SPE 116364

Entrance Pressure of Oil Based Mud into Shale: Effect of Shale, Water
Activity, and Mud Properties
Andres Oleas, SPE, Collins E. Osuji, SPE, Martin E. Chenevert, SPE, and Mukul M. Sharma, SPE,
University of Texas at Austin

Copyright 2008, Society of Petroleum Engineers

This paper was prepared for presentation at the 2008 SPE Annual Technical Conference and Exhibition held in Denver, Colorado, USA, 2124 September 2008.
This paper was selected for presentation by an SPE program committee following review of information contained in an abstract submitted by the author(s). Contents of the paper have not been
reviewed by the Society of Petroleum Engineers and are subject to correction by the author(s). The material does not necessarily reflect any position of the Society of Petroleum Engineers, its
officers, or members. Electronic reproduction, distribution, or storage of any part of this paper without the written consent of the Society of Petroleum Engineers is prohibited. Permission to
reproduce in print is restricted to an abstract of not more than 300 words; illustrations may not be copied. The abstract must contain conspicuous acknowledgment of SPE copyright.

Abstract
Oil-based muds (OBMs) have been developed to combat drilling problems often caused by shale hydration. Therefore, it is of
utmost importance to understand the interaction of OBMs as they contact shales. Past research (Chenevert 1970) has shown
how the movement of water from OBMs can be controlled by the addition of salt. This paper deals with the movement of the
oil phase of the OBM, as described by its hydraulic Entrance Pressure. Although the oil filtrate of the OBM does not
hydrate the shale, it can penetrate and flow into the shale at a certain entrance pressure. Such flow into shale can be as
damaging as water flow, because it increases the pore pressure of the shale, which can cause wellbore failure. It is of primary
interest to understand this when using OBMs in shales. It is also important to understand how factors such as the emulsifier
concentration in the OBM and the porosity of the shale affect this entrance pressure.
The objective of this study is to perform laboratory tests in order to determine and quantify the factors that control the entry
pressures for shales. For this purpose, five OBM samples with different emulsifiers and oil and water concentrations were
prepared. The study was also intended to derive an understanding of the effects of shale porosity on entrance pressure. In
order to vary the porosity of the test samples, it was convenient to place them in various controlled environments with relative
humidity (i.e. water activities). Data are reported for Arco China shale samples having porosities of 1.8% (native), 3.9%, and
4.9%, at water activities (aw) of 0.72, 0.86, and 0.96, respectively.
It was observed that as the emulsifier concentration increased, the oil breakthrough pressure increased. It was also observed
that as the porosity of the shale is reduced (smaller pore throats), the entrance pressure for the mud increases.
Introduction
Shales are low-permeability sedimentary rocks with small pore radii that have medium to high clay content, in addition to
other minerals, such as quartz, feldspar, and calcite. The distinguishing features of shale are its clay content and lowpermeability, which results in poor connectivity through narrow pore throats. Shales are also fairly porous and are normally
saturated with formation water, with several factors affecting their properties, such as burial depth, water activity, and the
amount and type of minerals present.
Considering the fact that shales account for 70 75% of the formations drilled around the world (Manohar, 1999), it is
important to understand and minimize shale-related problems while drilling. Drilling performance has exhibited the
effectiveness of OBMs in combating drilling problems caused by shale hydration, differential pressure sticking, corrosion, and
high formation temperatures (Simpson 1978). However, when using a water-based mud, water movement from the mud to the
shale results in swelling stresses and pore pressure increases that lead to wellbore failure.
OBMs are water-in-oil emulsions that contain water, emulsifiers, organophilic clay, and a weighting material (Growcock,
et, al. 1994). The water phase is usually a calcium chloride (CaCl2) salt solution, with a water activity (aw) that resembles the
aw of the formation. This eliminates water transfer to or from the water-sensitive zones and thereby maintains a stable
wellbore. The water in the oil is stabilized with a primary emulsifier (often a fatty acid salt), while the weighting material and
the drilled solids are made oil-wet and dispersed in the mud with a secondary emulsifier. It is thought that both emulsifiers
have dual roles, with the primary emulsifier also acting to some extent as a wetting agent, and the secondary emulsifier acting
as a true emulsifier.
Ions that are added to a water-based mud (WBM) reduce the water activity (aw) of the fluid, and consequently, water
movement into the shale is reduced due to osmotic effects (Chenevert, M. E. and Sharma, A. K. 1991). This effect is not long

SPE 116364

lasting because the hydrated ions are not very restricted and they thereby invade the low-salinity shale. However, for OBMs,
an efficient membrane exists around each water droplet, and very little (if any) ion transfer occurs.
Background of the Problem
Even though the osmotic pressure generated by the OBM prevents the flow of water into the shale, this membrane might not
be completely efficient. Data from different tests using inverse emulsion drilling fluids do not yield a perfect osmotic
membrane (Schlemmer, F. J et. al. 2002). The nature of the emulsified salt solution and the emulsifier package may affect the
interaction of invert emulsion fluids with shales, including the transport of fluids into or out of the shale.
The shale sealing characteristic is a result of the small water-wet pore sizes (100 nm or less), making it difficult for a nonwetting hydrocarbon fluid to penetrate a shale. In order to overcome the opposition of shale to fluid invasion, the hydraulic
pressure differential between the invading fluid and the water present in the shale needs to be higher than the capillary entry
pressure of the shale. When using an OBM, exceeding this capillary entry pressure will result in the oil filtrate of the mud
displacing the free water of the shale.
It is expected that the entry pressure of OBM filtrate (oil-only) will be higher than the entry pressure of a water-based mud;
this is because it is difficult to separate the emulsified water droplets from the emulsifier coating, and even after separation
occurs, the filtrate is immiscible with the pore fluid. Therefore, the OBM filtrate needs to displace the pore fluid in order to
invade the shale. This could explain the ability of an OBM to maintain a stable wellbore during drilling operations. The
capillary entry pressure can be calculated by Equation 1.
Pc = 2

cos Eq.1
r

where is the interfacial tension between the mud filtrate and native pore fluid, is the contact angle between the drilling
fluid and the rock surface, and r is the pore radius. This equation suggests that increasing the interfacial tension and contact
angle can increase the capillary pressure for a given pore size.
Even though a high entrance pressure is an important component in understanding the interaction between OBMs and shale
formations, it is not the only aspect to be considered. It is known that shale stability is a time-dependent problem, meaning
that the state of stress and strength of a shale varies when the shale is invaded over a period of time. Stresses in the shale at the
wellbore wall are altered as the drilling fluid filtrate pressures up the pore-fluid in the shale.
Scope of Research
This work was initiated to achieve the following goals:
1. Establish a testing procedure and equipment suitable for measuring entrance pressures of shale samples.
2. Determine the effect of OBM composition on the entrance pressure.
3. Measure the entrance pressure of various OBMs into shale of varying porosities.
Arco China Shale Properties and Preparation
The Arco China shale core used during the laboratory testing was cored at a depth of 11,812 ft. and was preserved at the rig
site in polyethylene bags covered with heavy-duty plastic. After opening the plastic covering in the research lab, the core was
immediately immersed in mineral oil so as to prevent any contact with air prior to sample encapsulation, cutting, and slicing of
the tests samples.
A mineralogic analysis of the shale was performed by Newpark Laboratories and the results are given in Tables 1 and 2.
Based on the clay analysis, illite is the main clay present. It can be inferred that the Arco China shale does not have a high
affinity to absorb water, due to the low surface area of this mineral (80m2/gm) as compared to the surface area of smectite (750
m2/gm) (Manohar 1999). A Cation Exchange Capacity (CEC) value of 9.3 was reported, suggesting that the shale is not very
reactive, and the petrophysical data confirms that the shale is very tight, with a porosity of 1.8% and a permeability value of
0.039 microdarcies.
XRD - X- Ray Difraction
Quartz
Feldspar
Calcite
Total Clay
Kaolinite
Chlorite
Illite
Smectite
Mixed layer (Illite/Smectite)

