Flow-Rate Behavior and Imbibition
in Shale
Dongmei Wang, SPE, Raymond Butler, Hong Liu, and Salowah Ahmed, University of North Dakota
Summary
As part of our investigations of a new chemical imbibition idea
(using surfactant or brine formulations) to stimulate oil recovery
from shale, we are studying oil flow through and, especially, brine
intake into shale to displace oil. Our first studies in this area focused
on an outcrop shale, specifically the Odanah member of Pierre
shale in North Dakota, USA. We studied porosity, permeability
to oil, permeability to water, and spontaneous brine intake for the
Pierre shale. We found that porosities for Pierre shale cores were
relatively high—from 25 to 35%. Porosities for our measurements
of Bakken cores averaged less than 3%. Bakken oil imbibed into
dry Pierre shale cores (up to 5 mm in thickness) to the same extent
as could be achieved by forced injection of oil (i.e., achieving the
same oil saturations for both processes). Permeability to a clean
mineral oil (Soltrol 130™) was higher than for Bakken oil—appar-
ently because of deposition of wax/asphaltenes/particulates on the
Pierre core faces when injecting Bakken oil. Permeability to oil for
Pierre shale cores (with no water present) ranged from 3.32×10−5
to 2.19×10−4 md when injecting Bakken oil and from 4.85×10−4 to
2.34×10−3 md when injecting Soltrol 130. Permeability to Bakken
oil for a Bakken core (with no water present) averaged 4.84×10−4
md. In Pierre shale and Bakken cores with thicknesses ranging
from 0.65 to 5 mm, permeabilities were basically independent of
flow rate, in agreement with expectations from the Darcy equa-
tion. Saline brine spontaneously entered into oil-saturated Pierre
cores, yielding recovery values up to 41% of original oil in place
(OOIP). During exposure to brine, our results indicated an increase
in permeability—presumably by mineral dissolution during forced
brine injection and by cracking (possibly caused by clay swelling)
during spontaneous brine intake. This result is encouraging for
the application of imbibition to enhance oil recovery from shale.
Before these studies, we feared that exposure to brine might reduce
shale permeability because of clay swelling. The laboratory results
will help during a current study of surfactant and brine imbibition
in the Bakken formation.
Introduction
Shale is an important source of oil and gas in North America. Most
shale reservoirs have a low porosity and ultralow permeability
with natural fractures. Shale formations have long been considered
important source rocks, capable of producing oil at economic rates
when completed by hydraulically fractured horizontal wells. As part
of our investigations of a new chemical imbibition idea (using sur-
factant or brine formulations to stimulate oil recovery from shale),
we are studying oil flow through and, especially, brine intake into
shale to displace oil. The ultimate objective of our studies is to deter-
mine whether surfactant or brine formulations can imbibe into, and
displace oil from, oil shales. Our primary target is the Bakken shale
in North Dakota. However, because of limited availability of Bakken
core samples, our first studies focused on the Pierre shale (specifi-
cally from an outcrop in northern North Dakota). The Pierre shale
has been stated to contain 70–80% clay, of which approximately
80% is mixed-layer smectite/illite (Neuzil 1993). Our first steps
involve characterizing porosity and permeability of shale samples.
Copyright © 2011 Society of Petroleum Engineers
This paper (SPE 138521) was accepted for presentation at the SPE Eastern Regional
Meeting, Morgantown, West Virginia, USA, 12–14 October 2010 and revised for publication.
Original manuscript received for review 25 October 2010. Revised manuscript received for
review 17 February 2011. Paper peer approved 14 March 2011.
August 2011 SPE Reservoir Evaluation & Engineering
Examination of the literature reveals numerous procedures have
been used to measure porosity and permeability for shale. Reyes
and Osisanya (2002) measured permeability to deionized water and
nitrogen for various shale rocks, using an effective-stress concept.
They applied laboratory results to develop an empirical correlation
between permeability and porosity for various shales. Chenevert
and Sharma (1993) showed a relationship between permeability
and effective stress using experimental data. Permeability values
measured under effective stresses up to 8,000 psi show the Welling-
ton shale to have values as low as 0.30×10−6 md. Osisanya (1995)
estimated shale permeability from a modeling equation using
swelling data from shale contacted with various aqueous fluids. His
study measured water vapor pressure. Three experiments measured
permeability to liquid, with deionized water used as a drive and
compression fluid. Shale permeabilities to water may vary because
of effects of brine hardness and shale clay content. Gas permeabili-
ties have been estimated from pressures measured during degassing
of helium-saturated core plugs, core chips, or drill cuttings. For 68
test results using this method, permeabilities of a Devonian shale
with natural fractures were measured in the nanodarcy range (2 to
2,000×10−9 darcies) (Luffel et al. 1993). Previous measurements of
the permeability range from 0 to 20 md for the Middle member of
the Bakken formation, but they average only 0.04 md, based on a
correlation between porosity and permeability (Pitman et al. 2001).
Well tests from the Bakken formation near Billings, Montana,
USA, indicate a permeability range from 0.05 to 2.3 md (Cramer
1986). Sanyal et al. (1972) developed an instrument to measure
liquid permeabilities of very tight Precambrian rocks (as low as
1.16×10−3 md), which involved a pump based on thermal expansion
of liquid, and they used pressure decline to calculate permeability.
Luo et al. (1996) introduced an approach linking the downstream
response directly to the rock permeability and compressibility for
oscillating-pressure measurements in ultralow-permeability media
(i.e., shale, intact igneous rocks, salt, low-porosity carbonates,
and anhydrite) with time-varying properties. On the basis of this
method, the permeability inverted using a direct visual curve-match
technique. This method was suggested to be capable of measuring
permeability as low as 10−8 to 10−10 md (Luo et al. 1996).
For simplicity during our first studies, we determined porosi-
ties and permeabilities without the application of high overburden
stresses. These methods will be described first in this paper. (Our
future research will use overburden stresses. For now, our interest
is primarily in scoping whether brine and surfactant imbibition is
feasible as an oil-displacement mechanism in shale.) Permeabili-
ties will be determined over a range of flow rates and throughput
values using both a refined oil and Bakken crude. Next, we test the
ability of the cores (filled with oil) to spontaneously pull in brine
(a process that we will loosely call “imbibition”). These tests will
also involve a refined oil and Bakken crude.
Method
Fig. 1 provides an illustration of the permeability-measuring
system. In this method, an ISCO Model DX-100™ syringe pump
was used. This pump (which has a built-in pressure transducer)
provides a wide range flow rates (from 0.001 to 60 cm3/min) for
any pressure up to 10,000 psi (690 bar or 70 MPa). The system
shown in Fig. 1 provides a method to evacuate and saturate the
core slices before permeability measurement.
In this system, Valves A and B are two-way valves to control
flow of distilled water to/from the pump. Valve C is a two-way
bypass valve that is used during evacuation and saturation of the
505
 Valve B
Gauge Valve A

