IPTC-18377-MS

Mitigating Shale Drilling Problems through Comprehensive Understanding

of Shale Formations
Mohammed K. Al-Arfaj, Abdulazeez Abdulraheem, and Abdullah Sultan, King Fahd University of Petroleum &
Minerals; Md. Amanullah, Saudi Aramco; Ibnelwaleed Hussein, Qatar University

Copyright 2015, International Petroleum Technology Conference

This paper was prepared for presentation at the International Petroleum Technology Conference held in Doha, Qatar, 6 –9 December 2015.

This paper was selected for presentation by an IPTC Programme Committee following review of information contained in an abstract submitted by the author(s).
Contents of the paper, as presented, have not been reviewed by the International Petroleum Technology Conference and are subject to correction by the author(s).
The material, as presented, does not necessarily reflect any position of the International Petroleum Technology Conference, its officers, or members. Papers
presented at IPTC are subject to publication review by Sponsor Society Committees of IPTC. Electronic reproduction, distribution, or storage of any part of this paper
for commercial purposes without the written consent of the International Petroleum Technology Conference 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 where and by whom the paper
was presented. Write Librarian, IPTC, P.O. Box 833836, Richardson, TX 75083-3836, U.S.A., fax ⫹1-972-952-9435

Abstract
In order to develop an inhibitive water-based mud capable of mitigating the adverse effects of shale-mud
interactions, it is important to characterize the shale sample in terms of its geological structure,
mineralogical composition, reactivity potential, etc. Further, the shale-mud interactions should be studied
through a series of experimental tests such as swelling, dispersion and inhibition durability.
This paper presents the results of characterization and testing of one of the studied shale samples with
X-ray diffraction, micro-CT, ultrasonic rock mechanics testing, capillary suction time and cation exchange
capacity. The paper also shows how petrophysics data of shale formations can be utilized to improve and
optimize drilling practices in order to achieve the ultimate goal of enhanced wellbore stability. Depending
on clay content, different shale formations have different responses when exposed to drilling fluids. It is
therefore very important to characterize the shale formation to develop the appropriate drilling fluid.
The tested shale sample was found to be a silica-rich shale with a small percentage of clay minerals,
mainly kaolinite. Characterization scheme included also Micro-CT where the images revealed the
heterogeniety and fractures in the internal matrix. Dynamic elastic moduli were determined using
ultrasonic rock mechanics testing. A cation exchange capacity (CEC) value of 2.5 meq and capillary
suction time (CST) value of 42.6 seconds indicated low tendency of the shale rock to both swelling and
dispersion.

Introduction
Drilling stable boreholes in shale formations can be a very challenging task when water-based drilling
fluids are to be used. The interactions between water phase in drilling fluids with shale rocks cause
different drilling problems such as shale swelling and dispersion. The extent to which a shale sample
swells or disperses depends on the clay content of the shale. Some types of clay have more swelling
tendency while others have more dispersion tendency. Therefore, identifying the type of clay present in
a shale rock is very important to develop drilling fluids capable of mitigating shale drilling problems.
2 IPTC-18377-MS

Because of the environmental regulations and continues efforts to reduce well construction costs,
different operators have been shifting from oil-based muds to inhibitive water-based muds to drill shale
formations with variable rate of success. For inhibitive water-based muds, different shale inhibitors have
been used to inhibit and stabilize the shale against swelling and dispersion. To optimize the shale inhibitor
selection, shale characterization should be carried out which includes but not limited to: mineralogy
determination, potential for hydration and swelling, pore structure study and membrane efficiency
estimation. This is the reason why various authors highlighted the importance of shale characterization to
provide a viable solution to eliminate shale-drilling fluid interactions or mitigate the severity of shale-
drilling mud interactions. (Chenevert 1970, Simpson et al. 1998, Amanullah 2013)
This paper introduces part of the characterization scheme carried out on one of the tested shale samples
to study its mineralogy, petrophysics, presence of fractures, ultrasonic test response, pore space and
reactivity.

X-Ray Diffraction
X-ray diffraction is the most frequently and widely used technique used to study clay minerals. In addition
to the application of this technique to determine clay mineralogy, it can be used to study clay swelling by
measuring the clay interlayer spacing. (Anderson, 2010)
In this study, powder method was used where a sample is prepared by crushing shale particles to a fine
powder then placing small amount on a sample holder. The sample holder is charged to the XRD
instrument and exposed to x-ray beam while being rotated through a range of angles. Minerals with
different crystalline structures have different responses to the beam. This will result in a pattern depending
on the minerals that are present in the sample. Different minerals have different peak positions and
intensities. (Stephens, 2009) Upon examination of the XRD pattern, qualitative, semi-quantitative and
quantitative analyses can be carried out using a minerals library of more than 500,000 entries to determine
clay mineralogy.
A qualitative XRD analysis was run for the shale sample. The XRD test was run for a start angle of
4° and stop angle of 80° to cover the whole range of expected minerals. The speed scan was set to 1 °/min
with step size of 0.02°. The voltage was set at 30 kV and current at 15 mA.