Weight %
42.0
16.0
19.0
24.0
15.0
12.0
42.0
22.0
10.0 (13/87)

Table 1 - Arco China shale mineralogical composition

Density
(gr/cc)

Porosity
(%)

Median Pore
Aperture diameter
(microns)

Air
Permeability
(md)

2.69

1.8

0.0158

0.000039

Table2 - Arco China petrophysical properties from mercury injection

SPE 116364

The water activity of the shale (aw) is defined as the vapor pressure of the shale divided by the vapor pressure of pure water
at the same temperature. Therefore, following the procedure developed earlier (Chenevert, 1969), an adsorption isotherm for
the Arco China shale was measured. The procedure for determining the water activity was done at atmospheric conditions,
using five desiccators with five different saturated salts of known activities. Table 3 describes the salts used and their
corresponding theoretical and measured water activities.
Salt
aw theoretical aw measured
CaCl2
0.3
0.34
Ca(NO3)2
0.5
0.544
NaCl
0.76
0.777
KCl
0.86
0.873
KH2PO4
0.96
0.963
Table 3 - aw of salts used to develop Arco China adsorption isotherm

The procedure used to determine the native moisture content of the shale starts by cutting 0.5 cubic samples of the shale.
After cutting the samples, their initial weight was recorded (wi). They were then dehydrated in an oven at 220oF for about 48
hours. The samples were then weighed (wd), and the weight loss was recorded. Separate cubic samples were placed in the
desiccators which had controlled activity atmospheres. The air in the desiccators was extracted using a vacuum pump, so as to
speed up moisture absorption or desorption. The samples were weighed every day until no further changes were observed, at
which time the weights were recorded as the final weights (wf) of the shale samples. At this point, the shale samples were
considered to be in equilibrium with the controlled atmospheres in the desiccators, and to, therefore, have known water
activities. The native moisture content and the percentage variation of weight of the samples were calculated using Equations 2
and 3, respectively. The results are summarized in Table 4 and Fig. 1.
Native moisture content % = wi wd 100 ....... (2)
wd

Percentage water adsorption % = w f wi 100 (3)

wi

Native Moisture Content (%) = ((wi-wd)/wd)*100

SAMPLE

wi (gr)

wd (gr)

1
2
3
4
5

6.617
7.911
6.565
6.202
6.333

6.553
7.862
6.525
6.163
6.287

water absorbed
weight after
Native Moisture
from dry sample
hydration (gr)
Content (%)
(gr)

Water Absorbed
from original
sample (%)

Water Absorbed
from dry sample
(%)

6.578
7.887
6.568
6.215
6.361

0.025
0.977%
-0.589%
0.38%
0.025
0.623%
-0.303%
0.32%
0.043
0.613%
0.046%
0.66%
0.052
0.633%
0.210%
0.84%
0.074
0.732%
0.442%
1.18%
Average 0.715%
Table 4: Native Moisture Content and Water Absorbed for Arco China shale
Adsorption isotherm curve for Arco China shale
0.60%

Shale altered
to this aw

Water Absorbed (%)

0.35%

0.10%

R =1
0

0.25

0.5

0.75

-0.15%

-0.40%

-0.65%

Water Activity

Fig. 1 Adsorption Isotherm for the Arco China shale

As demonstrated in Figure1, the native water activity of the Arco china shale is 0.72, the point at which there was no
water loss or gain.

SPE 116364

Shale Sample Preparation

The original core that was preserved at the well site was 4 inches in diameter and 6.5 inches long. The pressurized testing
cell used in this study requires the shale test specimen to be 2.5 in diameter and 0.260 0.020 inches thick. Consequently, the
core needed to be cut and sliced to satisfy the required cell measurements. Using a circular saw, the core was cut along its axis
into two half-moon pieces. These two pieces were then cut obtaining two core columns of dimensions 1.4 x 1.4 x 6.5
each. The two core columns were placed in a can filled with mineral oil for preservation.
Materials and Sample Incapsulation Procedure
The materials used to prepare the shale samples include the following: a plastic tube of 2.5 OD x 2.25 ID x 11 length;
an acrylic base; epoxy curing agent; and resin.
The procedure to obtain circular samples of 0.260 0.020 inches consisted of sealing the 1.4 x 1.4 shale column inside
the center of the plastic tube using a 2-part epoxy. After curing, the tube-epoxy-shale unit was sliced into test specimens 0.26
thick using an oil-cooled diamond saw. A typical specimen is shown in Fig.2.

Fig. 2 - Shale sample after slicing

Characterization and Preparation of Oil-Based Muds

The three major components of an OBM are synthetic oil, the aqueous phase, and the emulsifiers. The aqueous phase is
normally a calcium chloride solution (CaCl2) in the range of 25 to 40% by weight. The presence of CaCl2 provides the
osmotic pressure needed to prevent the movement of water within the emulsified droplets (applied?) to the shale. Normally
two emulsifiers are used in an OBM formulation. The first emulsifier lowers the interfacial tension of the aqueous phase to
allow small-sized droplets to be formed, but will not form a physical barrier around them. The barrier is obtained by the use of
a second emulsifier that provides high emulsion stability, high temperature tolerance, lower filtrate loss, and better solids
wetting.
Shale stability using OBMs is accomplished by eliminating the wellbore hydration caused by water-based muds. Adjusting
the CaCl2 concentration to match the water activity of the troublesome shales provides a stable wellbore, since the transfer of
water to or from the water-sensitive zones is minimized (Growcock, et, al. 1994). Laboratory swelling-tests confirmed the
balanced activity concept by showing that water adsorption does not take place when the activity of the water in the shale is
equal to the activity of the water in the mud (Chenevert, 1970).
A good OBM must satisfy some guidelines to be considered acceptable, including an oil-only filtrate of no more than 5 to
10 ml, and an electrical stability (ES) of 500 Volts or higher (Simpson, 1978).
The ES value is considered an emulsion stability parameter (Growcock, et, al., 1994). High values of ES voltage are
directly related to more stable emulsions. On a given well, the lowering of values of ES voltage indicate the need to add
emulsifiers to the system in order to obtain stability. In general, the ES and the HTHP fluid loss are considered the main
parameters used to evaluate OBM stability. They are both expected to move in opposite directions. In this study, the HTHP
fluid loss equipment was not available, so the low temperature low pressure API cell was used in its place.
Mud Preparation Procedure
The base fluid used to form every mud sample of this study consisted of 600 ml of Escaid 110 oil, 24 grams of emulsifier
1 (EZ-Mul) and 8 grams of emulsifier 2 (X-Vis). All components were stirred at 5000 RPM for 5 minutes. Later an additional
200 ml of Escaid were added to the mixer and stirred for 2 more minutes. This was the first step prior to the preparation of the
five different muds to be tested with the Arco China shale samples. This base fluid was later altered by the addition of CaCl2,
lime and mineral oil, at different concentrations so as to obtain five different oil-base muds (Table 6). The emulsifiers used in
the preparation of the base fluid are Baroid products.
During the preparation of the five mud samples, the API filtration and ES tests were performed at different stages in order
to monitor the stability of the mud. In the initial test, the mud was hot-rolled for 15 hours at 260oF, after it was mixed in the
constant speed mixer so as to make the emulsions more stable. The five samples are described in Tables 5 and 6.
The five muds that were tested with the Arco China shale were the result of adding different volumes of calcium chloride
solution (CaCl2 30% w/w, Eq. 3) and Escaid 110 to the base fluid.