Valve D Valve E
Core holder

Shale slice

Valve C

Valve F
Transfer ISCO Pump
cylinder
Oil Outlet
DI water inlet
Vacuum

Fig. 1—System for permeability measurement.

core slice. Valves D, E, and F are three-way valves that control fluid accurately with a Carrera precision digital caliper, which read to
input/outflow for the transfer cylinder. The core holder accom- 0.01 mm. Table 1 list properties of the cores used for the first
modates cylindrical core slices that are 25–26 mm in diameter porosity measurements.
and 0–10 mm in thickness, at pressures up to 3,000 psi (207 bar We routinely measured the length (thickness) at 5 to 10 loca-
or 20.7 MPa). tions for each core and reported the average in Table 1. However,
all measurements were never more than ±0.01 mm of the average
Core Samples, Oils, and Brine. The shale rock plugs are from value—demonstrating the flatness of the surfaces.
the Odanah member of the Pierre shale and the Middle member of We used two oils: (1) a mineral oil, called Soltrol 130™, and
the Bakken formation (Wells 16433). The Pierre shale is light grey (2) Bakken formation crude oil. Soltrol 130 is an isoparaffin that
shale and mostly silica, but has some carbonate (oyster fossils). had a viscosity of 1.6 mPa·s and a density of 0.76 g/cm3 at 23°C.
As an outcrop, it is siliceous, noncalcareous, and has hard, slate- The Bakken crude was from Well BL-Davidson 2-11H and was
like, iron-stained joints, with a yellow bentonite near its base. It generously provided by Hess Oil Corporation. It has a density of
shows ferruginous concretions and forms conspicuous cliffs. Our 0.78 g/cm3 and a viscosity of 1.8 mPa·s.
core plugs were typically 25–26 mm in diameter and 1–5 mm
in thickness. The dimensions of each core were measured very Porosity- and Permeability-Testing Procedure. The following
steps were used during determination of porosity and permeability:
• Step 1: Filter the oil through Whatman 4™ filter paper.
• Step 2: Measure the oil viscosity using a Brookfield viscom-
TABLE 1—DIMENSIONS AND POROSITY
OF PIERRE CORES
eter with UL-Adapter.
• Step 3: Place the shale slice into the core holder.
Length, Porosity, volume • Step 4: Pump distilled water into the transfer vessel, then
Core mm Diameter, mm fraction pump the test liquid (crude oil or Soltrol 130 oil) into the transfer
1 1.17 24.63 0.336 cylinder. For the brine experiments, add another transfer cylinder
(that contains brine) after the oil transfer cylinder. In this way, dis-
2 0.92 25.30 0.278 tilled water from the ISCO pump drives oil from the first transfer
3 0.99 24.83 0.349 cylinder, to displace brine (in the second transfer cylinder) into the
4 1.04 25.43 0.268 core and core holder.
5 0.86 24.98 0.336 • Step 5: Apply vacuum to the shale material for 1 hour to
remove any gas from the lines and core.
6 0.91 25.39 0.295
• Step 6: Pump the test liquid into the core, and maintain the
7 2.33 25.35 0.339 vacuum for an additional 1 hour.
8 1.84 26.20 0.350 • Step 7: Increase the injection rate until a constant pressure is
9 1.96 26.28 0.303 reached. Otherwise, maintain constant rate and observe pressure
10 2.12 25.19 0.353 changes.
• Step 8: After the first liquid drop is produced, observe and
11 1.79 26.13 0.349 record the pressure changes. Look for pressure stability on the
12 2.95 26.52 0.348 order of 1 hour.
13 2.08 26.46 0.349 In all experiments, the temperature was ambient (approximately
14 3.00 26.31 0.355 23°C).
15 4.03 26.64 0.275
Data Analysis and Discussion
16 4.06 26.38 0.267 Porosity Measurements. Porosity of the shale cores was deter-
17 4.35 26.51 0.263 mined by weight differences before and after saturation with the
18 4.55 26.47 0.247 oil. Weight measurements were made using a Mettler Toledo
19 4.87 26.24 0.345 Model XP504™ analytical balance that reads weights to 0.0001 g.
Eq. 1 provides the method for porosity determination:
20 4.98 25.90 0.345
21 4.92 26.40 0.324 ␾ = (Wo – W1)/(␳o Vshale), . . . . . . . . . . . . . . . . . . . . . . . . . . . (1)

506 August 2011 SPE Reservoir Evaluation & Engineering

 50

1mm : Method A, Bakken oil

2mm : Method A, Bakken oil
45
4mm : Method B, Bakken oil
5mm : Method A, Sotrol 130
40
Porosity, %

35

30

25

20
1 2 3 4 5 6
Sample No.

Fig. 2—Porosity results for Pierre shale samples.