Figure 1—XRD results for the tested shale sample

IPTC-18377-MS 3

From qualitative analysis for the XRD pattern, the major peaks corresponds to quartz with minor peaks
in the range from 7 to 15 where clay peaks should appear. Therefore, this shale sample is classified as
silica-rich shale rather than clay-rich shale as it is the case in the remaining samples.

Spectral Gama Ray

Gama ray data, NMR and other types of logging tools are powerful tools to identify the clay mineralogy,
determine shale reactivity and predict the rock response when contacted by drilling fluids. Using
petrophysical properties to characterize shale can help determine the appropriate drilling fluid and shale
inhibitor to be used. Therefore, to optimize the shale inhibitor selection, shale characterization should be
carried out which includes but not limited to: mineralogy determination, potential for hydration and
swelling, pore structure study and membrane efficiency estimation.
The spectral gamma ray log is a tool to measure the natural gamma radiation of the main radio-isotopic
sources such as potassium, uranium and thorium. It is used to determine the proportion of the radiation
mainly coming from these three elements. The ratio of Th/K is utilized to identify clay mineralogy for
different shale formations. The abundance of thorium is measured in ppm while that for potassium is
measured in %. The results combined with cation exchange capacity and capillary suction time tests are
used to give indication about shale reactivity extent.
Lithology identification and differentiating between sandstone and shale formations using total gamma
ray log can be a challenging task because some sands give high total gamma ray readings. Spectral gamma
ray can help in differentiating both types of formations according to the percentages of the particular
radioactive minerals. Cross-plots such as those shown in Fig 2 and Fig 3 can be used for lithology
identification. (Glover)

Figure 2—Thorium/potassium cross-plot used to identify lithology (Macfarlane, 1988)

4 IPTC-18377-MS

Figure 3—Thorium to potassium ratio cross-plot used to identify lithology (Glover)

The cross-plot in Fig 2 can be used first to determine if the rock sample has high clay content. Then
the cross plot in Fig 3 can be used to have a more precise estimation about the clay types present although
the former cross-plot can be used to identify the clay types as well to some extent. As it is clear from Fig
3, as the ratio of Th/K increases, the rock sample is found to have more clay-type particles such as illite
and kaolinite.
Upon examination of the spectral gamma ray data carried out for the shale formation in this study, an
average value for both thorium and potassium abundances was taken starting from 10 feet above the exact
depth of the shale plug sample until 10 feet below that depth. The average value for thorium was 6.6 ppm
while that for potassium was 0.02 %. From the first cross-plot, that corresponds to the heavy thorium-
bearing minerals with high possibility to have kaolinite as well. For the second cross-plot and by
calculating the Th/K ratio as 330, although it was found to be of the range of the plot (logarithmic scale)
but it can be assumed to have high kaolinite content again.
As XRD pattern did not show high peaks for clay minerals, it can be confirmed from the first cross-plot
at least that this shale plug sample does not have high clay content. This outcome is to be examined also
by cation exchange capacity and capillary suction time tests.
Micro-CT
Micro Computed Tomography takes images of a sample by sections where x-rays are used to penetrate
the sample. After processing, 2-D or 3-D images can be generated after reconstruction of the sections
above each other to produce multi-dimensional representations of the rock sample. These representations
allow the study of the pore space and internal matrix of the sample and the fluid flow behavior. The field
of view and voxel for this technique are in the range of 10 to 0.5 micrometer. One main advantage of this
test is the non-destructive nature and, therefore, micro-CT is usually run prior to any other types of testing
such as rock mechanics or even XRD and SEM. Also, porosity estimations can be conducted using special
analysis software. This is useful when isolated and fine pores exist that are smaller than conventional
reservoir rock. This technique gives visualization of the pore network whether pore are connected or
isolated. It gives statistical analysis and estimates the percentage of each pore size in the rock matrix
excluding nano-pores as they can not be detected using Micro-CT.
The micro-CT system includes an X-ray source and detector, a high-precision revolving stage, a mount
for the rock specimen, a motor support, a mechanism for positioning the specimen, and a data acquisition
and analysis system. Using the X-rays transmitted by the sample, micro-CT produces images where the
darker regions are the regions that absorb more X-rays and the brighter regions are the regions that absorb
less X-rays. Several factors affect the absorption intensity including material density, thickness and also
IPTC-18377-MS 5