SPE 116364

% weightCaCl 2 =

CaCl2
Eq. 3
CaCl2 + H 2O( deonized )

Mud Base fluid (ml) Escaid (ml)

Mud 1
Mud 2
Mud 3
Mud 4
Mud 5

100
100
100
100
100

CaCl2 - 30% w/w

Lime (gr)
(ml)

100
100
100
0
50

SG Base Fluid =
SG Escaid 110 =
SG CaCl2 =

45
90
180
45
45

2.5
2.5
2.5
2.5
2.5

0.78
0.78
1.25

Emulsifier
Concentration/Total
Mud Weight (%)
3.1%
2.5%
1.8%
4.6%
3.7%
Escaid
78 gr

CaCl2 / Escaid w/w Vol Oil (%) Vol Emulsion (%)

0.37
0.74
1.47
0.75
0.49

80.0%
67.6%
51.6%
66.2%
74.9%

Base Fluid (100 ml)

EZ-Mul
3 gr

20.0%
32.4%
48.4%
33.8%
25.1%

X-Vis
1 gr

Table 5 - Mud matrix and relevant ratios

Mud
Mud
Mud
Mud
Mud
Mud

1
2
3
4
5

Base Fluid
(ml)

Escaid
(ml)

CaCl2 (30%)
(ml)

Lime (gr)

Emulsifier
Concentration / Total
Mud Weight (%)

100
100
100
100
100

100
100
100
0
50

45
90
180
45
45

2.5
2.5
2.5
2.5
2.5

2.9%
2.3%
1.6%
4.6%
3.6%

CaCl2 / Escaid API filtrate

w/w (%)
(ml)
0.37
0.74
1.47
0.75
0.49

ES
(Volts)

Mud aw

1130
380
200
795
830

0.57
0.61
0.66
0.66
0.57

5.2
4.6
8.1
0.9
3

Table 6 - Oil-base muds properties and representative ratios

The mud preparation procedure was developed while mixing the first mud (mud 3). Both filtration and ES values were
measured. The initial mud was mixed using the multimixer. The next step was to monitor the ES and temperature while
mixing the mud at different speeds using the constant speed mixer until the maximum speed of 19000 rpm was reached. Fig. 4
describes the sequence of mixing that was followed and shows the response of the ES and temperature. The temperature
reached with the constant speed blender will depend on the friction between the mud and the blade inside the blender. After
the mud was mixed, it was hot-rolled overnight and then poured into a beaker and the ES was measured. The final
measurement of ES was used to show the benefits of the hot-rolling procedure. The same procedure was followed when
preparing the four other mud samples.
The general procedure for preparing laboratory OBMs started by mixing 100 ml of the base fluid with a defined volume of
CaCl2 solution and Escaid. Then, 2.5 grams of lime were added, after which the mixture was stirred using the multimixer and
recording an ES measurement every 5 minutes.
The speed of the mixer was increased gradually, using steps of 4000 RPM to the maximum allowable (the maximum speed
will depend on the friction between the mud and the rotating blade). The mud was stirred until the temperature of the mud
increased to a final temperature of 220oF. When the temperature was reached, a second ES measurement was taken. The
OBM was then cooled to ambient temperature and another ES measurement was taken.
The API filtration test that followed took filtration volume measurements after 1, 2, 3, 5, 7.5, 15 and 30 minutes. The hotroll oven was pre-heated to 260oF. The OBM was then hot-rolled for not less than 15 hours, after which a measurement of the
ES of the mud was taken. The mud was then cooled to ambient temperature and a final ES reading obtained. The filtration
test that followed used the same time intervals as the pre-hot-roll test. In total, five main ES data points were taken for each of
the mud samples prepared (Fig.3).
Electrical Stability
Mud 1

Mud 2

Mud 3

Initial Mud (Mud 3)

Mud 4

Mix 5

275

1600 Volts

19000 RPM

Temp (F) & ES (Volts)

250

1400 Volts
1200 Volts
1000 Volts
800 Volts
600 Volts

10000 RPM

15000 RPM

225
200
175
150
125
100
75

400 Volts

50
0

10

20

30

200 Volts

40

50

60

70

80

Time (min)

0 Volts
In multimixer for 5
minutes @ 71 F

In blender at maximum ES before filtration @

rpm @ 220 F
71 F

After hot-roll @ 190 F

ES before filtration @
71 F

Fig. 3 - ES data taken during OBM preparation

Temp (F)
ES before mixing
ES after hot-roll

ES (Volts)
ES after mixing before hot-roll

Fig. 4 - Sequence of preparation for Mud 3

90

SPE 116364

A comparison of the filtration data before and after hot-rolling is shown in Fig. 5 and 6. From the filtration tests, it can be
seen that the reduction in filtrate volume is significant.
Filtration at 71 F (before hot roll)
Mud 2

Mud 3

Filtration at 71 F (after hot roll)

Mud 4

Mud 5

Mud 1

80.0

9.0

70.0

8.0

60.0

7.0

50.0

6.0

Filtrate (m l)

Filtrate (m l)

Mud 1

40.0
30.0
20.0

Mud 2

Mud 3

Mud 4

Mud 5

5.0
4.0
3.0
2.0

10.0

1.0

0.0

0.0

0.0

5.0

10.0

15.0

20.0

25.0

30.0

35.0

0.0

5.0

10.0

15.0

Time (minutes)

20.0

25.0

30.0

35.0

Time (minutes)

Fig. 5 - API filtration before hot-roll

Fig. 6 - API filtration after hot-roll

As shown in Fig. 4, after all the oil-based mud preparation sequence had been completed, the final ES measurement had
improved by 100% for muds 2 and 3, and by more than 800% for the other muds. Muds 2 and 3 are the emulsions with a
lower emulsifier/CaCl2 water ratio. Therefore, it is believed that in a drilling situation, should formation water enter these
muds, the stability of these muds will decrease. For such muds, it is normal to add extra emulsifier to the muds to compensate
for the additional water entering the well, so as to maintain a stable emulsion. It is also noted in Fig. 3 that the ES for mud 4
decreased from 1300 to 550 V after it was hot-rolled. The ES then increased again to 800 Volts after it cooled down to
ambient temperature. This irregular behavior might indicate that for this particular mud, the hot-rolling is not beneficial, in
terms of improving the ES. Mud 4 has the highest emulsifier/CaCl2 ratio among the five muds.
The variation of ES with time for a mud is a direct indication of its stability while the mud is not being used. Fig. 7 shows
the ES data for the five OBMs. It can be seen that these muds maintain, or even increase, their ES properties with time. Muds
4 and 4b are the same mud; the only difference is that ES measurements were taken before and after Mud 4 was used in an
actual test, while Mud 4b was prepared without being tested. It is noted that the ES of the mud did not decrease after being
exposed to a pressurized test-environment for two weeks.

ES (Volts)

ES Variation with time for Oil-Based Muds

1400.0
1300.0
1200.0
1100.0
1000.0
900.0
800.0
700.0
600.0
500.0
400.0
300.0
200.0
100.0
0.0
0

10

12

14

16

18

20

22

24

26

28

30

32

34

36

38

40

time (days)

Mud 1

Mud 2

Mud 3

Mud 4

Mud 5

Mud 4b

Fig. 7 - ES measurement for OBMs

Shale Capillary Entrance Laboratory Pressure Test

Entrance pressure tests performed by different authors ave shown that it is possible to flow fluid through shales ay high
enough overbalance pressures (Al-Bazali, et. al. 2005). This study focused on the use of laboratory OBMs only, so as to
understand the behavior of shale while it is exposed to various oil-base mud emulsions. The capillary entry pressure
determines the sealing capacity of the rock, and the hydrostatic pressure necessary to overcome the capillary properties of the
shale. It is dependant on the following factors: interfacial tension between the water-wet shale and the non-wetting fluid, the
contact angle between them, and the pore throat radius (Eq. 4), where hH is the hydraulic head, Pc is the capillary entry
pressure, m is the density of the mud, and g is the acceleration due to gravity.