where ␾ is the rock porosity (dimensionless), W1 is the dry weight
of the shale rock (g), Wo is the weight after oil saturation (g), ␳o is
the oil density (g/cm3), and Vshale is the volume of the shale rock
(cm3). Two methods were used to saturate the cores. In Method
A, a vacuum was applied to the core; then oil was pumped into
the core using the apparatus described in Fig. 1. In Method B, the
core was simply placed into a beaker and oil imbibed spontane-
ously into the core during a 24-hour period. In all, 21 cores were
examined (see Fig. 2): six 1-mm cores, six 2-mm cores, six 4-mm
cores, and three 5-mm cores. The far-right column of Table 1 lists
porosity values for individual cores. In our experiments, no over-
burden pressure was applied. Of course, application of significant
overburden pressure can decrease porosity and permeability. In
future experiments, an overburden pressure may be applied. Our
interest at the present time is ultimately focused on establishing
the degree of imbibition that can occur.
A set of example calculations can provide the reader a feel for
the error associated with our porosity measurements. The shortest,
smallest-volume core that we used was 0.65 mm long (and 25.00 mm
in diameter). The error associated with measurement of a given
core dimension could be ±0.01 mm. Thus, this core had a total
volume of 319 mm3 ±5 mm3. After saturation with Soltrol 130
oil, this core weighed 0.0662 g (±0.0001 g) more than before
saturation. Soltrol 130 density was 0.76 ±0.01 g/cm3. So the pore
volume was 0.0871 cm3 or 87.1 mm3 ±2 mm3. Given this informa-
tion, the porosity was 0.273 ±0.011. Longer cores would have a
lower percentage error associated with the length measurements,
which, in turn, would reduce errors for the porosity measurements.
We note that the porosities measured for our shortest cores were
in the same vicinity as for our longer cores.
Throughout all the cores, our porosity measurements varied
from 25 to 35%. The average porosity for all 21 samples was
31.8%. Close examination of Fig. 2 reveals that porosity did not
correlate with the method of core saturation (Methods A or B), with
core thickness (from 1–5 mm), or with the type of oil used (Bak-
ken crude or Soltrol 130). Considering the accuracy of our weight
measurements, the typical error bar on a porosity measurement
was approximately 1 porosity percentage point. Thus, the porosity
variations seen in Fig. 2 (covering 10 porosity percentage points)
must be caused by natural variations from sample to sample. It
is interesting that the cores could be saturated as effectively by
spontaneous oil imbibition as by forced oil injection. It is also
interesting that the porosity was so high for our very-low-perme-
ability cores. Of course, we recognize that porosities may be less if
a high overburden pressure is applied to the core or if clay swelling
(because of contact with water) occurs (Osisanya 1995).
Earlier literature (Cheatham and Nahm 1990) reported that the
Pierre shale porosity was approximately 23% for a 100%-water-
saturated core. This value is consistent with our measurements.
Clay swelling could potentially reduce porosity.
Heat-flow research of Gosnold (1990) revealed that thermal
conductivities are different for the different members of the Pierre
Shale. The upper members of the Pierre shale show a higher
thermal conductivity than the lower members. On the basis of
this study, we suspect that our shale samples (which have high
porosities) originate from locations that have a higher thermal
conductivity.
Another study (Neuzil 1993) examined the deformation charac-
teristics of Pierre shales with low fluid pressure in South Dakota.
With this study, the porosity exhibited high porosities (30 to 40%)
for effective stresses from 0 to 35 MPa. This report is consistent
with our experimental results that were performed with low flow
rates at low liquid pressures.
We also used our method to measure porosities of Bakken
cores. As shown in Table 2, for cores from the middle member of
the Bakken formation, porosity averaged 2.87% for core samples
with 2-mm thickness. This result is consistent with porosities rang-
ing from 2–6%, reported from well logs in the Bakken formation
(https://www.dmr.nd.gov/oilgas/).
Measurements of Permeability to Oil. Assuming the flow is lin-
ear, permeability for fluid flow through shale can be obtained by
Darcy’s flow equation. Tables 3 and 4 provide Pierre shale perme-
ability measurements as a function of flow rate using Soltrol 130
oil and Bakken oil, respectively. Table 5 shows results for Bakken
oil in core from the middle member of the Bakken formation. The
apparatus shown in Fig. 1 was used to measure permeability.
A core disk (roughly 25 mm in diameter) was placed inside the
steel core holder. Flat O-rings were placed upstream and down-
stream of the core, and the top part of the core holder was screwed

August 2011 SPE Reservoir Evaluation & Engineering 507

 TABLE 2—DIMENSIONS AND POROSITY the section area of the core plug when employing Darcy’s flow
OF BAKKEN CORES equation to obtain the permeability for fluid flow through shale.)
No epoxy was used to seal the lateral edge of the core. Thus, it is
Length, Porosity, volume possible for fluid to travel from the core inlet (at approximately
Core mm Diameter, mm fraction 6–10 mm from the outside edge of the core) to the outside edge of
1 2.95 24.54 0.050 the core and then back to the core outlet (at a point approximately
6–10 mm from the outside edge of the core). However, this flow
2 2.17 24.85 0.010
path requires the fluid to travel through approximately 12–20 mm
3 2.34 24.98 0.015 of rock, whereas 5 mm (or less) of core must be traversed for fluid
4 2.27 24.8 0.016 going straight through the core. Consequently, the amount of fluid
5 2.11 24.84 0.012 that bypasses our core is negligible.
6 2.40 24.84 0.045 For each reading in Tables 3 through 5, a constant flow rate was
applied, and the pressure was observed as a stabilized condition was
7 2.26 24.94 0.020 achieved over many hours. The dimensionless pressure-transient
8 2.44 24.79 0.030 time (Matthews and Russell 1967) for our conditions was approxi-
9 2.72 24.81 0.038 mately 2 seconds in a 5-mm-long, 0.5×10−3-md core (assuming a
10 2.16 25.18 0.019 viscosity of 2 cp, porosity of 0.3, and system compressibility of
5×10−6 psi−1). The total liquid storage in our reservoir (upstream
11 2.55 24.83 0.055
of the core) was approximately 260 cm3. Given oil compressibility
12 2.28 24.90 0.022 of 10×10−6 psi−1, the maximum calculated time to achieve stabili-
13 2.21 24.75 0.017 zation was 10.6 hours (to achieve 41 psi) at our lowest rate (0.01
14 2.06 24.81 0.012 cm3/hr), and was 15 minutes (to achieve 112 psi) at our highest rate
15 2.35 24.91 0.046 (1.2 cm3/hr). For the experiments in Tables 3 through 5, the system
was not depressurized between rates, so the actual stabilization
16 2.38 24.89 0.054
time was less than the calculated maximum values.
Fig. 3 and Tables 3 through 5 reflect the variation of perme-
into place—squeezing the O-rings onto the core and providing a abilities seen during our studies. For a given core with Soltrol oil
seal to force the injected fluid to flow through the core. These (in Table 3), the results were fairly insensitive to flow rate—as
O-rings had an outside diameter of 26 mm and inside diameters expected from the Darcy equation. The average permeability to
of 15.87 to 19.17 mm. (These diameters were used to calculate Soltrol 130 oil was 4.85×10−4 md in a 4.98-mm-long Pierre slice

