IPTC-17800-MS

Preliminary Test Results of Inhibitive Water-Based Muds Used to Mitigate

Unconventional Shale Drilling Problems
Mohammed K. Al-Arfaj, Saudi Aramco; Enamul Hossain,
and Abdullah Sultan, King Fahd University of Petroleum & Minerals Md. Amanullah, Omar Al-Fuwaires,
and Turki Al-Subai, Saudi Aramco

Copyright 2014, International Petroleum Technology Conference

This paper was prepared for presentation at the International Petroleum Technology Conference held in Kuala Lumpur, Malaysia, 10 12 December 2014.

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Abstract
Unconventional resources include oil and gas present in shale, tight sandstone and tight limestone
formations. Shale oil can be produced from deposits of shale with estimates of about 5 trillion barrels of
oil in place around the world. Because of the high content of clay in the shale formations, water-based
drilling fluids tend to cause wellbore instability problems when drilling this type of formations. When it
comes in contact with water, clay starts to react, swell and/or disperse leading to shale disintegration and
sloughing. As a result of shale sloughing down into the borehole, cleaning efficiency of drilling fluids
decreases significantly. Moreover, tight hole problem is expected which may cause drillpipe to get stuck
and, as a result, increases non-productive time and well construction cost.
Several types of shale inhibitive drilling fluids were developed using different shale inhibitors and
stabilizers. Developing an inhibitive drilling fluid with long-term inhibition can eliminate the need for
unnecessary casing and reduce tripping time. Multiple formations including the shale formation can be
drilled and cased in one hole section.
This paper summarizes preliminary laboratory testing results for characterizing one shale sample and
assessing the interactions with different water-based mud systems. Shale characterization included
determination of mineralogical composition using X-ray diffraction and determination of cation exchange
capacity (CEC) while shale-mud interactions evaluation included swelling, dispersion and inhibition
durability tests.

Introduction
Unconventional resources refer to any petroleum resource that can not be recovered and produced using
conventional methods. Examples include: shale gas, tight gas and shale oil. These resources exist in shale
and tight sandstone formations with very low permeability. Therefore, hydraulic fracturing is usually
necessary to produce at economic rates.
Shales represent a large portion of the unconventional resources in Saudi Arabia. While conventional
shale formations are the source rock for oil and gas, unconventional shale formations are the source rock
2 IPTC-17800-MS

and the reservoir at the same time. The well is drilled and completed into the shale zone. Since
conventional water-based mud systems (WBMs) cause shale instability, there is a need to develop
inhibitive water-based muds that provide the required long-term shale inhibition especially when drilling
development wells horizontally through shale formations to exploit unconventional resources. Although
drilling with oil-based drilling fluids can provide better shale inhibition, higher penetration rates and good
lubricity, the environmental regulations and the high cost of such fluids make it difficult to justify the
decision to drill long horizontal shale sections with these fluids.
Shale formations are characterized based on clay content and composition. Clay minerals are grouped
mainly into five groups: kaolinite, smectite, illite, chlorite and vermiculite. Previous experimental work
showed that smectite group has the highest reactivity and sensitivity to water compared to the other groups
from swelling point of view. Because the degree of reactivity depends on the shale composition and, also,
shale composition differs from one area to another, it is necessary to do shale characterization before an
inhibitive drilling fluid is recommended for a certain shale formation. Shale characterization includes
determining the clay content and reactivity as well as determining the water activity of the shale sample.
Chenevert (1970) conducted a laboratory work utilizing the drilled cuttings to measure the water activity
of different shales based on the adsorption characteristics. Isotherms for adsorption and desorption were
established after drying and placing shale drilled cuttings in a desiccator and allowing them to reach
equilibrium. Based on the isotherms and the weight percentage of water in the shale, a scale from 0.1 to
1.0 was suggested for the water activity.
Shale swelling can be defined as the increase in shale volume when exposed and hydrated by water.
Hydration is an equilibrium process which depends on parameters such as shale composition, fluid
composition, pressure and temperature. Since pressure is the only varying property while drilling a well,
it controls the equilibrium water content of the shale. Roehl and Hackett (1982) described three
mechanisms of swelling: surface hydration, ionic hydration and osmotic hydration. Surface hydration
usually occurs in clays with low CEC such as illite. Although illite has relatively a large number of
compensating ions, it does not show high tendency to swelling. This is because the cations substitution
takes place in the outer tetrahedral layer. Therefore, they are more difficult to exchange due to their
interactions and attractive forces to the negative charges of the clay. The second mechanism is the ionic
hydration where hydration shells are formed around the compensating ions that contribute to the lattice
substitutions in the clay structure. The factors controlling this mechanism include the concentration,
location and types of compensating ions. This mechanism only occurs in clay types of high CEC values.
The third mechanism is the osmotic hydration that is basically due to the difference in salinity of the shale
rock fluid and the drilling fluid. If the salinity of the drilling fluid is lower than that of the shale rock fluid,
water tends to move and diffuse into the shale rock and hydrate shale particles. The absorption of water
causes the shale to behave as two layers with repulsive potential leading to the expansion of the clay
matrix.
Shale dispersion is the erosion and disintegration of shale cuttings. Dispersion depends on the stresses
around the borehole, degree of hydration, shale composition, annular velocity and brittleness degree of the
shale rock. Rocks behave in brittle mode are prone to disintegration more than ductile rocks. Also, the
sedimentation history and the heterogeneity of the shale rock can play an important role. (Bol, 1986).
Different proactive and reactive solutions to mitigate shale reactivity problems have been identified and
used in the field. One solution is to increase the weight of the drilling fluid to mechanically stabilize
shales. However, excessive increases in the weight of the drilling fluid result in decreasing the penetration
rate and increasing the drilling costs. Another solution to retard shale inhibition is to reduce fluid loss.
Reducing fluid loss minimizes the water invading the formation and, as a result, minimizes shale contact
with water. Also, several salts such as KCl were used to minimize shale swelling. Although they can
provide good shale inhibition, they have the disadvantages of causing corrosion to the pipe and the
difficulty to dispose of waste due to high salt content. (Myers, 1993, Stephens et. al., 2013)
IPTC-17800-MS 3