SPE 116364

hH =

Pc

m g

Eq.4

A large capillary pressure prevents entry of the oil into the shale, since the pressure differential is lower than the minimum
capillary entry pressure (Manohar 1999). Capillary pressures for low permeability water-wet shales can be as high as 2200 psi
for a pore radius of 10 nm.
Entrance Pressure Test Description
The entrance pressure test and equipment used was very similar to the one used by Al-Bazali in 2005. A shale sample of
0.260.010 inches thick by 2.5 inches in diameter was placed in a metallic chamber that had top and bottom ports that allowed
the shale sample to be subjected to different OBMs and pore fluids (Fig. 8 and 9).
T1
V8

Upstream Fluid

T2

N2
V7

V6

C2

VV

Piston reaction chamber

N2

V1a
V5

Shale sample

C1

Cell Chamber
VB2
Vacuum Pump

V3
T6

Hand Pump
V4

VB3

V2

Downstream Fluid
VB1

Vacuum Pump
V1a

Fig. 8 - Main cell used to measure the

Oil breakthrough pressure

Fig. 9 Test Equipment schematic

As mentioned above, the shale sample was exposed to a top oil fluid (OBM) and bottom NaCl fluid of 35,000 ppm salinity
(simulated sea water) or a CaCl2 solution at 30% w/w. During the test, the pressure differential across the shale was initiated
by first setting the upstream (top of sample) and downstream (bottom of sample) pressure to 50 psi, then gradually increasing
the upstream pressure. The entrance pressure was detected at the moment an increase in the pressure of the bottom side of the
shale was observed. Once the downstream pressure stabilized, the upstream pressure was again increased and the behavior of
the downstream pressure was observed. During the tests, time between pressure-increase steps (100 to 250 psi at a time) was
at least eight hours. This extended period allowed the entire system to stabilize its internal volume of fluid and temperature.
The duration of each of the tests was as long as one week.
Temperature-Pressure Sensitivity
Because the top and bottom fluid chambers were very small, it was necessary to determine how the pressure
measurements of the equipment were affected by temperature variations. This was done by increasing the temperature of the
entire test unit and measuring the response, as shown in Fig. 10. A temperature increase of one degree Fahrenheit can produce
a 15 psi change in pressure, thus all experiments were run under tightly controlled temperature conditions. As will be shown
below, cell temperature values are often reported along with entrance pressure data.

105

370.0

100

320.0

95

270.0

90
85

220.0
Downstream = NaCl 35000 ppm

170.0

80
75

120.0
Upstream = NaCl 35000 ppm

70.0

Temperature (F)

Pressure (psi)

Temperature Calibration - Test Cell with Solid disc

420.0

70
65

20.0
0

12

16

20

24

Time (hours)

Upstream Pressure (psi)

Downstream Pressure (psi)

Temperature (F)

Fig. 10 - Pressure response (inside cell) to temperature changes

SPE 116364

Entrance Pressure Tests

Arco China shale at 0.72 Activity
After the system was successfully tested for temperature effects and leaks, five tests were performed using the native 0.72
activity Arco China shale. These fluids consisted of fresh water, oil, and emulsion muds. As shown in Figures 11 to 14, over
the time period shown, none of these fluids were able to penetrate this shale, even after applying about 1500 psi differential
pressure.
The first test consisted of attempting to obtain breakthrough utilizing fresh water. For this purpose, both the top and the
bottom lines, and consequently the cell, were filled with fresh water. The outcome of this Initial Test 1 is shown in Fig. 11.
Arco China Shale (aw=0.72) - Initial Test 1
Date: 14-Sep-2005
No Breakthrough
1600

Pressure (psig)

1400
1200
1000

Water (aw=1.0)

800
600
400
200

Water (aw=1.0)

0
0

24

48

72

Time (hours)
Upstream Pressure (psi)

Downstream Pressure (psi)

Fig. 11 - Initial Test 1 using fresh water in the top and bottom

As shown, no pressure increase was registered on the bottom side after 60 hours, even though the upstream pressure was
increased to 1500 psig for 8 hours. From this observation, it is concluded that the permeability of the shale was too low and
the size of the pore throats very small. Due to pressure limitations of the equipment, the pressure could not be increased above
1600 psig. Three additional tests using Mud 4, Escaid 110, and Mud 3 produced similar results (Figs. 12, 13 and 14).
Arco China Shale (aw=0.72) - Initial Test 3
Date: 4-Oct-2005
No Breakthrough
1600

1800
1600
1400
1200
1000
800
600
400
200
0

1400

Mud 4 (aw=0.661 - EC = 4.6%))

Pressure(psi

Pressure (psig)

Arco China Shale (aw=0.72) - Initial Test 2

Date: 26-Sep-2005
No Breakthrough

Escaid 110

1200
1000
800
600
400

NaCl (aw=0.985)

Air at Patm

200
0

12

24

36

Hours
Upstream Pressure (psi)

48

10

15

20

Time (Hours)

Downstream Pressure (psi)

Fig. 12 Initial Test 2 using Mud 4 in the

top and NaCl in the bottom

Upstream Pressure (psi)

Downstream Pressure (psi)

Fig. 13 Initial Test 3 using Escaid 110 in the

top and Air in the bottom

25

SPE 116364

Pressure (psig)

Arco China Shale (aw = 0.72) - Initial Test 4

Date: 7-Nov-2005
No Breakthrough
1300
1200
1100
1000
900
800
700
600
500
400
300
200
100
0

Mud 3 (aw = 0.655 - EC = 1.8%)

NaCl 35000 ppm (aw =

24

48

72

96

120 144 168 192 216 240 264 288 312 336 360

Time (hours)
Upstream Pressure (psi)

Downstream Pressure (psi)

Fig.14 Initial test 4 using Mud 3 in the top and NaCl in the bottom

Alteration of Shale Porosity

Given the lack of fluid penetration over the time allotted, it was decided to open up the pores of the 0.72 aw shale samples in an
attempt to obtain breakthrough. Therefore, samples were partially hydrated by placing them in desiccators with controlled
humidities of 0.86 and 0.96.
The samples weight increase by water absorption was monitored every day, and it was observed that weight equilibrium
was essentially reached after two weeks.
It was of interest to calculate the change in porosity of the shale; this was done by placing several shale samples that had
been altered to 0.86 and 0.96 aw back into the 0.72 aw desiccator and recording their weight loss. A sample calculation of the
new porosity is shown below:
- wi = 5.148 g (aw = 0.72)
- w2 = 5.055g after dehydrating the sample in the oven
- w3 = 5.186 g after hydrating the sample in a 0.76 water activity desiccator
Knowing the dimensions of the sample (1.728 x 1.610 x 1.857 cm) and assuming that the pore fluid (water) has a density
of 1 g/cc, the porosity calculation gave the results shown below:
i =

V pores

f =

Vtotal

5.148 gr 5.055

1gr / cc
= 0.018
=
(1.728 1.610 1.857 )cm3

V pores
Vtotal

This is the initial porosity of the rock

5.186 gr 5.055

1gr / cc
= 0.026
=
(1.728 1.610 1.857 )cm3

This is the final porosity of the rock after hydration.