TABLE 3—PERMEABILITY OF PIERRE SHALE SAMPLES SATURATED WITH SOLTROL 130 OIL
Flow rate, Pressure drop, Permeability to Average permeability,
3
Sample cm /hr psi oil, md md

D: 25.00 mm
–3
0.3 26.5 2.43 10
Deff: 15.87 mm 0.6 56 2.30 10
–3
2.43 10
–3

L: 0.65 mm 1.2 112 2.30 10

–3

–4
o : 1.6 mPa-s 0.01 41 4.01 10
–4
0.019 66 4.73 10
–4
D: 26.22 mm 0.038 130 4.80 10 –4
4.85 10
Deff: 15.88 mm 0.075 255 4.83 10
–4

L: 4.98 mm 0.150 486 5.07 10

–4

o : 1.6 mPa-s 0.300 869 5.67 10

–4

TABLE 4—PERMEABILITY OF PIERRE SHALE SAMPLES SATURATED WITH BAKKEN OIL

Flow rate, Pressure drop, Permeability to Average permeability,

3
Sample cm /hr psi oil, md md
–5
0.015 323 3.73 10
D: 26.13 mm
–5
0.055 683 6.48 10
Deff: 15.98 mm 0.075 810 7.43 10
–5
1.05 10
–5

L: 2.19 mm 0.105 877 9.61 10

–5

o : 1.8 mPa-s 0.300 945 2.54 10

–4

–5
0.015 184 2.49 10
–5
D: 25.16 mm 0.030 329 2.79 10
Deff: 19.17 mm 0.060 641 2.86 10
–5
3.32 10
–5

L: 1.2 mm 0.085 665 3.91 10

–5

o : 1.8 mPa-s 0.105 702 4.57 10

–5

–4
0.025 232 1.90 10
–4
D: 26.21 mm 0.045 509 1.56 10
Deff: 15.98 mm 0.075 795 1.67 10
–4
2.19 10
–4

L: 4.82 mm 0.105 857 2.16 10

–4

o : 1.8 mPa-s 0.205 990 3.66 10

–4

508 August 2011 SPE Reservoir Evaluation & Engineering

 TABLE 5—PERMEABILITY OF BAKKEN CORE SAMPLES SATURATED WITH BAKKEN OIL
Flow rate, Pressure drop, Permeability to Average permeability,
3
Sample cm /hr psi oil, md md
–4
D: 24.54 mm 0.015 78 2.87 10
Deff: 16.32 mm 0.030 95 4.73 10
–4
–4
4.84 10
L: 4.26 mm 0.075 145 7.74 10
–4

o : 1.8 mPa-s 0.015 392 4.01 10

–4

where Deff is the effective diameter inside of the O-ring.

1.0
5mm, Sotrol Oil
0.9
1mm, Bakken Oil
2mm, Bakken Oil
0.8
5mm, Bakken Oil
Permeability to Oil, microdarcies

0.7 1mm, Bakken Oil

0.6

0.5

0.4

0.3

0.2

0.1

0.0
0.001 0.01 0.1 1
Flux, ft/D

Fig. 3—Permeability to oil vs. flow rate in Pierre shale.

