SPE-192290-MS

Shale-Fluid Sensitivity for an Unconventional Shale Formation

Raed Alouhali; Mohammed Al-Arfaj; Mohammed Al-Rashead; Shaun Hayton, Saudi Aramco

Copyright 2018, Society of Petroleum Engineers

This paper was prepared for presentation at the SPE Kingdom of Saudi Arabia Annual Technical Symposium and Exhibition held in Dammam, Saudi Arabia, 23–26
April 2018.

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
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Abstract
Shale instability is a major problem for drilling operation. Shales make up over 75% of drilled
formations and are responsible for 90% of wellbore instability problems. There are many problem
associated with shale drilling such as wellbore instability, cuttings dispersion, stuck pipe, and bit balling.
Shales used to be the problematic formations that needed to drill through with the minimum number of
problems, lowest possible lost time and generally the shortest possible open-hole time to minimize fluid
sensitivity issues. However, with the advancement in drilling and production techniques, some shale
formations are now the target for hydrocarbon production, meaning that much longer periods of open-hole
are required for horizontal drilling, logging and completion meaning fluid sensitivity is an increasingly
important question..
In this paper, we evaluate the shale-fluid sensitivity of a target unconventional shale formation. A total
of 20 samples from 6 different wells were used in this study. The mineralogy of all 20 samples were
analyzed using XRD. Then two shale-fluid sensitivity tests (dispersion test and capillary suction time test)
were run on the samples using four different water based fluids (7% KCl, 3% KCl, 3% NaCl, and 5%
NH4Cl) in addition to fresh water and diesel which were used to establish bounding parameters.
Overall, all inhibitors performed well, with 7% KCl and 3% KCl being the best performing inhibitors
for drilling shale formations of this composition followed by 5% NH4Cl and lastly 3% NaCl.

Introduction
Shale formations have three features that distinguish them from other formations in the oil industry.
They usually have low permeability, regardless of porosity, because of narrow pore throats, they have
high clay content, and they often have large coefficient thermal expansion difference between them and
water (Lal & Amoco, 1999).
Drilling through shale, especially reactive shale, is usually accompanied by several challenges. Stuck
pipe, caving, and cuttings dispersion are amongst the most common problems faced during shale drilling.
Drilling programs usually offer special sections for drilling through shale with specific drilling fluid
design and inhibitors. It will also include anticipated drilling problems that occurred at offset wells nearby
and how they treated it. But what worked for an offset well doesn’t necessarily mean it will work for all
other wells.
One approach to shale inhibition is by adding salts such as KCl to water based drilling fluid, this is
referred to as reverse osmosis. The theory behind it is when you add salt to the drilling fluid, it increases
the ions concentration of the drilling fluid. The semi-permeable membrane produced by the electrical field
SPE-192290-MS 2

around the clay particle now allows water from the clay to flow in the direction of the drilling fluid.
Contrarily, in fresh water system, the semi-permeable membrane would allow the water to flow from the
drilling fluid into the clay thus causing the clay particles to be activated and react with the drilling fluid
(Al-Arfaj, Hossain, & Amanullah, 2014). Another approach is to use non-aqueous fluids such as oil based
mud or synthetic oil while drilling shale sections. Non-aqueous systems are significantly more expensive
than aqueous systems and require very careful handling in mixing, circulating and disposal according to
the local environmental protection rules and regulations.
Clay mineral composition is considered a major factor in problems associated with shale. The
interaction of these clay minerals with the drilling fluid causes the undesirable change in the physical
properties of the shale formation. Smectite is the clay mineral causing most drilling problem followed by
illite (O’ Brien & Chenevert 1973). Swelling of smectite, specifically smectite saturated with sodium ions
has been proved to be a major source of shale instability problems (Anderson et al., 2010).