In literature, there are several mechanisms by Table 1Mineralogical composition of the shale sample

which shale inhibition can be achieved. One mech- Compound Percentage

anism is to reverse the osmosis phenomenon by Kaolinite-Al2Si2O5(OH)4 57
adding salts to the drilling fluid such as KCl. In the Quartz-SiO2 23
osmosis theory, the electrical field around the clay Muscovite 8.9
particle acts as a semi-permeable membrane and MicroclineKAISi3O8 3.8
Goethite-FeOOH 1.2
water in the drilling fluid tends to pass the mem- Gibbsite-Al(OH)3 0.7
brane into the clay matrix and hydrate it. Adding Illite Mixed Layers I-S 5.4
salt to the drilling fluid makes it more concentrated
with ions and, now, water from the clay matrix
flows in the opposite direction, i.e. from clay to Table 2Mineralogical composition of the clay fraction of the shale
drilling fluid. This hinders the contact and hydration sample
of clay particles with water and provides inhibition. Element/Compound Percentage
(Al-Arfaj and Amanullah, 2014) Another shale in- Illite 6
hibition mechanism is by reducing the porosity and Illite-Smectite 15
permeability to drilling fluid filtrate. Sodium and Kaolinite 79
potassium silicate fluid have the ability to physi- Clay Size 25
% of Smectite in Illite-Smectite 70
cally plug the shale pores through a process of
polymerization and precipitation. They also
strengthen the shale formation through cementing
the grain contacts by precipitate. Furthermore, this porosity and permeability reduction can even facilitate
the first mechanism and enhance the osmotic effect. Therefore, silicates can work effectively by these two
mechanisms to provide the required shale inhibition (Bailey et. al., 1998).
In this study, chemical aspects of the shale swelling and dispersion problems are discussed. One
outcrop shale sample representing one of the most frequently encountered shale types is characterized
based on x-ray diffraction and cation exchange capacity (CEC). Swelling, dispersion and inhibition
durability tests were carried out to thoroughly understand the fluid-rock interactions when drilling this
shale formation with water-based muds. Based on this study, inhibitive water-based muds with short-term
and long-term inhibition can be identified or developed.
Shale Mineralogical Analysis
The mineralogical composition can be determined using different techniques such as x-ray and NMR.
Shale sample used in this study was taken from outcrop and analyzed in x-ray laboratory to determine the
mineralogical composition in order to assess the degree of shale reactivity. Table 1 shows the mineral-
ogical composition of the shale sample while table 2 shows the clay size fraction and the percentage of
Smectite in the illite-smectite mixed layer.
The x-ray results show that the shale sample is more prone to dispersion than to swelling since the
percentage of Kaolinite (57%) is much greater than the percentage of the illite-smectite. Since the
percentage of smectite in particular is less than 70% of the 5.4% that represent illite-smectite mixed layers,
no significant swelling is expected for this type of shale with this mineralogical composition.
Cation Exchange Capacity Test
Cation exchange capacity test (CEC) was conducted to determine the reactivity of the shale sample. One
gram of the shale sample was ground to a particle size of less than 75 microns. Then, the sample was
mixed in an Erlenmeyer flask with 25 ml of 2% tetrasodium pyrophosphate. The sample was boiled gently
for 10 minutes. After that, it was cooled down to room temperature and diluted with water to a volume
of 50 ml. Titration started by adding methylene blue solution in increments of 0.5 ml while being stirred
with a magnetic stirrer. The flask contents are swirled after each addition of the methylene blue solution
4 IPTC-17800-MS