atomic number. The test is run under atmospheric pressure while the temperature is set as required.
Mechanical forces can be subjected to the sample while imaging to simulate real operating conditions.
This is due to the fact that there is not effect of electric or magnetic field on the X-rays. (Manual)
CT works by measuring the linear attenuation coefficient. It is defined by Beer’s law as a measure of
the fraction of X-rays passing through the sample. It is primarily dependent on effective atomic number
at low energies while at high energies it is a function of bulk electron density. (Boruah, 2015) The distance
ratio of the X-ray source and the sample to that of X-ray source to the camera was adjusted for image
acquisition.
In this study, micro-CT is used to fully characterize the shale sample and understand its pore structure
and heterogeneity and if there exist any fractures or other features. The main components of the micro-CT
machine include the X-ray source that generate X-rays of a range varying from 30 to 160 kV to produce
sample images and create reference images with X-ray source filter holder. The second main component
is the sample stage which is a platform to mount the sample upon in a sample holder and make it ready
for microscopy. The third main component is the detector assembly that picks up the X-ray images of the
sample. Another component is the visual light camera that produces and provides images to the visual
light camera window. It is located behind the sample stage and used for positioning the sample, detector
and X-ray source.
The analysis was carried out on the full plug sample whose height is 3 in and diameter is 1.5 in. The
x-ray source used 80 kV/ 7 W with exposure time of 1 second and 1601 projections. For the image
acquisition process, the ratio of the distance between the sample and the camera was adjusted. Slices of
2D images are generated. Then the slices were processed to reconstruct the 3D tomogram image. A filter
was used to reduce noise before segmentation. Processing the images requires differentiating between
pores, matrix, organic content and minerals using CT numbers. Every component has a range and
differentiated in the image using different colors. (Boruah, 2015)
Fig 4 shows cross-sectional and side views of the tested shale sample. The internal structure of the
shale sample was heterogeneous with different minerals. Two parts can be seen in the images: black where
the kerogen content is high and a lighter part where kerogen content is low. Fractures and micro-fractures
exist clearly in the structure. Some of the fracture appear to be filled with some material such as calcite.
Pores were identified in different types: microfractures, within the grains and between the grains.

Figure 4 —Micro-CT images for the tested shale sample

6 IPTC-18377-MS

Ultrasonic Testing
Geomechanics plays a vital role in drilling through shale formations. In addition to the impact of clay
content on the chemical properties of the shale rock, the rock mechanics aspects also affect rock behavior
as represented by compressive strength and elastic moduli. Dynamic moduli are evaluated through
ultrasonic testing, a non-destructive approach for studying the physics of the rock and its response to wave
propagation. Pores, grains and clay particles have different responses to sonic waves and based on that,
lithology identification study can be conducted on the rock. Different parameters have impact on
ultrasonic measurements including density, porosity, stresses, water content, temperature, mineralogy and
grain size.
The two main modes of propagation of acoustic waves in solid materials are compressional waves
(P-waves) and shear waves (S-waves). While the solid particles oscillate parallel to the direction of
propagation (in the longitudinal direction) in the case of P-waves, the oscillations are at right angle to the
direction of propagation in the case of S-waves and therefore these waves are called transverse waves. The
velocities of the two types of waves are controlled by two moduli: bulk modulus for P-waves and shear
elasticity for S-waves.
While mechanical testing such as triaxial compressive test gives the static Young’s modulus and
Poisson’s ratio, ultrasonic testing gives the dynamic moduli and the velocities of the waves through the
rock. As wellbore stability studies require the use of static moduli, dynamic moduli can be converted to
static using published correlations. Further, the wave velocities can be used to help in identifying
lithology, estimate porosity and to help in the identification of compaction and over-pressured zones. As
a result, rock quality can be assessed and cracks and defects can be identified. (Soroush, 2011)
The basic components of the ultrasonic test machine include hydraulic pumps, pressure intensifiers for
pressurizing confining chamber and axial chamber, core holder for acoustic velocity measurements and
data acquisition system. Three types for modes of operation for velocity measurement are available: pulse
echo, through transmission and pitch catch. This study used the first mode in which a transducer switches
from active to passive mode to measure the reflections within a material. In ultrasonic test, the rock sample
is placed between three wave transmitters: one for P-waves and two for S-waves and three receivers: one
for P-waves and two for S-waves. A wide-band acoustic signal is sent by the transmitter into the sample
from one end. The signal propagates through the sample until it is picked up by the receiver at the other
end. The time taken by P and S waves to travel through the sample can be measured and waves velocities
can be calculated since the distance between transmitters and corresponding receivers is known (Gao,
2015). To assess rock anisotropy, wave velocities parallel and perpendicular to bedding plane were
measured.
Several parameters have impact on the wave velocity and anisotropy in shale rocks. These parameters
include stress state, stress history, smectite content, organic content, microstructure and physico-chemical
interactions with pore fluids before drilling and with drilling fluids while drilling. Laboratory experiments
under controlled conditions can help in estimating the effects of these parameters. (Dodds, 2007)
Table 1 summarizes the ultrasonic results along with the conditions used to run the test. Three
waveforms were produced, one for P-waves and two for S-waves. The first arrivals of the waves were
recorded and analyzed to calculate the values of dynamic Young’s modulus and Poisson’s ratio.
IPTC-18377-MS 7