Methodology and Procedure

To evaluate the reactivity of the shale samples, two tests were used: capillary suction time test, and
dispersion test. These two tests are common methods to measure and compare the reactivity of shale
samples with different fluids. As for the mineralogy of the samples, XRD analysis was used to determine
the mineralogical composition of the sample. Below is a brief explanation about each test and test
procedure.
Capillary suction time (CST) test was originally used to test for water pollution control in the United
Kingdom. It was latter adapted by the oil and gas industry as a method for measuring the reactivity of
shale. The procedure for this test is straight forward. First grind the shale sample to 70-mesh then combine
5 g of the sample with 50 ml of the fluid being tested and mix them for 2 hrs. using a magnetic stirrer.
Place 5 ml of the resulting slurry in a cylindrical mold and measure the time taken for the fluid to wick
through paper. Repeat using non-reactive (blank) material. Then calculate the reactivity using
CSTratio = (CSTsample – CSTblank)/CSTblank
The higher the CSTratio, the higher the reactivity of the shale for example, CSTratio < 3 means low reactivity,
CSTratio between 3 and 5 means moderate reactivity, and CSTratio > 5 means high reactivity.
Shale dispersion test is another method to measure the reactivity of shale samples. It is very effective
in screening potential inhibitors to be used in drilling a shale section. One of the advantages of this test is
it doesn’t require core sample or plugs. It can be run using drilling cuttings collected from the well. For
the best result, cuttings recovered while drilling with non-aqueous fluid is preferred over sample collected
with aqueous fluid because the shale would have already reacted with the water in the aqueous drilling
fluid and the test result will be affected. The shale dispersion test is affected by many criteria such as the
rotation speed of the roller oven, the moisture content of the shale, the test temperature, the viscosity of
the test fluid, and the shale composition. Dispersion test is carried out using the specific drilling fluid with
a weighed quantity of shale sample. The fluid and shale are placed in a roller-oven cell where it is agitated
for 16-24 hours at a specified temperature. After cooling to room temperature, the fluid is poured over a
mesh size screen and the retained shale pieces are washed, weighed and dried overnight at 200°F. After
drying the samples are reweighed and with the post testing weight being compared to the weight of the
original sample to calculate the recovery percentage.
X-ray diffraction (XRD) analysis was used to obtain the mineralogy of the samples. XRD analysis is
based on Bragg’s law
𝜆 = 2𝑑 𝑠𝑖𝑛𝜃
SPE-192290-MS 3

Where λ is the wavelength of the X-ray beam, d is the distance between adjacent planes of atoms and θ is
the angle of incidence of the X-ray beam. XRD is used to identify unknown minerals by comparing the
diffraction patterns produced when powdered sample is irradiated by X-ray to known patterns of minerals
and then identifying the unknown minerals. Full core samples or cuttings can be used to run an XRD test.
To run the test, first, crush the sample via jaw crusher then pulverize it to a powder using shaker and
shatter box and split via cone and quartering to ensure a representative sample. The powdered sample is
placed into the sample holder and held in place with a glass slide. The sample is scanned from different
angles and the produced diffraction profile is then analyzed to semi-quantitatively identify the composition
of the sample. After that, the clay fractions were separated from the bulk powder sample using water
dispersion and analyzed by the XRD analyzer.

Results and Discussion

The overall recovery from the dispersion test results are shown in Table 1. For this test, 20 samples
from six different wells were tested using six different fluids: two grades of Potassium Chloride, Sodium
Chloride, Ammonium Chloride, freshwater, and diesel. Freshwater and diesel were used to benchmark the
shale reactivity of the samples. Shale tends to be extremely reactive when exposed to fresh water while
with diesel it shows least reactivity. Most reactive shale will swell and deteriorate in the presence of fresh
water whereas diesel is considered among the best inhibitors for reactive shales. The other four fluids are
7% KCl, 3% KCl, 3% NaCl, and 5% NH4Cl. These fluids are typically used as inhibitors in the drilling
operations. The test was conducted to evaluate the reactivity of shale to these fluids to help in the selection
of the best inhibitor for drilling shale sections with mineralogical compositions similar to those tested
here. As indicated in Table 1 (dark green best, dark red worst), 7% KCl and 3% KCl consistently show
the highest recovery where as 3% NaCl and 5% NH4Cl have the lowest. This is illustrated in figures (1-
6) for samples one to six respectively.