Figure 1X-ray pattern for the bulk shale sample and clay size fraction analysis

Table 3Inhibitive-Mud1
Material Unit Amount

Water bbl 0.796

Viscosifier-1 lb 5
Viscosifier-2 lb 0.875
Fluid Loss Additive-1 lb 4.5
Fluid Loss Additive-2 lb 1.5
Salt lb 25
pH controller-1 lb 0.25
pH controller-2 lb 0.25
Oxygen Scavenger lb 0.3
Figure 2The end point of titration for CEC test Shale Inhibitor lb 3

and one drop is taken from the solution with a Table 4 Inhibitive-Mud2

stirring rod and placed on a filter paper. When dye Material Unit Amount
appeared as a faint blue ring, the titration end point Water bbl 0.78
was reached. pH controller lb 0.25
The CEC value was determined to be 26 meq/ Fluid loss additive bbl 3.5
100 g. This high value of CEC indicated the high Viscosifier gal 0.6
Salt lb 25
reactivity of this shale sample. The CEC value can Shale Inhibitor lb 3
measure the amount of positively charged ions that
are present in the shale sample to neutralize the
negatively charged clay particles (Stephens et. al.,
2009). These positive ions are readily exchangeable
upon contact with water and eventually cause the
shale to react and swell.
Mud Formulations
Two different types of drilling fluids were tested to
evaluate shale swelling, dispersion and inhibition
durability. Tables 3 and 4 give the formulation for
each type of drilling fluid. Figure 3Shale swelling test apparatus
IPTC-17800-MS 5

Figure 4 Shale plug before (left) and after (right) swelling test

Figure 5Shale swelling test results with both inhibitive muds

Shale Swelling Test

Shale swelling is a major problem encountered frequently when drilling shale formation with water-based
muds. When a shale formation with high smectite content comes in contact with water, it starts to swell
and expands. This may lead to two types of rock failure: soft swollen shale when interactions are strong
and heaving shale when interactions are low to moderate. (Darley, 1969)
The shale sample in this study was tested for shale swelling test to evaluate its reactivity in the presence
of fresh water and the two inhibitive muds. This test also can assess the inhibition quality provided by the
drilling fluid being tested. It helps in evaluating and ranking different inhibitive drilling fluids in order of
their capability to inhibit clay-rich formations. In theory, as the percentage of smectite and mixed-layer
clays increases, the swelling percentage should increase as well. Therefore, swelling test gives indication
about the chemical interaction, i.e. hydration of clay particles when exposed to water. This test is carried
out using the linear swelling tester. The shale sample is crushed then a pellet of the crushed sample was
reconstituted using special equipment. The apparatus to measure the linear swelling of the shale pellet is
shown in fig 3 while fig 4 shows the pellet before and after being tested for swelling using one of the
inhibive mud systems. Unlike some other types of apparatus that measure the diameter increase of
uncontained shale sample, this apparatus measures the increase in length, i.e. thickness, of a contained
shale sample where the diameter is kept constant. Fig 5 shows that after 66.5 hours, the shale pellet
volume increase stabilized at 33% when inhibitive-mud1 was used compared with 36% when inhibitive-
mud2 was used. This indicates that inhibitive-mud1 performed a little bit better than the other mud in
terms of shale inhibition against swelling.
6 IPTC-17800-MS

Figure 6 Cuttings recovery (%) in shale dispersion test

Shale Dispersion Test

Dispersion test was conducted to measure the disintegration tendency of the shale sample in the presence
of fresh water and the two inhibitive muds. 10 grams of the shale sample with particle size of 4 8 mm
were mixed with each type of fluid and hot-rolled at 150 F for 16 hours. After that, the shale cuttings were
recovered on a 500-micron sieve, washed, dried for 24 hours at 105 C and then weighted. Shale recovery
percentage was determined as the ratio of the recovered shale cuttings weight after dispersion to the
original cuttings weight of 10 grams.
Dispersion with water was tested to represent the worst case scenario, to assess the shale tendency to
dispersion and to compare the behavior of the shale sample in the presence of water and other inhibitive
water-based muds. The results showed high dispersion tendency with fresh water, i.e. about 96% of the
samples was dispersed. This agrees with theory since the sample has high Kaolinite content (57%). Shale
samples with high Kaolinite content should have high dispersion tendency.
While shale recovery percentage for inhibitive-mud1 was about 85% shale recovery, inhibitive-mud2
gave moderate inhibition to dispersion with about 52% shale recovery. This indicates that the former is
a good inhibitive mud and does not require modifying the formulation. However, modification of
inhibitive-mud2 formulation should be considered if there is a need to use it to drill shale formations.
Modification can be done by adding some shale inhibitors or changing the type of the shale inhibitor if
one already exists.