and was 2.34×10−3 md in a 0.65-mm-long Pierre slice. Perme-
ability to Soltrol 130 was determined to be 2×10−4 and 2.33×10−4
md for two other 5-mm-thick Pierre cores. These differences are
probably caused by natural slice-to-slice variations in permeability
of the source rock. It is possible that part of the difference may
be associated with length of the cores. Longer cores may have
Fig. 4—Apparent wax deposit after Bakken-crude-oil flow.
lower-permeability portions that noticeably reduce the composite
permeability of the core. In the thinner core, we may fortuitously
have more-permeable rock. However, in Table 4, note that a 4.82-
mm-long core was more permeable than the two shorter cores. In
Table 5, note that the permeability of the 4.26-mm-long Bakken
core averaged 4.84×10−4 md—two times the average value for the
4.82-mm-long Pierre core in Table 4.
Permeability variations were noticeable when Bakken oil was
used. For a given Pierre core slice with Bakken oil (Table 4), a
greater variation in permeability occurred at different flow rates,
although there was no definitive trend with changing flow rate.
Also, note that the permeability to Bakken oil was generally lower
than that to Soltrol oil. We suspect that differences in wax, asphal-
tene, and particulate content of the two oils may be responsible
for these observations. Fig. 3 shows additional data, comparing the
behavior with Soltrol in a 5-mm slice (from Table 3) with that for
Bakken oil in 1-, 2-, and 5-mm slices.
For permeability measurements with Bakken oil in Bakken
core, the low value was 2.87×10−4 md and the high value was
7.74×10−4 md. Again, permeability did not appear to depend on
flow rate (Table 5).
Fig. 4 shows a basis for our suspicion that wax/asphaltene/par-
ticulate deposition impacts our permeability measurements using
the Bakken oil. After oil saturation, we found a black waxy deposi-
tion on the surface of the slice. This observation helps explain why
permeabilities measured using Bakken oil were generally lower
than those using Soltrol 130. Fig. 5 provides further support for this
concept. This figure plots the apparent permeability to Bakken oil
vs. throughput (i.e., cm3 of oil per cm2 of shale area associated with

August 2011 SPE Reservoir Evaluation & Engineering 509

 1
Permeability to Bakken oil, microdarcys
0.8
0.6
0.4
0.2
0
0 0.1
Throughput, cm3/cm2
Fig. 5—Apparent permeability vs. throughput during Bakken-crude-oil flow.
the inlet core face) for three separate 5-mm cores. In each case, the
apparent permeability decreased with throughput, indicated some
level of plugging. Exactly why wax/asphaltene/particulate should
deposit on the core face is subject to debate. Perhaps it was present
in a finely suspended form in the oil and was accumulated on the
core face by filtration. (In Fig. 5, ft/D in the legend refers to the
flux or superficial fluid velocity during fluid injection—i.e., ft3 of
fluid per ft2 of rock area per day.)
Interestingly, we found that exposure to very high pressure gra-
dients could also temporarily reduce permeability. For the 0.65-cm
core in Table 3, after injecting at 1.2 cm3/hr, we increased the rate
to 2.4 cm3/hr. At this rate, the permeability dropped continuously,
to as low as 1.52×10−4 md, without any sign of stabilization. Upon
reducing the rate to 1.2 cm3/hr, permeability stabilized at 1.03×10−3
md. It appears that when a very high pressure gradient is applied
to the core, the shale was compressed into a much less permeable
state. When the pressure gradient was reduced, the core regained
most of its original permeability over time.
Permeability to Water vs. Oil. For the 4.85×10−4-md core in Table
3, we injected brine after injecting the Soltrol 130 oil. This brine
contained 271 g/L total dissolved solids (TDS), and was represen-
tative of Bakken formation water. The specific composition of the
brine was 218.8 g/L NaCl, 10.85 g/L KCl, 36.60 g/L CaCl2, and
4.7 g/L MgCl2. During injection at 0.03 cm3/hour (0.00445 ft/D),