Fig. 15 shows the porosity vs. water activity results obtained for the Arco China shale using water activity desiccators, set
at 0.76, 0.86 and 0.96 activity.
Shale Porosity change due to Water Activity Alteration
6.0%

Porosity (%)

5.0%

4.9%

4.0%
3.9%
3.0%
2.6%

2.0%

1.8%

1.0%
0.0%
0.7

0.75

0.8

0.85

0.9

0.95

Water Activity (fraction)

Fig. 15: Porosity Increase due to water activity alteration for the Arco China shale

10

SPE 116364

Breakthrough Pressure Tests using Altered Shale Samples

With shale samples of altered porosity now available, pressure breakthrough was achieved with fresh water, Escaid, and the
five OBMs. Tables 7 and 8, and Figs. 16 through 25 show the results.
The first test, Fig. 16, used fresh water in the top (upstream) and a sodium chloride solution was used to simulate reservoir
fluid in the bottom (bottom do you mean downstream?). The shale sample used in this initial test had an altered aw of 0.96. The
breakthrough pressure is proof that the pores of the shale had been enlarged in diameter and fresh water had invaded the
sample.
After pressure was increased several steps, and a final stable downstream pressure was observed, a reverse flow test was
performed. The reverse flow test consisted of reducing the upstream pressure below the last stable pressure observed on the
bottom side; the purpose of this test was to determine whether the downstream pressure follows the trend which was observed
while the upstream pressure was increased in steps. This assured that there was backflow from the bottom to the top,
confirming the communication between both sides of the sample.
It was also noted that after increasing the upstream pressure and achieving breakthough, the downstream pressure never
completely equalized the upstream pressure. This could indicate that there is an osmotic effect between the top fresh water
fluid and the saline pore fluid.
The results for the five initial tests (Fig 1116) are given in Table 7. Notice in Table 7 how increasing the porosity from
1.8% to 4.9% lowered the entrance pressure of oil from 1540psi to 40psi.

Pressure (psig)

Arco China Shale (aw = 0.96) - Initial test 5

Date: 21-Nov-2005
800
700
600
500
400
300
200
100
0

Fresh water (aw = 1.0)

NaCl 35000 ppm (aw = 0.985)

12

24

36

48

60

Time (hours)
Upstream Pressure (psi)

Downstream Pressure (psi)

Fig. 16: Test 5 using fresh water in the top and NaCl in the bottom with altered shale (aw = 0.96)
Initial Test Sequesnce
Test #
1
2
3
4
5

Final Differential
Pressure (psig)
1450
Water
0.00
0.72
1.8
1520
Mud 4
4.60
0.72
1.8
1450
Escaid 110
0.00
0.72
1.8
1250
Mud 3
1.80
0.72
1.8
Water
0.00
0.96
4.9
40
Table 7 - Initial Test Sequence for the Arco China shale
Top Fluid

EC (%)

Shale aw

(%)

Result
No Breakthrough
No Breakthrough
No Breakthrough
No Breakthrough
Breakthrough

It was of primary interest to measure and compare the oil breakthrough pressures obtained using (a) muds of different
compositions and (b) the same mud with shale samples altered to different water activities.

SPE 116364

11

Arco China Shale Tests at 0.96 Activity ( = 4.9%)

Arco China Shale (aw = 0.96) - Breakthrough Pressure
Test 1 - date: 30- Nov - 05
Upstream
Osmotic
Mud 3, aw = 0.66

Arco China Shale (aw = 0.96) - Breakthrough Pressure

T est 2 - date: 7-Dec-05
Upstream
Osmotic

Hydraulic

Hydraulic

Mud 1, aw = 0.57

Shale aw = 0.96

Shale aw = 0.96

NaCl, aw = 0.98

NaCl, aw = 0.98

Downstream

Downstream

700

1200
Mud 1 (aw=0.565)

600

1000
EC = 2.9%
BT P = 735 psig

Pressure (psig)

Pressure (psig)

500
Mud 3 (aw = 0.655)
400
EC = 1.6%
BT P = 194 psig

300

800
600
400

200

200

100

NaCl 35000 ppm (aw=0.985)

NaCl 35000 ppm (aw = 0.985)

0
0

24

48

72

96

120

144

168

24

48

Time (hours)
Upstream Pressure (psi)

72

96

120

144

Time (hours)

Downstream Pressure (psi)

Pressure Differential

Upstream Pres s ure (ps i)

Fig. 17

Downs tream Pres s ure (ps i)

Pres sure Differential

Fig.18

Arco China Shale (aw=0.96) - Breakthrough Pressure

Test 3 - date: 14-Dec-05
Upstream
Osmotic

Mud 2, aw = 0.61

Arco China Shale (aw = 0.96) - Breakthrough Pressure

Test 5 - date: 2-Jan-06
Upstream
Osmotic

Hydraulic

Mud 4, aw = 0.66

Shale aw = 0.96

Hydraulic

Shale aw = 0.96

NaCl, aw = 0.98

NaCl, aw = 0.98

Downstream

120

800.0

Downstream

1400.0

130

Mud 2 (aw=0.606

100

500.0
400.0
300.0

80

100

600.0

90

NaCl 35000 ppm (aw=0.985)

100.0
NaCl 35000 ppm (aw=0.985)

110

800.0

200.0

0.0

120

EC = 4.6%
BTP = 944 psig

1000.0

Pressure (psig)

EC = 2.3%
BTP = 475 psig

Temperature (F)

Pressure (psig)

600.0

Mud 4 (aw=0.661)

1200.0

400.0

80

200.0

70

60

24

48

72

0.0

96

60
0

24

48

72

96

120 144

168

192 216

240 264

288 312

336 360

384

408 432

456 480

504 528

552

Time (hours)

Time (hours)
Upstream Pressure

Downstream Pressure

Upstream Pressure (psi)

Downstream Pressure (psi)

Pressure differential

Temperature (F)

Pressure differential

Temperature (F)

Fig. 19

Fig. 20

Arco China Shale (aw = 0.96) - Breakthrough Pressure

Test 6 - date: 26-Jan-06

Arco China Shale (aw = 0.86) - Breakthrough Pressure

Test 7 - date: 15-Feb-06

Upstream
Osmotic

Mud 4, aw = 0.66

Upstream
Osmotic

Hydraulic

Mud 3, aw = 0.66

Hydraulic

Shale aw = 0.86

Shale aw = 0.96

NaCl, aw = 0.98

CaCl2, aw = 0.64

Osmotic
Downstream

Downstream

71.5

1100.0

Mud 3 (aw=0.655)

71.6

1200.0

1000.0

Mud 4 (aw=0.661)

1100.0

Temperature (F)

700.0

900.0

70.8

700.0
600.0
500.0

70.4

400.0

CaCl2 (30%)

300.0

71

800.0

Pressure(psig)

800.0

Temperature (F)

Pressure (psig)

71.2

EC = 4.6%
BTP = 299 psig

900.0

EC = 1.6%
BTP = 677 psig

700.0
600.0

70.5
500.0
400.0
300.0

70

200.0

70

200.0

NaCl (35000 ppm) aw=0.985

100.0

100.0

69.6

0.0
0

24

48

72

96

120

144

168

192

216

240

264

288

312

336

Time (hours)

360

69.5

0.0
0

24

48

72

96

120

144

Time (hours)

Upstream Pressure (psi)

Downstream Pressure (psi)

Upstream Pressure (psi)

Downstream Pressure (psi)

Pressure differential

Temperature (F)

Pressure differential

Temperature (F)

Fig. 21

Fig. 22

168

Temperature(F)

1000.0

12

SPE 116364

Arco China Shale Tests at 0.86 Activity ( = 3.9%)

Arco China Shale (aw = 0.86) - Breakthru Pressure
Test 13 - date: 19-Apr-06

Arco China Shale (aw = 0.86) - Breakthrough Pressure

Test 9 - date: 9-Mar-06
Upstream
Osmotic

Mud 5, aw = 0.57

Hydraulic

1000.0

Shale aw = 0.86

Downstream

Pressure (psig)

Temperature (F)