Inhibition Durability Test

To test the inhibition durability of a drilling fluid, the standard dispersion test should be carried out first.
Then, the inhibited shale cuttings are placed into a hot-roll cell and mixed with water to simulate a reactive
environment (Al-Arfaj and Amanullah, 2014). The steps are as the following:
a. 350 ml inhibitive mud was prepared for each of the selected mud systems using standard test
equipment and procedure.
b. 4 8 mm shale cuttings were prepared using shale cores or outcrop shales. For this development
outcrop shale was used.
c. 10 g of shale cuttings were added to 350 ml inhibitive drilling fluid into the hot roll cell. The cap
was screwed tightly and the cell was then placed on the roller of the hot roll oven to be rolled at
150 F and 35 rpm for 16 hours in the first stage of the test method.
d. After 16 hours, the cell was removed from the hot roll oven and then the cell contents were poured
into a 500 micron sieve.
IPTC-17800-MS 7

Figure 7Inhibition durability test results for inhibitive-mud1

e. The content of the sieve was washed with mildly running water to remove all shale pieces smaller
than 500 microns.
f. The cuttings were dried in an oven at 105 C for 24 hours
g. The dried shale was weighted.
h. 350 ml fresh water was poured into the hot roll cell again to represent a highly reactive fluid
environment to test the inhibition durability.
i. An amount of 5 gm dried shale cuttings that were recovered previously in step f was placed into
the fresh water of the hot-roll cell.
j. The cell was placed in the rolling oven and hot-rolled at 150 F for periods from 1 to 9 hours using
several inhibited cuttings samples that were inhibited by the same inhibitive mud system.
k. After rolling for the designated time period, the content was poured into a 500 micron sieve and
washed using mildly running water to remove all particles below 500 microns.
l. The weight was measured after drying at 105 C for 24 hours and then a plot of the mass recovered
as a function of rolling time was generated.
The inhibition durability test was conducted for the two inhibitive muds. Since this test requires 5
grams of inhibited shale cuttings to start with, it can be conducted only for those types of muds that are
able to inhibit the shale cuttings and give shale cuttings recovery of 5 grams or more in the dispersion test.
Therefore, this test can not be run for fresh water since the shale recovery in the dispersion test was less
than 1 gram.
Fig 7 and fig 8 show the results for inhibition durability of inhibitive-mud1 and inhibitive-mud2.
Although inhibitive-mud1 showed better results than inhibitive-mud2 in the dispersion test (85% com-
pared to 52%), it did not exhibit the same good performance for long-term inhibition testing. After only
3 hours, about 60% of the shale cuttings dispersed in water, i.e. only 2 grams were left out of 5 grams.
Figure 5 also shows that after maintaining the shale cuttings recovery at 2 grams for the period from 3
hours until 5 hours, it started to decrease gradually until it approached 1 gram after 9 hours. Figure 8
shows the inhibition durability results for inhibitive-mud2 where it was able to achieve long-term
inhibition. The figure shows clearly that the inhibition was more stable since only less than 20% of the
shale cuttings dispersed in water throughout the whole testing period. It maintained this good performance
although it did not achieve high inhibition in the dispersion test where only 52% of the shale cuttings were
recovered.
The results of this study clearly illustrate that although inhibitive-mud1 showed better performance in
inhibiting the shale sample against swelling and dispersion, this inhibition was not permanent. When the
results of inhibition durability test for the two inhibitive muds were compared, inhibitive-mud2 exhibited
8 IPTC-17800-MS

Figure 8 Inhibition durability test results for inhibitive-mud2

more inhibition stability and longevity. Therefore, if a repeated attack of a highly reactive drilling fluid
is anticipated while drilling this shale formation, it is crucial to provide long-term inhibition to the shale
to mitigate and avoid shale drilling problems.
Conclusions and Recommendations
1. Characterization of shale based on clay content, composition and reactivity is important to
understand its behavior when exposed to WBMs.
2. Development and assessment of inhibitive WBMs should consider the long-term as well as
short-term inhibition performance.
3. Inhibitive WBMs that perform well in inhibiting shale cuttings against dispersion do not,
necessarily, perform well in the swelling test or in the inhibition durability test.
4. Future work may include SEM analysis for the shale cuttings before and after dispersion and
swelling tests. Moreover, bulk hardness and fracture development tests might be carried out to
understand the mechanical behavior of the shale sample after being exposed to water.

Acknowledgement
The authors acknowledge the support from EXPEC Advanced Research Center management and Petro-
leum Engineering Department at KFUPM for their support and encouragement to carry out innovative
research and development activities and also for granting permission to publish this paper.

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IPTC-17800-MS 9

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