SPE
Society of Petf'Olelm Engineers of AIM E
SPE/DOE 11638
A Method for Evaluation of Formation Damage Due to
Fracturing Fluids
by L.J. Volk, * Amoco Production Go., and B.L. Gall, C.J. Raible," and H.B. Carroll, *
U. S. DOE, BErG
* Members SPE-AIME
This paper was presented at the 1983 SPE/DOE Symposium on Low Permeability held in Denver, Colorado, March 14-16, 1983. The material is subject
to correction by the author, Permission to copy is restricted to an abstract of not more than 300 words. Write SPE, 6200 North Central Expressway,
Drawer 64706, Dallas, Texas 75206.
ABSTRACT
The extent of formation damage due to invasion
of fracturing fluids during the hydraulic fracturing
process was studied. An apparatus, which can
simulate reservoir conditions, is described for
measuring permeability before and after fluids are
pumped across the surface of a core. Dynamic
fluid loss was also measured of fluid which passes
through the core plug.
After the fluid pump schedule was completed,
high gas pressure was applied in the reverse
direction from fluid leak-off to measure fluid
cleanup and the extent of core damage. The system
had a wide dynamic range and the measurements have
been automated.
INTRODUCTI ON
A potentially large natural gas resource
exists ;n low permeability reservoirs of the
western United States (1,2). Massive hydraulic
fracturing (MHF) has been used extensively to
increase production from tight blanket sands
(3,4). However, MHF results have been mixed for
the Mesaverde and Fort Union sands of the Rocky
Mountain area (5). Various studies have been
initiated to develop technology for producing
these low permeability, lenticular sands (6,7).
Many factors can reduce the effectiveness of
the hydraulic fracture treatment including damage
to the formation and propped fracture from the
fracturing fluids, fluid leak-off, clay swelling,
precipitation of solids or migration of fines.
Some studies have been done which estimate possible
formation damage in low permeability reservoirs in
order to design fluids or methods to minimize the
damage (8- 13) •
References and illustrations at end of paper.
333
In connection with the DOE Western Gas
Sands sub-program and Multi-Well Experiment,
it was desirable to build an apparatus which
could evaluate formation damage from fracturing
fluids by determining permeability to gas
before and after exposure at simulated reservoir
temperatures and fracturing pressures. The leak-
off rate of fracturing fluids can also be measured
with this apparatus.
Guar gum and its derivatives, such as
hydroxypropyl guar have been effective gelling
agents in fracturing fluids for many years. While
improved polymers have been developed, (13-16)
guars continue to be the dominate gelling agent
in use today.
EQUIPMENT DESCRIPTION
The system was designed to evaluate core
damage due to gelled fluid penetration and skin
effect at simulated fracturing conditions. Core
damage was estimated by measuring gas permeability.
In order to simulate fracturing conditions, equipment
was developed as shown schematically in Figure 1.
The apparatus used a heated, temperature controlled
pressure vessel and fluid pump capable of exerting
a hydrostatic stress up to 10,000 psi (69 MPa) on
a core sample. Test samples were cylinders 3.8
cm diameter and typically 1.2 to 2.0 cm in thick-
ness. Inside the test cell, the sample was mounted
in a rubber sleeve between 3.8 cm diameter end
pieces. One end piece contained a cavity, 3.3 cm
diameter and 0.5 cm deep, to allow fluid flow
across the core face. Flow rate across the core
surface was typically 2 cm Imin. This produced a
shear rate of 0.3 to 2 sec-lover the core surface.
Fluids were pumped into and out of this cavity
through two holes (0.3175 em) located for maximum
hole spacing in the cavity. Fluid pressure was
maintained at the core face by a back pressure
regulator located downstream of the fluid cavity
as shown in Figure 1.
2 A METHOD FOR EVALUATION OF FORMATION DAMAGE DUE TO FRACTURING FLUIDS
The other core end piece was connected with
minimal volume tubing to allow fluids to pass
through the core. Fluid that passed through the
core was collected and weighed with an electronic
balance. The accumulated weight was recorded with
a strip chart recorder. Alternately, fluid fractions
could be collected with a fluid fraction collector.
These f~actions were weighed and analyzed by gel
p~rme~tlo~ chromatography for molecular weight
dlstrlbutlon and polymer concentrations.
Following the fluid or gel pumping operation
the equipment was changed to measure restored gas
permeability. First, the fluid cavity and connect-
ing tubing was cleared of excess fluid with a low
pressure nitrogen flow leaving gel buildup or filter
cake on the core face and the core fluid saturated.
Then, high pressure nitrogen was forced through
the core and filter cake as shown in Figure 2. For
some tests, nitrogen saturated with water vapor at
a temperature equal to the core temperature was
used to more accurately simulate reservoir conditions
Nitrogen flow through the core (related to the
effective core permeability) was measured versus
time with a gas flow measurement system.
GAS FLOW MEASUREMENT SYSTEM
In order to measure gas flow through a core
damaged with fracturing fluids, a system was devised
to measure and record the increase gas flow rate
wi~h.time. The initial gas flow through low perme-
ablllty core saturated with fracturing fluid was
extremely low. As saturation decreased, higher
gas flows were observed until the core reached
irreducible water saturation and steady state gas