71.5

900.0
800.0
700.0

71

600.0
500.0
400.0

P r e s s u r e (p s ig )

1000.0

72

Mud 5 (aw=0.567)

EC = 3.6%
BTP = 886 psig

1100.0

71.25

800.0
700.0

71

600.0

70.75

500.0
400.0

70.5

300.0
200.0

70.5

300.0

70.25

NaCl (35000 ppm) aw=0.985

100.0

NaCl (35000 ppm ) aw =0.985

200.0
100.0

24

48

72

96

70

0.0

70

0.0
0

120 144 168 192 216 240 264 288 312 336 360 384 408 432

24

48

72

96

120

144

168

192

Time (hours)

Time (hours)
Upstream Pressure (psi)

Downstream Pressure (psi)

Pressure differential

Temperature (F)

Upstream Pressure (psi)

Fig. 23

Downstream Pressure (psi)

Pressure differential

Temperature (F)

Fig. 24

Arco China Shale (aw = 0.86) - Breakthrough Pressure

Test 11 - date: 3-Apr-06
Upstream
Osmotic

Escaid, aw = 0

Hydraulic

Shale aw = 0.86
NaCl, aw = 0.98
Downstream
600.0

71.5

Escaid 110

EC = 0%
BTP = 321 psig

71

400.0

300.0

70.5

200.0

Temperature (F)

Pressure (psig)

500.0

100.0
NaCl (35000 ppm ) aw =0.985

70

0.0
0

24

48

72

96

120

144

168

Time (hours)
Upstream Pressure (psi)

Downstream Pressure (psi)

Pressure differential

Temperature (F)

Fig. 25

Base Fluid
Mud
(ml)

T e m p e r a tu r e ( F )

NaCl, aw = 0.98

1200.0

71.5

Base Fluid

BTP = 855 psig

900.0

Escaid (ml)

CaCl2 (30%) (ml)

Mud 1
Mud 2
Mud 3
Mud 4
Mud 5

100
100
100
100
100

100
100
100
0
50

45
90
180
45
45

Mud 3

100

100

180

Shale aw = 0.96
Breakthrough
Emulsifier
CaCl2 / Escaid API filtrate
ES
Lime (gr) Concentration /
Pressure
w/w
(ml)
(Volts)
(Psig)
CaCl2 (%)
2.5
6.76
0.37
5.2
1130
890
2.5
3.38
0.74
4.6
380
601
2.5
1.69
1.47
8.1
200
194
2.5
6.76
0.75
0.9
795
1023
2.5
6.76
0.49
3
830
414
Shale aw = 0.86
2.5
1.78
1.47
8.1
200
796

SPE 116364

13

Base Fluid
Mud
(ml)

Escaid (ml)

Mud 1
Mud 2
Mud 3

100
100
100

100
100
100

Mud 3

100

100

Mud

Base Fluid
(ml)

Mud 1
Mud 5
Mud 4

100
100
100

Shale aw = 0.96 (same volume of Escaid in all muds)

Emulsifier
Breakthrough
CaCl2 / Escaid API filtrate
ES
CaCl2 (30%) (ml) Lime (gr) Concentration /
Pressure
w/w
(ml)
(Volts)
CaCl2 (%)
(Psig)
45
2.5
6.76
0.37
5.2
1130
890
90
2.5
3.38
0.74
4.6
380
601
180
2.5
1.69
1.47
8.1
200
194
Shale aw = 0.86
180
2.5
1.78
1.47
8.1
200
796

Shale aw = 0.96 (Same Emulsifier/CaCl2 Concentration in all muds)

Emulsifier
Breakthrough
CaCl2 / Escaid API filtrate ES
Escaid (ml)
CaCl2 (30%) (ml) Lime (gr) Concentration /
Pressure
w/w
(ml)
(Volts)
(Psig)
CaCl2 (%)
100
45
2.5
6.76
0.37
5.2
1130
890
50
45
2.5
6.76
0.49
3
830
414
0
45
2.5
6.76
0.75
0.9
795
1023
Table 8 - Test Results for the Arco China shale using altered shales

Computation of Pore Entrance Radius

It is possible to calculate the pore entry radius (r) of the shale, assuming that the sodium chloride solution on the bottom
(downstream side) is similar to the pore fluid in the shale. For this purpose, the interfacial tension between the top fluid filtrate
and the sodium chloride was measured using a tensiometer (see Table 9). The estimated pore entry diameter (radius) was
calculated using Equation 1.
Pore Entry Diameters for shale water activities of 0.86 and 0.96
0.86 aw shale

0.96 aw shale

0.04000

Interfacial Tension between upstream and downstream fluids

Upstream Fluid
Mud Filtrate 1
Mud Filtrate 2
Mud Filtrate 3
Mud Filtrate 4
Mud Filtrate 4
Mud Filtrate 5
Escaid
Base fluid filtrate

Interfacial Tension (D/cm)

15.04
12.50
12.78
9.21
7.80
8.55
21.06
4.32

Table 9: Interfacial Tension measurements

Pore Entry Diameter (microns)

Downstream Fluid
NaCl (35000 ppm)
NaCl (35000 ppm)
NaCl (35000 ppm)
NaCl (35000 ppm)
CaCl2 (30% w/w)
NaCl (35000 ppm)
NaCl (35000 ppm)
NaCl (35000 ppm)

0.03500
0.03000
0.02500
0.02000
0.01500
0.01000
0.00500
0.00000
MF3 (EC=1.6%)

MF4 (EC=4.6%)

MF5 (EC=3.6%)

Mud Filtrate

Fig. 26: Pore entry diameters for water activities of 0.86 and
0.96

Altered Shale Permeability

It was also of interest to observe the relation between permeability and oil breakthrough pressure. The Arco China shale
samples with altered water activity were exposed to KCl fluids, so as to measure their vertical permeability. Permeabilities for
both 0.96 and 0.86 aw were determined using the Darcy equation (Eq. 6). In Eq. 6, k represents the permeability of the sample,
q is the flowrate obtained from the slope in Fig. 29, is the viscosity of the flushing fluid (KCl), L is the thickness of the shale
sample, A is the cross sectional area of the sample, and P is the difference between the upstream and the downstream
pressure.
k=

qL . Eq. 6
AP

The equipment and procedure used to measure permeability are the same as was utilized in the oil breakthrough test. The
only difference consists of the steps followed after the sample has been flushed with the test fluid.

14

SPE 116364

Potassium chloride (KCl) was the fluid used in the bottom and top chambers for the permeability measurements for each of
the altered samples. In the first study, a 0.96 water activity KCl solution was utilized, with the 0.96 altered shale. In the
second study, a 0.86 water activity KCl solution was used with an 0.86 altered shale sample. The purpose of using a solution
with the same water activity as the shale was to minimize the osmotic effects between both sides of the shale and the shale
itself. KCl solution was utilized because potassium is the best inhibitive ion for minimizing the hydration of clays and shales.
Before the permeability was measured, the samples were flushed using the KCl solutions.
In order to apply Eq. 6, a constant drawdown pressure was maintanined by using a hand pump connected directly to the
bottom side, and the downstream pressure was maintained constant by removing fluid. Recording the pump volume and the
time permitted the development of a flow versus time chart (Fig. 29), from which the flowrate was obtained for the 0.96 and
0.86 aw shales.
Permeability - Constant drawdown
0.040

0.035
Shale aw = 0.96
q = 0.0073 ml/hour
k = 0.0403 md

0.030

Flow (ml)

0.025

0.020

0.015

0.010

0.005

Shale aw = 0.86
q = 0.0011 ml/hour
0.0056 md

0.000
0

Time (hours)

Fig. 27: Determination of Flowrate for Permeability Tests

From Fig. 27, it is observed that the slope (flowrate) of 0.0073 ml/hr for the 0.96 aw shale is higher than the slope for the
0.86 aw shale (0.0011 ml/hr). This result was expected, considering the higher porosity (4.9%) for the 0.96 aw shale, as
compared to the porosity of the 0.86 aw shale (3.9%). The permeabilities of the 0.96 and 0.86 aw shales were found to be
0.0403 and 0.0056 md, respectively.