Table 1 Dispersion test results

Recovery %
Sample 7% KCl 3% KCl 3% NaCl 5% NH4Cl Freshwater Diesel
Sample1-A 94.36 94.59 94.06 94.22 92.91 98.06
Sample1-B 94.21 94.32 93.59 94.01 92.65 97.80
Sample1-C 95.02 94.97 94.42 94.50 92.63 98.46
Sample2-A 97.29 96.81 96.72 96.75 95.24 98.30
Sample2-B 96.60 96.50 95.86 96.07 94.25 97.39
Sample2-C 97.35 97.28 96.92 97.08 96.22 98.34
Sample2-D 97.28 97.24 96.94 97.13 96.08 98.30
Sample3-A 95.88 95.98 95.71 95.63 94.69 98.82
Sample3-B 96.44 96.29 96.06 96.01 95.77 98.99
Sample3-C 97.60 97.51 97.42 97.36 97.09 99.64
Sample4-A 95.08 94.83 94.46 94.78 92.68 96.26
Sample4-B 94.87 94.97 94.79 94.68 92.87 97.18
Sample5-A 95.33 95.43 94.82 94.84 93.36 97.06
Sample5-B 94.51 94.59 94.44 94.10 93.11 96.66
Sample6-A 96.22 96.02 95.34 95.66 92.66 97.14
Sample6-B 95.99 96.08 95.97 95.83 92.05 96.82
Sample6-C 96.80 96.61 96.25 96.37 94.83 97.42
Sample6-D 96.43 96.47 96.14 96.18 94.50 96.90
Sample6-E 96.71 96.88 96.63 96.56 96.51 97.03
SPE-192290-MS 4

Sample6-F 97.33 97.27 97.10 97.28 95.14 98.02

Results for capillary suction time (CST) tests are shown in Table 2. For this test 12 shale samples from
four different wells were used to conduct the study. Capillary suction time ratio is a good way to measure
reactivity of shales to different fluids. The ratio is a measurement to the reactivity of the shale where
CSTratio < 3 means low reactivity, CSTratio between 3 and 5 means moderate reactivity, and CSTratio > 5
means high reactivity. Freshwater, as to be expected, has the highest capillary suction time ratio going as
high as 33 in sample 4-B (Fig. 7). Sodium Chloride shows the 2nd highest capillary suction time ratio with
shale after water which means it is the least effective inhibitor in this study. Both concentration of
Potassium Chloride as well as Ammonium Chloride show low values in the capillary suction time ratio
indicating they are working well as inhibitors for these shale samples.

Table 2 Capillary Suction Time Test Results

Capillary Suction Time Ratio

Sample 7% KCl 3% KCl 3% NaCl 5% NH4Cl Freshwater
Sample1-A 0.79 0.74 1.28 0.77 2.06
Sample1-B 0.66 0.93 0.98 1.01 2.82
Sample1-C 0.92 0.95 1.51 0.97 2.79
Sample2-A 0.74 0.88 1.18 0.96 4.95
Sample2-B 0.98 1.05 1.46 0.97 10.87
Sample2-C 1.07 1.13 1.12 0.95 6.04
Sample2-D 1.11 0.92 1.49 0.89 5.24
Sample3-A 0.96 0.94 1.15 0.97 1.34
Sample3-B 1.96 2.58 2.48 2.11 2.62
Sample3-C 1.19 1.31 1.02 1.02 1.92
Sample4-A 3.52 3.92 5.89 3.67 33.14
Sample4-B 1.65 1.45 2.05 1.38 8.92

As for the mineralogy, XRD was used to identify the composition of the shale samples. Each sample
was tested 3-4 times. A semi-automated approach was used to identify the peaks and determine the mineral
composition of each sample. All these samples are from the same formation but from different
geographical locations and geological subdivisions of the target shale. Table 3 shows the XRD test results
for all 20 samples. The composition varies significantly even for samples from the same well but different
depths.
SPE-192290-MS 5