Table 1—Results for ultrasonic testing with different confining pressures

Cation Exchange Capacity (CEC)

Cation exchange capacity test (CEC) was conducted to determine the reactivity of the shale sample
through measuring the exchangeable cations. Since shale layers are negatively charged, they need to have
cations such as sodium, potassium or calcium to be neutral in charge. The tendency of the shale to
exchange those cations can give indication on the shale reactivity. Higher CEC values indicate higher
shale reactivity.
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 10 ml of de-ionized water, 15 ml Hydrogen Peroxide and 1 ml
sulfuric acid (5N). 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 and one drop is transferred from the solution with a
stirring rod and placed on a filter paper. When dye appeared as a faint blue ring, the titration end point
was reached.
For the tested shale sample, the end point reached at 2.5 mL which is equal to 2.5 milliequivalents per
100 g of clay, Fig 5. Every drop on the filter paper is a 0.5 mL increment and the faint blue ring developed
completely at the fifth drop. This indicated a low tendency to cation exchange capacity and, in turn, low
tendency to swelling. This low CEC result can indicate the low smectite content of this shale sample and,
on the other hand, high kaolinite content in the clay fraction.

Figure 5—Cation Exchange Capacity test results showing the end point
8 IPTC-18377-MS

Capillary Suction Time (CST)

While CEC test can be used as a measure of the tendency of the shale sample to swelling due to the cation
exchange process, capillary suction time can be used as a measure of the tendency to dispersion, i.e.,
disintegration. Several factors affect the dispersion process including the stresses around the borehole,
degree of hydration, shale composition, annular velocity and brittleness degree of the shale rock. In
general, brittle rocks have more tendency to dispersion than ductile rocks. (Bol, 1986) In this test, capillary
suction time determine the rate of water release from the slurry. Long suction time is indicative of the high
tendency to dispersion since water is not released quickly from the solution so the shale particles tend to
disperse into water.
In this study, CST was conducted to determine the tendency of the shale sample for clay dispersion.
The CST apparatus, Fig 6, was assembled by placing test blotter paper on top of the sensory trays. Then,
the sensor plates were placed on top of the test blotter paper with the probe side down touching the blotter
paper. After that, the stainless steel funnel was placed into the sensor plate. An amount of 3 grams of
crushed shale sample was mixed for 5 minutes in an Erlenmeyer flask with 75 ml of de-ionized water. The
mixing speed was fast enough to have a vortex to ensure good blending so shale particles were kept
suspended in the fluid. After mixing, an amount of 5 mL of the slurry was transferred and injected into
the stainless steel funnel. The filtrate of the slurry started to move and spread on the blotter paper. The
timer of the apparatus was triggered when the filtrate reached to the first circle (probe). This was the start
of the testing time. The timer stopped when the filtrate arrived at the second circle (probe) where the test
finished and the time measured was taken as the time for the slurry filtrate to travel a measured distance
at pre-determined conditions.