flow. The time to obtain equilibrated permeability
often required hours even days. It was desirable
to not only periodically measure gas flow, but also
to ascertain when steady state flow was attained.
Therefore, an automated system was developed to
measure a widely variable gas flow rate that
accompany the changing permeability.
Various methods have been devised to measure
gas flow and core permeability. Two methods of
interest based on nonsteady state gas flow have
been described. Jones (17) measured pressure draw
down of pressure reservoir located upstream of a
core sample. More recently, Freeman and Bush (18)
described a method to measure low permeability
cores wi~h a nonsteady state gas flow through a
sample wlth a downstream pressure buildup test.
Both methods reported rapid analysis times with
go?d.accuracy. The method described in this paper
utlllzes a downstream pressure buildup (~P )
in a known volume. A solenoid valve, installed on
~he outlet of a known volume, was closed period-
lcally for a specific time interval and then
opened allowing equilibration to atmospheric
pressure. The pressure buildup was measured with
a pressure transducer and the resulting pressure
(~Pt) displ~yed.o~ a strip c~art recorder. Figure
3 snows a slmpllfled schematlc of the essential
components and parameters.
If steady state flow th~ough a core is assumed,
the volume of an ideal gas (V ) passing through
the core in time (t) can be c~lculated by the
relationship:
SPE 11638
c t
( 1)
For the system described in Figure 2, a close
approximation of the mean volume (V ) at the mean
:ore pressure (P ) may be determineS by using the
ldeal gas relati8nship when ~P c»~P t·
(2 )
Equation 2 can be rearranged to give:
t t c
. . (3)
Pc Tt
Combining equations 1 and 3, a permeability value
can be calculated
.
. . . . . (4)
At the commencement of pressure buildup, the pressure
(P t ) downstream of the core (V t ) was equilibrated
to atmosphere pressure (p). rherefore, P P
and ~P (initial) = P.-p? Assuming stead} sta~e
flow, ~t the end of t~e Bressure buildup period,
~p (flnal) P.-P = P.-(P +~P). For gas flow
thFough the cor~, i lin~ar ~ela~ionship was observed
between the pressure buildup in the confined
volume and time so long as ~P »~P. Experimental
tests revealed essentially a lineartpressure
buildup with time up to 20 percent of ~P . The
experimental procedure followed for flowcmeasure-
ments limited ~P to less than 5 percent of ~P .
Under actual exp~rimental conditions, the effeEtive
pressure across the core, ~Pc in equation 4 was:
~Pc = ~ [6P c (initial) + 6P c (final)]
Pi-CPo + ~ 6P t )
Also, the effective mean core pressure (P ) can be
expressed as: c
'" ~ [pc (initial) + Pc (final) ]
Pi + P + ~P )]
P. + (p
=~ [ 0 + lot
2 2
=~ [Pi + (PO+~6Pt)J
Therefore, equation 4 can be rewritten in experi-
mentally measured parameters.
The above formulation assumes a constant temperature
(T t ) and pressure equilibrium throughout the
bUildup volume. The temperature of the gas leaving
the core is approximately the core temperature (T )'
c
334
SPE 11638 VOLK, GALL, RAIBLE, CARROLL
However, even at elevated core temperatures, the
gas rapidly cools to Tt (ambient temperature) due
to the low heat capacity of the gas relative to
the plumbing. Pressure and temperature measurements
at the exit of the cell verify the assumption re-
quired to use equation 5. Furthermore, flow rates
measured by conventional techniques agree with those
determined using equation 5.
Technique of Gas Flow Measurement
Typically, regained-permeability experiments
involved slowly increasing flow. In order to as-
certain the time required to establish steady state
flow, automated flow measurement was an important
consideration in system design. Figure 4 is a
schematic of the auto-ranging flow monitoring
system. A timer was used to operate solenoid
valve (SV'A'). This valve was periodically closed
for some time, t, allowing pressure build-up in
the downstream volume. The volume, previously
referred to as V , includes the combined volume of
valves, pressure t transducers, test cell downstream
of the core outlet, and connecting tubing. This
volume was measured as 90 cm 3 • Normal cycle time was
5 or 10 minutes with SV'A ' closure time of one
minute. However, these times could be selected in
0.1 minute multiples to provide flexibility in
properly scaling pressure build-up, ~P. Also,
two pressure transducers were used wit~ ranges of
0-100 torr and 0-1000 torr. Depending on sample
permeability and P., either the low or high range
was used. 1 matograms for broad MW polydextran standards.
A strip chart recorder displayed the pressure
build-up from which flow rates could be calculated.
The flow system automatically increased downstream
volume, V , as the pressure, ~P , increased to
some pres~t value in order not to exceed recorder
full scale (R f ). This was accomplished by monitor-
ing the transdBcer voltage output. Normally, the
voltage monitor was set at 90 and 95 percent of Rfs '
If the transducer voltage increased to 90 percent
of R ,SV'B ' opened connecting the 160 cm 3 tank,
V , fa the downstream manifold. This increased
tRe total volume to 250 cm 3 • Similarly, if bP t
increased to 95 percent of R ' SV1C 1 opened
connecting an additional 950 f ~m3 tank, V . When
either of these solenoid valves opened, ft remained
open until reset by the operator. An example of
recorder response for a regained-permeability test
is shown in Figure 5. This figure shows a typical
sequence of valve operation and the resultant ~Pt
attenuation due to increased downstream volume.