Table 3 XRD test results

K- Illite/ Illite /
Sample Quartz Plagioclase Calcite Dolomite Siderite Pyrite Marcasite Kaolinite Chlorite Kerogen
Feldspar Smectite Mica
1-A 14.5 0.0 2.7 3.2 0.0 4.0 5.3 0.0 15.3 7.9 23.9 9.4 13.9
1-B 15.8 0.0 4.8 0.6 0.0 2.7 4.2 0.0 16.4 14.2 17.5 16.4 7.8
1-C 17.6 0.0 4.8 1.0 1.0 0.2 5.1 0.3 13.5 10.6 15.0 11.6 19.3
2-A 13.0 3.3 3.6 0.0 0.0 0.0 2.2 0.0 13.4 24.4 20.5 9.6 8.9
2-B 15.4 3.8 4.3 0.0 0.0 0.0 2.0 0.0 14.5 26.6 19.1 9.5 4.1
2-C 36.7 5.1 4.7 0.0 0.0 0.0 8.0 0.0 10.7 15.4 4.0 3.6 11.0
2-D 34.0 5.5 5.2 0.0 0.0 0.0 5.9 0.0 11.8 18.5 5.3 5.1 8.0
3-A 18.8 0.0 6.8 0.0 1.2 0.0 13.8 1.0 15.9 14.0 0.0 2.1 26.5
3-B 50.2 0.0 4.5 0.0 1.9 0.0 5.3 0.7 12.2 9.3 0.0 1.1 14.9
3-C 69.6 0.0 2.8 0.0 0.8 0.0 1.3 0.5 6.2 6.0 0.0 0.7 12.0
4-A 16.2 0.0 3.8 0.0 0.0 2.4 1.4 0.0 26.6 11.5 13.0 25.1 0.0
4-B 15.5 0.0 3.1 1.3 2.1 0.5 2.5 0.5 30.3 16.7 11.5 16.0 0.0
5-A 18.8 0.5 3.5 0.4 0.0 1.2 0.9 0.0 12.1 16.5 4.6 39.6 1.9
5-B 14.6 0.3 2.8 0.2 1.4 0.0 2.7 0.3 27.2 18.5 2.9 19.9 9.4
6-A 14.4 0.7 4.2 0.0 0.0 0.7 2.2 0.0 21.8 12.9 15.9 22.8 4.3
6-B 10.5 0.4 4.0 0.0 0.0 0.2 1.1 0.0 26.0 16.6 15.6 22.4 3.2
6-C 15.9 0.0 3.2 0.0 0.0 0.0 3.9 0.4 22.1 18.6 8.2 13.9 13.8
6-D 12.3 0.9 3.4 0.0 0.0 0.0 1.5 0.0 31.7 14.3 12.2 21.3 2.4
6-E 13.0 0.0 2.6 0.4 0.0 0.0 2.6 0.6 24.7 19.1 7.6 23.3 6.0
6-F 9.9 0.0 4.7 0.0 0.0 0.0 4.1 0.6 7.3 43.6 2.4 18.8 8.6

No obvious correlations between the reactivity of the shale samples compared to the mineral
composition, shown in Table 3, were noted. The dispersion test results versus mineralogy of the sample,
were plotted in Fig. 8 to produce a dispersion test plot matrix. Diesel is the only fluid showing any direct
correlation with some of the mineralogy parameters. The most obvious one is the inverse relationship
between diesel dispersion test recovery and chlorite content, where an increasing concentration of chlorite
there is a decrease in the shale recovery percentage. A similar trend is observed for illite/smectite, there is
an inverse relationship between recovery percentages for shale sample ran with diesel and illite/smectite
content.
Using linear regression and the data available from this study, a model was developed to represent the
shale recovery percentage from dispersion test using diesel. The model has an R2 value of 0.91 and relative
absolute error of 35%. The model is shown in Table 4.
Table 4 Diesel Dispersion Test Model

Linear Regression Model

Diesel =

-0.11 * K-Feldspar +
-0.1297 * Siderite +
-0.072 * Illite/Smectite +
-0.0191 * Illite & Mica +
-0.0469 * Chlorite +
100.2211
SPE-192290-MS 6

Summary
The study shows the results of two shale-fluid sensitivity test using four standard inhibitors used in
drilling operations, compared to sample mineralogy from a range of samples from an unconventional shale
target. From the dispersion test, the best aqueous inhibitors are the 7% KCl and 3% KCl. They
outperformed the two other aqueous fluids (3% NaCl, and 5% NH4Cl). As for the capillary suction time
test, NaCl is the worst inhibitor amongst the four fluids. 7% KCl, 3% KCl, and NH4Cl are performing
similarly good in reducing the capillary suction time ratio and therefore are performing well in inhibiting
the shale sample. From these results, 7% KCl is the best inhibitor followed by 3% KCl. For economic
reasons, 3% KCl is recommended to be used as an inhibitor for drilling similar shale formations and to be
switched to 7% KCl for boost in shale inhibition as needed.