permeability to water stabilized at 7.37×10−4 md—almost 50%
greater than the previous permeability to oil. We then injected Sol-
trol oil again, and observed a second permeability to oil of 9.8×10−3
md—almost a 20-fold increase from the original permeability to
oil, even though the core presumably had connate-water saturation
(Swr). Apparently, exposure to the brine somehow increased perme-
ability, perhaps by mineral dissolution or by inducing very small
cracks. Upon removing the core from the core holder no cracks
were visible, and the core dimensions were exactly the same as
for the original dry core.
Measurements of Brine Intake. In this section, we examine
the ability of brine to be spontaneously drawn into oil-saturated
Pierre cores. Brine imbibition is central to our ultimate hope that
that this process may be a viable means to improve oil recovery
from Bakken oil reservoirs. Note that our Pierre cores were from
a dry outcrop—suggesting that they initially had no significant
oil or water saturation (i.e., they were “air saturated”). As noted
in our procedures earlier, oil was introduced into the cores either
(1) by pulling a vacuum on a dry core, followed by oil injection,
or (2) allowing oil to saturate simply by placing a dry core into
510
5-mm thick core slices
0.118 ft/D
0.024 ft/D
0.012 ft/D
0.2 0.3
a beaker of oil (Method B in the Porosity Measurements subsec-
tion). During oil saturation of a dry core, presumably, the rock
surfaces would prefer to be wetted by oil than by air (Tang and
Firoozabadi 2002).
In the following experiments, we examine the ability of brine
to enter oil-saturated cores. For cores that were saturated with oil
but with no prior exposure to brine, the reader might question
whether the brine saturation process that we observed can techni-
cally be called “imbibition.” Some might argue that the wetting
state of the core must be known in advance (specifically, it must
be “water-wet”) before spontaneous water intake can be labeled
“imbibition.” Nevertheless, we will use the term “imbibition” to
describe spontaneous brine intake by the core.
The oil-saturated core from the preceding section was then
suspended below a Mettler-Toledo XP504 analytical balance and
immersed in a 100-cm3 beaker of the 27.1% TDS Bakken brine
already mentioned. The balance was zeroed immediately after the
core was suspended and immersed. Subsequently, by monitoring
weight vs. time, we could follow the rate of water imbibition into
the core. Because Soltrol 130 density (␳o) was 0.76 g/cm3 and the
brine density (␳w) was 1.205 g/cm3, we could convert weight gain
(ΔW) during the course of the experiment to the percent OOIP
displaced using Eq. 2:
%OOIP = 100·(ΔW)/[( ␳w /␳o −1)·(OOIP)]. . . . . . . . . . . . . (2)
The solid circles in Fig. 6 plot the oil recovery vs. time for this
brine-intake experiment. After 1 day of immersion, 20.3% OOIP
had been recovered.
A similar experiment was performed with a new 5-mm-thick
core, except this core was saturated only with Soltrol 130 oil (using
Method A). The permeability to oil was 2.37×10−4 md. Brine intake
was examined with this core using the same technique as just
described above. Results from this experiment are shown by the
open diamonds in Fig. 6. For this core, we noted that substantial
cracks developed during the brine-intake process, as can been
seen in Fig. 7. A substantial jump in oil recovery occurred when
these cracks opened. Before these studies, we feared that exposure
to brine might reduce shale permeability because of clay swell-
ing. In contrast, during exposure to brine, our results indicated
an increase in permeability—presumably by mineral dissolution
during forced brine injection and by cracking (possibly caused
by clay swelling) during spontaneous brine intake. This result is
encouraging for future application of imbibition to enhance oil
recovery from shale.
August 2011 SPE Reservoir Evaluation & Engineering
 50