Figure 6 —Capillary Suction Test Apparatus

CST test was conducted twice on the same shale sample with de-ionized water. The average of the two
time results was 42.6 seconds. According to Wilcox and Fisk (1983) classification, capillary suction time
of less than 300 seconds is classified as low tendency to dispersion.
Conclusion
This paper presented part of the characterization carried out for one of the shale samples to be tested in
this study. The shale sample was looked at and tested using six different elements: XRD, spectral gamma
ray data, micro-CT, ultrasonic rock mechanical testing, cation exchange capacity and capillary suction
time. These tests were conducted to find: shale mineralogy, clay content, internal matrix, dynamic
elasticity moduli, tendency to swelling and tendency to dispersion. Results can be summarized as the
following:
IPTC-18377-MS 9

– XRD results showed silica-rich shale with minor peaks in the 2-theta range of clay minerals
– That small percentage of clay content was found using spectral gamma ray data and cross plots to
have kaolinite as the main clay type present.
– Micro-CT results indicated heterogeneity and the presence of fractures and micro-fractures within
the rock matrix.
– Ultrasonic testing results yielded dynamic Young Modulus in the range of 47-55 GPa and dynamic
Poisson’s ratio in the range of 0.073-0.103 for confining pressures ranging from 5 to 25 MPa.
– CEC test results showed low tendency to cation exchange and therefore low tendency to swelling
as CEC value was found to be 2.5 meq.
– CST test results indicated low tendency to dispersion as CST value was found to be 42.6 seconds.

Acknowledgement
The authors would like to acknowledge the support provided by: Saudi Aramco EXPEC ARC Drilling
Technology laboratory, Baker Hughes laboratories at Dhahran TechnoValley and Halliburton laboratories
at Dhahran TechoValley.

References
1. Amanullah, Md., Dendrimers and Dendritic polymers- Application for superior and intelligent
fluid development for oil and gas field applications. Paper SPE 164162 prepared for presentation
at the Middle East Oil and Gas Show & Conf, Manama, Bahrain, 10-13 March, 2013.
2. Anderson, R., Ratcliffe, I., Greenwell, H, Williams, P, Cliffe, S, Coveney, P, Clay Swelling – A
Challenge in the Oilfield, Earch-Science Reviews 98 (2010) 201–216.
3. Boruah, A., Ganapathi, S.; Microstructure and pore system analysis of Barren Measures Shale of
Raniganj field, India, Journal of Natural Gas Science and Engineering, 26 (2015) 427–437.
4. Chenevert, M. E: ⬙Shale Control with Balanced-Activity Oil- Continuous Muds⬙, Journal of
Petroleum Technology, October 1970, pp 1309 –1316.
5. Dewhurst, D., Sarout, J., Piane, C., Siggins, A., Raven, M., Empirical strength prediction for
preserved shales, Marine and Petroleum Geology, 67 (2015) 512–525.
6. Dodds, K., Dewhurst, D., Siggins, A., Ciz, R., Urosevic, M., Gurevich, B., Sherlock, D.,
Experimental and theoretical rock physics research with application to reservoirs, seals and fluid
processes, Journal of Petroleum Science and Engineering 57 (2007) 16 –36.
7. Gao, Q., Tao, J., Hu, J., Yu, X., Laboratory study on the mechanical behaviors of an anisotropic
shale rock, Journal of Rock Mechanics and Geotechnical Engineering, 7 (2015) 213–219.
8. Glover, P. W.; Petrophysics MSc Course Notes, Rock Physics and Rock Meachanics, Department
of Geology and Petroleum Geology, University of Aberdeen.
9. Macfarlane, P., Townsend, M., Whittemore, D., Doveton, J., Staton, M., Hydrogeology and water
chemistry of the Great Plains (Dakota, Kiowa, and Cheyenne) and Cedar Hills Aquifers in Central
Kansas, Kansas Geological Survey, Dakota Project, Original document dated December 1988,
Electronic version placed online April 1996, Website link: http://www.kgs.ku.edu/Dakota/vol3/
KCC/kcc06.htm, date of access: October 3rd, 2015.
10. Simpson, J.P., Walker, T.O., and Alaskson, J.K.: ⬙Studies Dispel Myths, Give Guidance on
Formulation of Drilling Fluids for Shale Stability⬙, IADC/SPE 39736 Presented at the 1998
IADC/SPE Drilling Conference held in Dallas, Texas, 3-6 March 1998.
11. Soroush, H, Qutob, H., Evaluation of rock properties using ultrasonic pulse technique and
correlating static to dynamic elastic constants, Paper prepared for presentation in the 2nd South
Asian Geoscience Conference and Exhibition, GEOIndia, 2011, Jan 12-14.
10 IPTC-18377-MS

12. Stephens, M., Gomez, S., and Churan, M.; Laboratory Methods to Assess Shale Reactivity with
Drilling Fluids, AADE 2009-NTCE-11-04, National Technical Conference & Exhibition, New
Orleans, Louisiana.
13. Wilcox, R., Fisk, J., Mathematical Model Aids in Analyzing and Classifying Shales, paper SPE
11813, 1983.