Nitrogen, with ideal gas properties, was used
for flow measurements. The system has a flow
measurement range of 4 orders of magnitude using
all equipment parameters. Assuming 11 atmospheres
pressure drop (AP ) and mean pressure (Pc) of 6
atmospheres acros~ a core, the system is ca~able .
of measuring .002 to 20 cm 3 /sec. For a tYPlcal Slze
core used in these experiments, this corresponds
to a permeability range of 0.4 to 5000 J-ld. For
unattended operation using the same criteria, the
system would measure approximately 0.002 to 0.25
cm 3 /sec or 0.4 to 60 J-ld for low flow operation.
Permeabilities measured with this system were
effective or apparent gas permeabilities. Klin-
ken berg corrected permeabilities were determined
335
3
by measuring gas permeabilities at 3 mean pressures
and extrapolating to infinite mean pressure. Many
of the permeability values used in the following
discussion will be gas permeabilities at 1000 psig
(6.9 MPa). These values are very close to the
Klinkenberg corrected permeabilities.
MOLECULAR WEIGHT DETERMINATIONS
High pressure liquid chromatography (HPLC)
techniques (19) were used to determine the presence
and molecular weight distribution (MWD) of fractur-
ing fluid polymers passing through the cores. A
liquid chromatographic system, equipped with a
HPLC pump, automatic injection refractive index
detector and three Toyo Soda columns (two-G5000PW,
one-G3000PW) (20), was used to separate molecules
according to size. The method, commonly known as
gel permeation chromatography (GPC), elutes the
largest molecules first with progressively smaller
molecule elution. Dextran standards with a known
molecular weight (MW) were used to characterize
the col umn set. Dextran molecules, however, are
more linear molecules than those of guar and guar
derivatives (21) so that the absolute calibration
with respect to guar polymers is not precise.
However, comparative MW curves and changes in the
molecular size distribution of the broken polymers
were possible using the column set.
Figure 6 shows a composite of the MWD chro-
Each standard curve represents a MW range with the
average MW indicated near the apex of each curve.
The exclusion limit of the column set is approxi-
mately 3 to 5 million. Some of the T-2000 standard,
which has an extremely broad MW range, is excluded
from the column packing pores resulting in a
bimodal curve. In the remaining discussion, refer-
ences to molecular weights of gels are for illustra-
tive comparisons. Actual gel MW is not known.
Unbroken hydroxypropyl guar (HPG) elutes at
the exclusion limit, indicating a MW greater than
5 million as shown in Figure 7. Broken gel,
however, elutes within the separation range of the
column set. Figure 7 also shows the MWD of HPG
fracturing fluid containing breaker and heated to
343°K for various time durations. The composite
chromatogram shows distributions of progressively
smaller molecular size as the duration of the oxi-
dation increases.
The GPC system was useful for detection of
gels in fluid leak-off, as well as, estimating
size of molecules which penetrated through core
samples. Broken gels were also characterized
prior to being used in regained-permeability
experiments.
EXPERIMENTAL PROCEDURES
Gel Preparation
Hydroxypropyl guar (HPG) was prepared in 40
and 80 lb/1000 gal concentrations (4.8 gm/L and
9.6 gm/L). The polymers were hydrated in a
potassium dihydrogen phosphate solution brought to
pH 10 with 10 percent KOH. After hydration, the
solution pH was lowered to between 6 and 6.5.
Typical viscosities measured with a Fann 35
4 A METHOD FOR EVALUATION OF FORMATION DAMAGE DUE TO FRACTURING FLUIDS
Viscometer were approximately 117 cp at 300 rpm
(479 sec l for the 80 lb gel and 35 cp at 300 rpm
(479 sec-I) for the 40 lb gel.
Core Preparation
Core for these experiments were low permeability
sands from the following wells: CIGE-Zl Natural
Buttes Unit, Bitter Creek Field, Section 21, T10S,
R22E, Uintah County, Utah, depth 6499 feet and
from the Multi-Well Experiment #1, Rulison Field,
Piceance Basin, Section 34, T65, R94W, Garland
County, Colorado, depth 7884 and 7955 feet. Cores
from these two wells will be identified as CIGE-21
and MWX-l in the text of this paper. Core plugs
approximately 3.8 cm in diameter and 1.2 to 2.0 cm
in length were dried in a vacuum oven and their
porosities determined by vacuum saturation with 2
percent KN~. They were then placed in the regained-
permeability apparatus where the general procedure
described below was followed.
Regained Permeability Procedures
Gas permeability of the core (Klinkenberg
corrected) was first determined for the dry core.
Then, brine (2 percent KN0 3 ) was pumped through
the core to saturate and determine brine
permeability (Figure 1). This step was followed
by reverse flow with nitrogen (Figure 2) and the
reqained-permeability curve was measured as
illustrated in Figure 5. The differential pressure
across the core was typically 1000 psig (6.9 MPa).
Nitrogen gas flow was allowed to continue until
maximum flow or equilibrium was obtained. This
regained-permeability curve was later used to
estimate core damage. The maximum permeability
obtained with undamaged core will be referred to
as k., or initial permeability. Unbroken gel was
then1pumped across the core to determine fluid
leak-off along the core face. Broken gel and/or
brine could be pumped to determine their effects
on fluid leak-off. Fractions of the fluid passing
through the core were also analyzed for the presence
of broken or unbroken gel using the GPC apparatus.
