fig. 12—Illustrations of the same initial skin number with differ- f o 5 initial porosity in the rock matrix
ent distribution of the damage material.

400 SPE Journal, December 1998

Acknowledgments
The authors thank Arco E&P Technology for their permission to
publish this paper. The chemical equilibrium calculations by the
Gibbs free energy minimization were derived from the computer
programs developed from the Stimulation, Logging, and Formation
Damage Research Consortium at the U. of Texas in Austin under
supervision of Larry W. Lake and Robert S. Schechter. To make
these analyses possible, their contributions are also acknowledged
and greatly appreciated.
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SI Metric Conversion Factors
bbl 3 1.589 873 E201 5 m3
cp 3 1.0* E203 5 Pazs
ft 3 3.048* E201 5 m
ft2 3 9.290 304* E202 5 m2
ft3 3 2.831 685 E202 5 m3
°F (°F232)/1.8 5 °C
in. 3 2.54* E100 5 cm
psi 3 6.894 757 E100 5 kPa
*Conversion factor is exact. SPEJ
Ying-Hsiao Li is a senior principal research engineer with Arco
E&P Technology in Plano, Texas. e-mail: yingli@arco.com. He
joined Arco in 1979 and has worked on a variety of research
issues including synthetic fuels, coal, miscible flooding, phase
behavior, formation damage, and stimulation. Li holds a BS
degree in chemical engineering from Tunghai U. and MS and
PhD degrees in chemical and fuels engineering from the U. of
Utah. John D. Fambrough is a senior research engineer at Arco
E&P Technology in Plano. He currently works on formation
damage and acidizing issues. Before joining Arco, he was a
senior chemist with BJ Services, where he worked in cementing,
sand control, and acidizing. Fambrough holds a BS degree in
zoology and an MS degree in biology from Texas A&M U. Carl
T. Montgomery is Research Advisor for well stimulation at Arco
E&P Technology in Plano, responsible for development and
transfer of stimulation technologies for Arco’s operating com-
panies. He holds a BS degree from Colorado State U. and an MS
degree in biochemistry from Ball State U. A 1998 –99 Distin-
guished Lecturer, Montgomery served on the SPE Editorial Re-
view Committee during 1984 –92 and as 1994 –95 SPE Produc-
tion & Facilities Executive Editor. He also served as a member of
the Forum Series in North America Steering Committee during
1989 –92 and in 1996 and as chairman of the 1998 Forum on
Fracture Diagnostics.
401