Recovery factor, %OOIP

Core with Swr
40
Core with no Swr

30

20

10

0
1 10 100 1,000 10,000
Time, minutes

Fig. 6—Brine intake into cores saturated with Soltrol 130 oil.

Fig. 7—Cracks that developed during brine intake.

Fig. 8 replots the data from Fig. 6 to reveal the brine intake
rate (expressed in cm3 of volume imbibed per cm2 of rock area
per day) vs. time. As expected, the brine-intake rate decreased
with time. However, the behavior was reasonably similar for the
two cores tested (i.e., with vs. without the presence of a connate-
water saturation).
In our experiments in this paper, no overburden pressure was
applied. We recognize that as overburden pressure increases, poros-
ity and permeability may decrease significantly, and consequently,
the imbibition rate may decrease. It is also possible that the ulti-
mate level of imbibition could be affected also. These topics will
be addressed in our ongoing research.
Conclusions
As part of an effort to assess the potential for imbibition to recover
oil from shale, we studied porosity, permeability to oil, perme-
ability to water, and spontaneous brine intake for the Pierre shale.
We found the following.
1. Porosities for Pierre shale cores were relatively high—from 25
to 35%.
2. Porosities for Bakken cores averaged less than 3%.
3. Bakken oil imbibed into dry Pierre shale cores (up to 5 mm in
thickness) to the same extent as could be achieved by forced
injection of oil (i.e., achieving the same oil saturations for both
processes).
4. Permeability to a clean mineral oil (Soltrol 130) was higher
than for Bakken oil—apparently because of deposition of wax/
asphaltenes/particulates on the Pierre core faces when injecting
Bakken oil.
1
Imbibition rate, cm/d
5. Permeability to oil for Pierre shale cores (with no water pres-
ent) ranged from 3.32×10−5 to 2.19×10−4 md when injecting
Bakken oil and from 4.85×10−4 to 2.34×10−3 md when injecting
Soltrol 130.
6. Permeability to Bakken oil for a Bakken core (with no water
present) averaged 4.84×10−4 md.
7. In Pierre shale and Bakken cores with thicknesses ranging
from 0.65 to 5 mm, permeabilities were basically independent
of flow rate, in agreement with expectations from the Darcy
equation.
8. A saline brine was spontaneously drawn into oil-saturated Pierre
cores, yielding recovery values up to 41% OOIP.
9. During exposure to brine, our results indicated an increase in
Pierre shale permeability—presumably by mineral dissolution
during forced brine injection and by cracking (possibly caused
by clay swelling) during spontaneous brine intake. This result
is encouraging for future application of imbibition to enhance
oil recovery from shale. Before these studies, we feared that
exposure to brine might reduce shale permeability because of
clay swelling.
Nomenclature
D = diameter, mm
Deff = effective diameter, mm
L = thickness, mm
PV = pore volume, cm3
q = flow rate, cm3/hr
Swr = connate-water saturation
Vshale = volume of the shale rock, cm3
W1 = dry weight of the shale rock, g
WO = weight after oil saturation, g
ΔP = pressure gradient, psi