A second regained-permeability curve was then
measured. This curve was compared with the previous
regained-permeability curve as a measure of core
damage due to gel exposure. The maximum permeability
obtained with the damaged core will be referred to
as kd or damaged permeability.
RESULTS AND DISCUSSION
Permeability Damage
A comparison of effective core permeabilities
to nitrogen at 1000 psig (6.9 MPa) after brine
saturation and after exposure to HPG under pres-
sure is shown in Table 1. At 343°K, the percent
core damage due to exposure to gel appeared to be
independent of initial permeability over a wide
range of low permeability cores (0.58 to 115 ~d).
In addition, the amount of damage was not sig-
nificantly changed when the fluid pressure was
decreased from 2000 psig (13.8 MPa) to 700 psig
(4.8 MPa). The test run at 295°K indicated less
core damage. Most likely the reduced amount of
damage could be attributed to the greater vis-
cosity of the fracturing fluid at room tempe-
rature.
336
SPE 11638
Depth of Gel Invasion
The depth of gel invasion was estimated by
performing regained-permeability measurements
before and after removing a portion of the damaged
core surface. For unbroken gels, most C1GE-Zl
cores returned to 95 percent of their original
permeabil ity (k.) with 0.1 cm or less of the
damaged core sutface removed. For example, CIGE-
21 (6499.7) had 100 percent permeabil i ty res-
toration with 0.02 cm removed. A CIGE-21 (6499.5)
core regained 95 percent of its original per-
meability when the gel coating on the core surface
was scraped off with a knife. No additional
permeabil ity restorati on was measured by removi ng
a small portion of the core surface. This in-
dicates, that within experimental error, the
reduction in gas permeability of this rock for-
mation ;s due to the filter cake on the core
surface.
Visual inspection of the gel buildup on the
core surfaces was made at various steps of the
experimental procedure. After pumping HPG gel
across a core surface for 4 hours with a fluid
loss coeffcient of .0018 ft/min~, the gel coating
was approximately 0.1 cm in thickness (at ambient
pressure} and had a soft, elastic consistency.
After a regained-permeability test was performed,
the gel coating was a thin dehydrated film with a
brittle texture. When humidified nitrogen was
used in the regained-permeability procedure, the
gel coating appeared to be completely dry.
In another test, a mixture of 40 lb (4.8
gm/L) HPG gel and 0.1 percent ammomium persulfate
was prepared. Then the unreacted gel mixture was
pumped across a core to form a gel filter cake.
The HPG gel and breaker in the filter cake were
allowed to react on the core surface for 24 hours
at 343°K. These conditions were used to simulate
breaking conditions of a filter cake on a frac-
tured surface.. After the reacti on ti me of 24
hours, the core was removed. The appearance of
the filter cake was not Significantly different
from a filter cake without breaker. A portion of
the gel was removed and dissolved in solvent for
GPC. A significant amount of solid matter had to
be filtered prior to GPC analysis. Analysis of
the filtered mixture indicated broken polymer.
Under these conditions, it appeared that there was
insufficient breaker present in the concentrated
gel filter cake to complete gel reaction. Under
the same conditions the nonconcentrated HPG solution
has a viscosity less than 3 cp Cat 479 sec- 1 ).
This would indicate the possibility of fracture
damage due to incomplete gel breakup.
Gel Passage Through the Core
As discussed in the previous section, it was
determined that unbroken gel did not pass through
the low permeability cores. However. HPG gel
broken with ammonium persulfate did penetrate
through the core. At room temperature broken HPG
caused a 30 percent reduction in regained-perme-
ability (37.5 to 26.2 ~d) for a C1GE-21 (6499.2)
core. Broken guar which passed through the core
had the same MWD as the original broken HPG gel.
SPE 11638 VOlK, GAll, RAIBLE, CARROLL
The permeability reduction was most likely due to
the insoluble material produced on breaking which
formed a filter cake. This residue would not be
evident in a GPC chromatogram. Removing 0.14 cm
from the core surface restored the permeability to
36.6 lJd.
Broken HPG gel was found to pass through both
a core and a core with filter cake buildup in
te s t s run a t 343 0 K• Us i ng C1GE- 21 ( 6499. 7) ,
broken HPG gel also penetrated the core with
approximately the same MWD as the original solution
(Figure 8). If a gel coating of unbroken HPG
was first formed on the surface of the core,
broken gel passed through the core with a lower
MWD than that in the solution (Figure 9). There-
fore, the filter cake has effectively a much
smaller pore structure than does the core. The
core essentially passes molecules of molecular
weight of 10 5 -10 6 without significant attenuation.
The filter cake, however, begins retaining molecules
having molecular weights greater than 10 4 •
Time Required to Restore Permeability
The time required to regain stable permea-
bility should depend on the type of fluid used to
saturate the core, temperature, original per-
meability of the core, and the pressure of the
clean-up gas. Table 2 lists the time needed to
obtain 80 percent of the final regained-permea-
bility, t 8' using N2 at 1000 psig (6.9 MPa). The
value of ~ percent was an arbitrary choice to
facilitate comparisons.
As expected, the cores cleaned up consi-
derably faster at 343°K, partially due to the
lower viscosity of water (brine or filtrate) at