Test Intepretation and Conclusions

Base Fluid and Escaid 110 tests
For all tests run, the same Base Fluid was used as a starting point to prepare the emulsions. This fluid was also used
alone, as the top fluid for tests 12 and 13. The results are shown in Table 10:
Base Fluid
(ml)

Escaid
(ml)

100

100

Escaid (gm)

Emulsifier
Content (gr)

Emulsifier
Concentration
(gr/gr)

Breakthrough Pressure

78
4
0.051
368 psig (shale aw = 0.96)
855 psig (shale aw = 0.86)
Table 10: Base Fluid composition and Oil breakthrough Pressure results

Using only the mineral oil (Escaid 110), the test was also repeated in tests 10 and 11, without surfactant as the top fluid.
The results are shown in Table 11:
Upstream Fluid

Shale aw

Breakthrough
Pressure (psig)

Escaid 110
Escaid 110

0.96
0.86

153
321

Table 11: Oil breakthrough Pressure results using Escaid 110 as top fluid

SPE 116364

15

These results (Fig. 28) show a large difference in entrance pressures between the tests that used the base fluid as compared
to the tests that used only Escaid 110. A lower entry pressure is observed when oil is used as the top fluid, even though the
interfacial tension between the oil and the pore fluid (21 dynes/cm) is much larger than that measured between the base fluid
and the same pore fluid (4.3 dynes/cm). In addition, wettability alteration of the shale to oil wetting conditions should reduce
the capillary pressure needed to invade the shale pores. Clearly, the experimental trends do not show this behavior.
Breakthrough Pressure
Escaid and Base Fluid

0.090

900

0.080

800
700

0.070

P re s s u re (p s ig )

E n try P o re d ia m e te r
(m ic ro n s )

Pore Entry Diameter

Escaid and Base Fluid

0.060
0.050
0.040
0.030
0.020
0.010

600
500
400
300
200
100
0

0.000
Escaid

Escaid

Base Fluid

Base Fluid

Filtrate

Filtrate

Shale (aw = 0.96) Shale (aw = 0.86)

Shale (aw = 0.96) Shale (aw = 0.86)

Fig. 28: Oil breakthrough Pressure and Pore Entry Diameter for Escaid and Base Fluid

Therefore, based on capillary entrance pressure calculations, changes in the interfacial tension and wettability should lead
to smaller pore entry pressures with the base fluid. Using the capillary pressure equation (Eq. 1), an effective pore entry
diameter was calculated for both the base fluid and the pure mineral oil (Escaid 110). Fig. 30 shows that the pore diameters
calculated in this manner are significantly larger when the Escaid is used, as compared to when the base fluid is used. Because
this difference in the estimated pore entry diameter is so large (a factor of 10), it suggests that the mechanism of pore
penetration by the oil is controlled by both capillary pressure and other factors, which will be discussed in the following
paragraphs.
Fig. 29 shows invasion of the oil into the pore space of the shale when pure mineral oil is used. This process of invasion
must be controlled by capillary pressure, as the interface between the brine in the pore space and the mineral oil does not
contain any surfactants. However, the interface between the base fluid containing surfactants and water must behave in a more
elastic manner. This conjecture is based upon our experimental observations, which suggest that despite the interfacial tension
being lower, the pressure needed to invade the pore space is significantly higher. The additional pressure drop needed to
invade the pore space may be related to the energy required to elastically deform the interface between the base fluid and the
brine saturating the shale pore space. The surfactants used in the base fluid (EZ-Mul [a quarter amine] and X-Vis [a
Polymerized Fatty Acid]) are both known to stabilize emulsions by adsorbing on the oil-water interface and forming a rigid
interfacial film.
It is known that the force required to deform the elastic surface film is 1) proportional to the rigidity of the film (Adkins
1951), and 2) inversely related to the pore throat size. Our hypothesis, which states that the pore entry pressure is controlled by
the elasticity of the interface, is supported by the experimental observations, which show that the entry pressure increases as
the concentration of emulsifier is increased (higher concentrations of emulsifier make the film more rigid). Our hypothesis is
also consistent with our observation that the pore entry pressure increases as the aw of the shale is reduced.
Hydraulic Gradient

Hydraulic Gradient

OIL

BASE FLUID

OIL

Pore Throat

Interfacial Tension
4.32 D/cm

Pore Throat

Interfacial Tension
21.04 D/cm
PORE
FLUID

Fig. 29: Oil (Escaid 110) pore invasion

PORE
FLUID

Fig. 30: Base fluid pore invasion

16

SPE 116364

Effect of Water Droplets and Emulsifier Concentration in Base-Oil

In the results reported above, no emulsified water droplets were present in the liquid fluid. In this section, we discuss
results in which water droplets are present in the oil-based mud. The addition of water droplets results in an additional
resistance to flow provided by the mud cake, which is formed by the water droplets coating the surface of the shale.
As illustrated in Fig. 31, increasing the emulsifier concentration increases the oil breakthrough pressure for the different
muds containing water droplets. Increasing the concentration of CaCl2 in the mud results in larger water droplets, and
therefore, higher permeability of the filter cake and lower oil breakthrough pressures (Fig. 32).
Upstream
Fluid

Base Fluid
(ml)

Escaid
(ml)

CaCl2
(ml)

% Emulsifier
Concentration/Total
Mud weight (gr/gr)

Water
Content (%)

Breakthrough
Pressure (psig)

Mud 1
100
100
45
2.9%
20%
735
Mud 2
100
100
90
2.3%
32%
475
Mud 3
100
100
180
1.6%
48%
194
Table 12: Oil breakthrough Pressure for muds with different CaCl2 concentration (awshale = 0.96)
Breakthrough Pressure vs. Emulsifier Concentration (muds
with different CaCl2 content - muds 1,2, 3)

Breakthrough Pressure vs. Emulsifier Concentration (muds with

different CaCl2 content - muds 1, 2, 3)

Breakthrough Pressure
(psig)

Breakthrough Pressure (psig)

800
700
600
500
400
300
200
100
0
1.5%

1.7%

1.9%

2.1%

2.3%

2.5%

2.7%

2.9%

3.1%

800
700
600
500
400
300
200
100
0
15

20

25

30

35

40

45

50

55

% of CaCl2 brine in emulsion

Emulsifier Concentration (%)

Fig. 31: Oil breakthrough pressures for muds with

different CaCl2 concentration (aw shale = 0.96)

Fig. 32: Oil breakthrough pressures vs. CaCl2 content (aw shale = 0.96)

At high concentrations of emulsifier and low water content, small droplets of water with thick layers of emulsifier provide
a low-permeability cake that resists the flow of oil filtrate into the pore space.
Results were also obtained by diluting the base fluid with different quantities of pure Escaid oil (muds 1, 4 and 5). Table
13 shows the pore entry pressures for these muds. Figs. 33 and 34 show the effect of emulsifier concentration as well as of
Escaid concentration on the capillary entry pressure. No clear trends are observed in this case. This is because as the base oil
is diluted with the Escaid mineral oil, both the emulsifier concentration and the water-to-oil ratio in the mud are changing.
Since both the water content and the emulsifier concentration affect the pore entry pressure, it is difficult to make substantial
conclusions based on these plots.
Upstream
Fluid

Base Fluid
(ml)

Escaid
(ml)

CaCl2
(ml)