0.1
ΔW = weight change, g
␮o = fluid viscosity, mPa·s
␳o = oil density, g/cm3
0.01
␳w = brine density, g/cm3

0.001 Acknowledgments
Core with Swr
Core with no Swr We thank Hess Corporation and the North Dakota Geological
Survey’s Wilson M. Laird Core and Sample Library for support-
0.0001 ing core samples, and thank Will Gosnold, Richard LeFever, and
1 10 100 1,000 10,000 Joseph Hartman for providing useful technical information about
Time, minutes Pierre shale. Thanks also to Nels Forsman, Deborah Hanson,
and Hanying Xu for providing us the support and laboratory
Fig. 8—Brine-intake rate [in (cm3/cm2)/d or cm/d] vs. time items. We especially appreciate Randy Seright’s suggestions dur-
(replot of Fig. 6). ing the experiments. Partial funding for this work was provided by

August 2011 SPE Reservoir Evaluation & Engineering 511

RPSEA/DOE and NDIC under Contract Number 09123-09. This
support is gratefully acknowledged.
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512
SI Metric Conversion Factors
cp × 1.0* E–03 = Pa·s
ft × 3.048* E–01 = m
in. × 2.54* E+00 = cm
md × 9.869 233 E–04 = µm2
psi × 0.00689 E+00 = MPa
*Conversion factor is exact.
Dongmei Wang is a petroleum engineering scientist in the
department of geology and geological engineering at the
University of North Dakota since July 2009. E-mail: Dongmei.
Wang@engr.und.edu. Earlier, she was a department chief and
senior engineer of EOR department, and director of overseas
petroleum potential evaluation center at the Exploration and
Development Research Institute of Daqing Oilfield Company of
PetroChina, where she worked since 1987. Wang holds a bac-
calaureate degree in computer programming from the Daqing
Petroleum Institute of China (1987) and computer science from
the University of Changchun Science and Technology of China
(1999), and MS and PhD degrees from the Research Institute of
Petroleum Exploration and Development of China (2001 and
2007, respectively). Her expertise is in EOR project planning and
case design, numerical reservoir simulation, and economic eval-
uation. Raymond D. Butler is a research associate in the depart-
ment of geology and geological engineering at the University
of North Dakota. E-mail: Raybutler@engr.und.edu. He holds a
baccalaureate degree in geological engineering (petroleum)
(1970), an MS degree in geology (1973), and a PhD degree in
geology (1980), all from the University of North Dakota. Butler’s
specialty areas include sedimentology, stratigraphy, depositional
systems, petroleum geology, and hydrogeology. He has a broad
range of expertise and experience, ranging from numerous geo-
logic and hydrogeologic projects for industry and research in the
northern plains and Williston basin region, to petroleum explora-
tion in Montana and offshore Gulf of Mexico, and environmental
consulting. Hong Liu is a laboratory technician in the department
of geology and geological engineering at the University of North
Dakota, where she has worked since January 2008. E-mail: Hong.
Liu@engr.und.edu. Before that, she worked for Wilo Pump GMBH-
Beijing Branch as a secretary since 1996 and technical develop-
ment division, Microelectronics Center of Chinese Academy of
Sciences as an assistant engineer from 1994 to 1995, and Braking
Laboratory, Department of Mechanical Engineering of Southwest
Jiaotong University of China from 1986 to 1994. Liu holds a bac-
calaureate degree in mechanical and electronic engineering
from the Southwest Jiaotong University, Sichuan of China (1988)
and an MS degree in science of business from New Mexico
Institute of Mining and Technology (2004). Salowah M. Ahmed
is a laboratory technician in the department of geology and
geological engineering at the University of North Dakota where
she has worked since December 2008. E-mail: salowah.Ahmed@
engr.und.edu. She worked for North Dakota Geological Survey
as a volunteer Geologist in 2008 and for General Petroleum
Company of Egypt during 1983 to 1985 as a geologist. She holds
double baccalaureate degrees in geology and chemistry, and
computer programming from Ain Shams University of Egypt.
August 2011 SPE Reservoir Evaluation & Engineering