elevated temperatures. Exposure to HPG increased
the regained-permeability time.
A correlation between the ratio of clean-up
time after exposure to gel, teo (gel), and clean-
up time after exposure to brine, tso (brine), and
the initial permeability (k.) can be seen in
Figure 10 for tests perform~d with a confining
stress of 3000 psig (20.7 MPa). Until more work
can be accomplished, the exact nature of all the
factors influencing the relative rate of clean-up
is not known. Some possible factors, however,
include greater polymer deposition on the surfaces
of the more permeable cores since filtrate volume
is considerably greater for these cores.
In. addition, the cores with higher permeability
may have greater depth of invasion of the frac-
turing fluid polymer causing them to clean-up more
slowly. The final gas regained-permeability may
not be a strong function of filter cake thickness
or depth of invasion, but it may have some in-
fluence on the relative clean-up time.
Fluid Loss
In general, brine flow through a core or a
core with a gel build-up was linear with time.
Degraded HPG (fluid viscosity of 3 cp or less at
479 sec-i) also passed through a core and filter
cake with a flow rate that was linear with time as
shown in Figure 11. Although degraded HPG solu-
tion possessed some solids, apparently the rate of
deposition on the existing filter cake did not
significantly alter the cake permeability or
thickness within the experimental time limits.
337
5
Figure 12 illustrates typical fluid loss
curves observed for wall-building gels on cores.
The apparent negative spurt loss is due to the
presence of the core which provided additional
resistance to fluid flow. As expected, the slope
of the two fluid loss curves approach the origin
at zero slope, typical of Darcy flow. The per-
meability difference between the two core was
primarily responsible for the different slopes.
Fluid loss coefficients were calculated to be 1.3
X 10- 3 ft/m;n~ for C1GE-21 (6499.7) and 0.3 X 10- 3
ft/mi for MWX-l (7884C). In general, no dynamic
filtration effects were observed. This is due to
the low shear rate of the fluid as it passes over
the core and the rather large flow slot (0.5 cm)
relative to the filter cake thickness (0.1 cm or
less),
CONCLUSIONS
(1) An apparatus is presented for continuously
monitoring changing permeability of a
core over a wide range for extended periods
of time. This is accomplished automat;
cally while maintaining the core at in-situ
conditions. The principle behind this
technique can be extended to lower or
higher flow rates if desired.
(2) Depth of invasion of unbroken HPG is very
small, most likely less than 0.02 cm into
rock with permeabilities less than 120 ~d
(gas) and 600 psig per cm pressure gradient
ac ros s the core.
(3) Regardless of the rock permeability (0.6
to 115 ~d), the permanent damage remains
approximately constant at a given tempera-
ture (17-20 percent at 343°K).
(4) Degraded HPG passes through tight sand-
stone without significantly altering
even the high molecular weight fractions
(MW 0 f 10 5 - 10 6 ) •
(5} Only degraded HPG molecules with molecular
weights of 10 4 or less pass through un-
hindered if a gel filter cake is allowed
to form on the core surface.
(6) For core of the permeabilities used in
this study, with HPG, there appears to be
a correlation between the relative rate
of clean-up and the formation permeability,
(7) Humidification of the gas used in regained-
permeability tests does not seem to have
much effect on the rate of ultimate
permeability attained.
6 A METHOD FOR EVALUATION OF FORMATION DAMAGE DUE TO FRACTURING FLUIDS
NOMENCLATURE
A Core plug area perpendicular to flow, cm 2
ka Apparent gas permeability, wd
Apparent gas permeability at irreducible
water saturation after gel damage, wd
Apparent gas permeability at irreducible
k.
1
water saturation before gel damaqe, wd
L Core sample length measured parallel to
fl ow, cm
Arithmetic mean pressure in core,
~ (Pi + Pt ), atm
Pressure drop across core, Pi - Pt , atm
Absolute pressure at core inlet, atm
Atmospheric pressure, atm
Pressure buildup downstream of core in
volume (V t ), Pt - Po' atm
Absolute pressure in volume Vt ' atm
Volumetric flow rate through core at
Pc' cm 3 /sec
t Time, sec
Core temperature, OK
Ambient temperature of volume Vt ' OK
Time required for core permeability to
increase to 80 percent of its final
value after saturation
Vi seas ity, cp
Volume of an ideal gas at pressure P and
T cm 3 c presented at the SPE-AIME 50th Annual
c'
Vt Measurement volume downstream of core, cm 3
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SPE 11638
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11. Pence, S.A., "Evaluating Formation Damage in
Low Permeability Sandstone", Paper SPE 5638
Fall Meeting, Dallas, Tx, Sept. 28-0ct. 1
1975. '
12. Ho1ditch, S.A., "Factors Affecting Water
Blocking and Gas Flow from Hydrau11ica1ly
Fractured Gas Wells," J. Pet. Tech.,
Dec. 1979, pp. 1515-1534.
13. Black, H.N., Ripley, H.E., Beecroft, W.H.,
and Pamplin, L.O.," Drilling and Fracturing
Improvements for Low Permeability Gas Wells
in Western Canada," J. Pet. Tech., Jan. 1981.
pp 26-32.
14. White, J.L., and Means, J. 0., "Polysac-
charide Derivatives Provide High Viscosity
and Low Friction at Low Temperatures ," J.
Pet. Tec h. , ., 1975. pp 1067 - 1073 •
15. McDaniel, R.R., Houx, M.R., and Barringer,
O.K., "A New Genertion of Solid Free Frac-
turing Fluids," Paper SPE 5641 presented at
the 50th Annual Fall SPE Meeting, Dallas,
TX., Sept. 28-0ct. 1,1975.
SPE 11638 VOLK, GALL, RAIBLE, CARROLL 7