% Emulsifier
Concentration/Total
Mud weight (gr/gr)

Oil Content
(%)

Breakthrough
Pressure (psig)

Mud 1
100
100
45
2.9%
80%
735
Mud 4
100
50
45
4.6%
66%
944
Mud 5
100
0
45
3.6%
75%
320
Table 13: Oil breakthrough Pressure for muds with different Escaid 110 concentration (awshale = 0.96)

SPE 116364

17

Breakthrough Pressure vs. Escaid 110 concentration (muds

with different Escaid 110 content - muds 1, 4, 5)

1000

1000

900

900

Breakthrough Pressure (psig)

Breakthrough Pressure (psig)

Breakthrough Pressure vs. Emulsifier Concentration (muds

with different Escaid 110 content - muds 1, 4, 5)

800
700
600
500
400
300
200
100
0
2.5%

3.0%

3.5%

4.0%

4.5%

800
700
600
500
400
300
200
100
0
65%

5.0%

70%

Emulsifier Concentration (%)

75%

80%

85%

Escaid 110 Concentration (%)

Fig. 33: Oil breakthrough pressures for muds with

different Escaid concentration (aw shale = 0.96)

Fig. 34: Oil breakthrough pressures vs. Escaid

content (aw shale = 0.96)

Effect of Osmotic Pressure

To test the importance of osmotic pressure in the pore entry pressures, mud 4 (containing 0.985 aw emulsified NaCl water)
was used on the top and 0.64 aw calcium chloride water was used as the bottom fluid. It is observed that the oil breakthrough
pressure is significantly larger when a higher aw fluid is placed on the downstream end (Fig. 35). This result clearly shows that
osmotic pressure differences across the shale can play an important role in controlling the entry pressures into the shale.
Indeed it appears as if a combination of the hydraulic gradient and the osmotic gradient will control the entry pressure into the
shale.

Pressure (psig)

Breakthrough Pressure
Mud 4 with different downstream fluids
1000
900
800
700
600
500
400
300
200
100
0
MF4 (EC=4.6%) NaCl

MF4 (EC=4.6%) CaCl2

Filtrate
Shale (aw = 0.96)

Fig. 35: Entrance Pressure Effect for mud 4 with different bottom fluids

This experimental result shows the importance of maintaining a significant osmotic pressure differential between the shale
and the OBM, so that the invasion of oil filtrate into the shale can be minimized. To the best of our knowledge, this is the first
clear experimental evidence provided for the relative magnitude of the osmotic contribution to pore entry pressures for oil-base
muds.
Effect of Shale Water Activity
The results reported thus far have focused on the shale with aw = 0.96. Similar results were obtained with the shale with
the water activity of 0.86. Fig. 36 shows the pore entry pressures for both the aw of 0.86 and 0.96. As might be expected, the
oil breakthrough pressure for the shale with lower aw is significantly higher than for the higher aw shale, because the pore sizes
are smaller.
An increasing trend in oil breakthrough pressure with emulsifier concentration is observed in both shales. Smaller pore
entry diameters are calculated for the shale with aw = 0.86, as compared to the shale with aw = 0.96, as shown in Fig. 38. This
is consistent with the loss in water content and the shrinkage of the shale when the shale was partially dehydrated in
desiccators.

18

SPE 116364

Breakthrough Pressure vs. Emulsifier Concentration

Comparison between shale aw = 0.96 and shale aw = 0.86
Muds 3,4 and 5
0.86 aw shale

0.96 aw shale

1000
Breakthrough P ressure (psig)

900
800
700
600
500
400
300
200
100
0
1.5%

2.0%

2.5%

3.0%

3.5%

4.0%

4.5%

5.0%

Emulsifier Concentration (%)

Fig. 36: Entrance Pressure comparison for shales altered to different water activity

Conclusions
The following conclusions are based on results obtained in this study for the Arco China shale:
1.

2.
3.
4.
5.
6.
7.

The pore entry pressures measured for shales are controlled both by capillary pressure (pore size, interfacial tension)
and the rigidity of the oil-water interface. The results obtained for surfactant laden interfaces show that a more rigid
oil-water interface, created by the addition of surfactant, results in higher oil breakthrough pressures, even when the
interfacial tension is lower.
Higher emulsifier concentrations in the base oil result in larger entry pressures, as a result of the increase in rigidity of
the oil-water interface.
The presence of water droplets in the OBM increases the pore entry pressures because the water droplets form a filter
cake and provide an additional resistance to the entry of oil filtrate into the shale.
Increasing water content and decreasing emulsifier concentration result in lower pore entry pressures.
The Arco China shale samples that have a smaller pore size have substantially higher pore entry pressures.
The osmotic pressure generated between the brine droplets in the oil-based mud and the pore fluid in the shale plays a
significant role in controlling the pore entry pressures.
OBMs should clearly contain 1) sufficient emulsifier to provide small droplet size and mechanical rigidity of the oilwater interface, and 2) a high concentration of calcium chloride in the water phase in order to take advantage of
osmotic gradients. These factors will cumulatively result in high pore entry pressures, resulting in minimum invasion
of oil and water filtrate into the shale.

SPE 116364

19

Nomenclature
= water activity
aw

= contact angle

= interfacial tension, dynes/cm

= porosity
CEC = cation exchange capacity
HTHP = high temperature high pressure
ES
= electrical stability (volts)
RPM = revolutions per minute
PPM = parts per million
Pc
= capaillary pressure (dynes)
EC
= emulsifier concentration

References
Adkins, J.E. and Rivlin, R.S., Large Elastic Deformations of Isotropic Materials, Faraday Laboratory of the Royal Institution, September
18, 1951.
Al-Bazali, T.M., Zhang, J., Chenevert, M.E., and Sharma, M.M., Measurement of the Sealing Capacity of Shale Cap-rocks, SPE 96100,
Presented at the SPE Annual Technical Conference and Exhibition held in Dallas, TX, 9 12 October, 2005.
Al-Bazali, T.M., Experimental Study of the Membrane Behavior of Shale during interaction with Water-Based and Oil-Based Muds,
Dissertation presented to the Faculty of the Graduate School of The University of Texas at Austin, Austin, Texas, May, 2005.
Chenevert, M.E., and Sharma, A.K., Permeability and Effective Pore Pressure of Shales, SPE 21928, Presented at the SPE/IADC Drilling
Conference in Amsterdam, 11 14, 1991.
Chenevert, M.E., Shale Alteration by Water Adsorption, SPE 2401, Presented at the SPE Fourth Conference on Drilling and Rock
Mechanics held in Austin, TX, 14 15 January, 1969.
Chenevert, M.E., Shale Control with Balanced-Activity Oil-Continuous Muds, SPE 2559, Journal of Petroleum Technology, 1970.
Growcock, F.B., Ellis, C.F., and Schmidt, D.D., Electrical Stability, Emulsion Stability, and Wettability of Invert Oil-Based Muds,SPE
20435, SPE Drilling and Completion, March, 1994.
Manohar, L., Shale Stability: Drilling Fluid Interaction and Shale Strength, SPE 54356, Presented at the SPE Latin American and
Caribbean Petroleum Engineering Conference held in Caracas, Venezuela, 21 23 April, 1999.
Schlemmer, R., Friedheim, J.E., and Growcock, F.B., Membrane Efficiency in Shale An Empirical Evaluation of Drilling Fluid
Chemistries and Implications for Fluid Design, SPE/IADC 74557, Presented at the SPE/IADC Drilling Conference held in Dallas, TX,
26 28 February, 2002.
Simpson, J.P., A New Approach to Oil-Base Muds for Lower-Cost Drilling, SPE 7500, Presented at the SPE/AIME 53rd Annual Fall
Technical Conference and Exhibition held in Houston, TX, 1 3 October, 1978.