16. Free, D.L., Fredrick, A.F., and Thompson, 19. Yau, W.W., Kirkland, J.Jo, and Bly, D.O.,
J.E., "Fracturing with a High Viscosity Modern Size Exclusion Liquid Chromatography,
Crosslinked-Gel Continuous Fracturing John Wiley and Sons, Inc., 1979.
Techni que, Paper 5640 presented at the
II

50th Annual Fall SPE Meeting, Dallas,
TX., Sept 28-0ct. 1, 1975.
17. Jones, S.C., "A Rapid Accurate Unsteady State
Kl i nkenberg Permeabi 1i ty ," Soc. Pet. Eng.
J., (Oct. 1972), pp 383-397.
18. Freeman, D.L., and Bush, D.C., "Low Per-
meability Laboratory Measurements by
Nonsteady State and Conventional Methods,"
Paper SPE 10075 presented at the SPE 56th
Annual Fall Technical Conference and
Exhibition, San Antonio, TX., Oct. 5-7, 1981.
20. Hashimoto, T., Sasaki, H., Aiura, M., and
Kato, T., "High Speed Aqueous Gel Permeation
Chromatography," J. Polym. Sci., Polymer
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1789-1800.
21. Barth, Ho G., and Smith, D.A., "High Per-
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of Guar Gum," J. Chromatogro, 206, (1981),
pp 410-415.

Tabl e 1. Regained-Permeability of Cores and Estimate of Core Damage

Core no Init; a1 After gel Core Temp. HPG gel
perm darnage damage concentration
Depth
ft *k i( ~jd) *k d (j,Jd) percent OK 1b/ 1OOOga 1 (gm/L)

Confining stress 3000 psig (20.7 MPa) and Fluid Pressure 2000 psig (13.8 MPa)
CIGE-21
6499.1 28.8 26.2 8 295 80 (9.6)
CIGE-21
6499.5 35.5 29.5 19 343 40 (4.8)
MWX-1
7955 0.58 0.48 18 343 40 (4.8)
Confining stress 1700 ps i 9 (11.7 MPa) and Fluid Pressure 700 psig (4.8 MPa)
MWX-l
7884A 5.3 4.4 17 343 40 (4.8)
MWX-l
7884C 4.5 3.6 20 343 40 (4.8)
CIGE-21
6499.7 115 91.6 20 343 SO (9.6)
*Perrneability measured at 1000 psig (6.9 r~Pa) nitrogen pressure

Table 2. Core Cleanup Time Under Various Conditions

Core no. Fluid N2 gas *tso Final Temp. Core
type humi difi ed perm. length
minutes ~d OK em

CIGE-21 brine no 280 2S.8 295 1.46

6499.1 80 lb gel no 477 26.2 295

CIGE-21 brine no 70 35.5 343 2.04

6499.5 40 1b gel no 140 29.1 343

MWX-l brine no 400 0.58 343 1.25

7955 40 lb gel no 400 0.48 343

MWX-l brine no 5S0 5.2 299 1.41

7884A brine yes 600 4.3 299
brine no 210 5.1 343
brine yes 210 5.3 343
40 lb gel yes 240 4.4 343

CIGE-21 brine yes 13 115 343 1. 35

6499.7 80 1b gel yes 35 91.6 343
*Time required to cleanup cores to SO percent of final core permeability (ki or kd)

339
 rHydrostatic stress

I
~"""","""'.,..,J..__/Rubber sleeve

E,ces~
fluid
Bock pressure
regulator
Displacement
Pressure tank

Pressure ---1 fluid

transducer Regulated
Hydrostatic nitrogen
pressure (Pi) I-
pressure I
High pressure
pump
~Pc : "- Pressure
transducer

-----0
test cell

[1n.CUJ
Li quid fraction
collector or Fractur ing fluid
B eCO'de,
Transducer
readout

Fig. 3-Simplified gas flow measurement system.

Electronic balance Core
Rubber sleeve
0-1000 mm
pressure transducer
Fig. 1-Schematic 0 f fracturing fluid simulator.
I
I

~::----
J
I

H ig h pressure
____-1--11, 1 <0,d,,1
Re

Hydrostatic pressure test cell _J 1

1
1
Pressure I
transduce~ Gas
O-IOOmm I
pressure transducer I
measurement I
system I
I
I
I
--'

Water
Nitrogen
humidifier

Fig. 2-Schemalic of regained-permeability

. gas flow. Atmospheric
pressure

Fig. 4-Schem a!'Ie of autoranging flow mOniloring system.

 18

14_
16

I
Il
>

>
+
fD

><f.
12
No oxidant

~IO Solvent
w
~ en peak
w z
o 24 Hours
~
8 a..
i= en
w
0::
ttl 0::
6 > o
+ f-
o
l ><f. W
r-

:i 1
w
o

~ Elution volume- 53 ml
I I I I 4
0 20 40 60 80 100 - Molecular size
RECORDER SCALE Fig. 7-Composile chromatogram showing molecular weight distribution change with time as H PG gel reacts
with oxidant breaker.
Fig. 5-Example of recorder response for regained·permeability test.

Average molecular weight

of dextran standa rds Exc lusion
I im it

w
en Sol vent
z Solvent w peak
o peak en
Cl.
en z
o
W a..
0:: en
w
0:: 0::
o
r- 0::
o o Broken HPG
w f-
r- o diluted by
w W 1/2 Broken H PG
o r- t h roug h core
w
o

25ml Elution volume - 53ml 25ml Elution volume ~ 53 ml

4-- Molecular size - - Molecular size
Fig. a-Molecular weight distribution of broken HPG gel passed through core compared with MW of the orginial
Fig. 6-Composlte gel permeation chromatogram for Dextran calibration standards.
broken HPG gel.
 30r-------------------------------~

Exclusion
limit
a:::
Solvent
I.iJ
(1) pea k
z
o IJ)

E
a..
(1) ~ 20
w Orig ina I broken
HPG\
01
a:::
r:
a::: I
o ~
I- W
u ~
W
I- 0
W
I.iJ I-
o Fluid passed «
...J
through gel ~ ::J
bu i Idup and :::E
::> 10
i:.··qre <.>
,~;~~ <.>
«
25 ml Elution volume ----IIi"' 53ml
- - Molecular size

Fig. 9-Molecular weight distribution of broken HPG gel passed through core and gel filter cake compared with
MW of the original broken HPG gel.

o 10 20 30 40
TIME, minutes
tsO(GEL) / tSO( BR I NE)
Fig. 11-Broken gel filtrate passage through a core with previously
deposited filter cake.
o

6.-------------------------------------------
0
G')
1:>
(J)

II
fTt 5
::0 N
3: 0
fTt
1:>
CD
IJ)
r E
-i ~ 4
-< (,>J
0
01

~
J:
<.9
W
1::
Q. 3: 3
.f:>
0 o
W
I-
«
...J
::J

~ 2
~~--------------------------~----------~ u
u
«
Fig. 10-Relalive cleanup lime vs. gas regained-permeability at 1.000
pSlg.

o~------~--------~-------L------~------~
2 4 6 8 10
TIME, minutes 1/2
Fig. 12-Typical fluid·loss curves for unbroken HPG gel.

s PE'" JJ1113 'X