References
Al-Arfaj, M. K., Hossain, E., Sultan, A., Amanullah, M., Al-Fuwaires, O., & Al-Subai, T. (2014, December 10). Preliminary Test Results of
Inhibitive Water-Based Muds Used to Mitigate Unconventional Shale Drilling Problems. International Petroleum Technology
Conference. doi:10.2523/IPTC-17800-MS
Alouhali, R. A., Soliman, M. Y., Emadi, H., & Amanullah, M. (2017, October 15). Experimental Evaluation of the Swelling Behavior of
Unconventional Shale Formation at and Near the Wellbore in the Presence of Various Drilling Fluid Systems. Society of Petroleum
Engineers. doi:10.2118/187594-MS
Anderson, R. L., Ratcliffe, I., Greenwell, H. C., Williams, P. A., Cliffe, S., and Coveney, P. V. 2010. Clay swelling—a challenge in the
oilfield. Earth-Science Reviews, 98(3), 201–216.
Bol, G. M., Wong, S.-W., Davidson, C. J., & Woodland, D. C. (1994, June 1). Borehole Stability in Shales. Society of Petroleum Engineers.
doi:10.2118/24975-PA.
Chenevert, M. E., & Amanullah, M. (1997, January 1). Shale Preservation and Testing Techniques for Borehole Stability Studies. Society of
Petroleum Engineers.
Fink, J. K. (2012). Clay Stabilization. Petroleum Engineer’s Guide to Oil Field Chemicals and Fluids, 125–148.
Lal, M. (1999, January 1). Shale Stability: Drilling Fluid Interaction and Shale Strength. Society of Petroleum Engineers.
Stephens, M., Gomez-Nava, S., & Churan, M. (2009). Laboratory Methods to Assess Shale Reactivity with Drilling Fluids. American
Association of Drilling Engineers, National Technical Conference and Exhibition, 1–7.
O'Brien D.E., and Chenevert M.E. (1973): "Stabilizing Sensitive Shales with Inhibited, Potassium-Based Drilling Fluids," JPT. Vol. 25, pp
1089–1100.
Stephens, M., Gomez-Nava, S. and Churan, M., 2009. Laboratory methods to assess shale reactivity with drilling fluids. In AADE National
Technical Conference &amp; Exhibition. New Orleans, Louisiana, March 31-2 April 2009. Louisiana: American Association of Drilling
Engineers. pp 1–7.
SPE-192290-MS 7

Figures

Sample 1 Dispersion Test

99.00
98.00
97.00
96.00
95.00
94.00
93.00
92.00
91.00
90.00
89.00
7% KCl 3% KCl 3% NaCl 5% NH4Cl Freshwater Diesel

Sample1-A Sample1-B Sample1-C

Fig. 1-Sample 1 Dispersion Test

Sample 2 Dispersion Test

99.00

98.00

97.00

96.00

95.00

94.00

93.00

92.00
7% KCl 3% KCl 3% NaCl 5% NH4Cl Freshwater Diesel

Sample2-A Sample2-B Sample2-C Sample2-D

Fig. 2-Sample 2 Dispersion Test

SPE-192290-MS 8

Sample 3 Dispersion Test

101.00
100.00
99.00
98.00
97.00
96.00
95.00
94.00
93.00
92.00
7% KCl 3% KCl 3% NaCl 5% NH4Cl Freshwater Diesel

Sample3-A Sample3-B Sample3-C

Fig. 3-Sample 3 Dispersion Test

Sample 4 Dispersion Test

98.00
97.00
96.00
95.00
94.00
93.00
92.00
91.00
90.00
7% KCl 3% KCl 3% NaCl 5% NH4Cl Freshwater Diesel

Sample4-A Sample4-B

Fig. 4-Sample 4 Dispersion Test

SPE-192290-MS 9

Sample 5 Dispersion Test

98.00

97.00

96.00

95.00

94.00

93.00

92.00

91.00
7% KCl 3% KCl 3% NaCl 5% NH4Cl Freshwater Diesel

Sample5-A Sample5-B

Fig. 5-Sample 5 Dispersion Test

Sample 6 Dispersion Test

99.00
98.00
97.00
96.00
95.00
94.00
93.00
92.00
91.00
90.00
89.00
7% KCl 3% KCl 3% NaCl 5% NH4Cl Freshwater Diesel

Sample6-A Sample6-B Sample6-C Sample6-D Sample6-E Sample6-F

Fig. 6-Sample 6 Dispersion Test

SPE-192290-MS 10

Capillary Suction Time

35.00

30.00

25.00
CST Ratio

20.00

15.00

10.00

5.00

0.00

Capillary Suction Time Test 7% KCl Capillary Suction Time Test 3% KCl
Capillary Suction Time Test 3% NaCl Capillary Suction Time Test 5% NH4Cl
Capillary Suction Time Test Freshwater

Fig. 7-Capillary Suction Time for all Samples.

Fig. 8 Dispersion Test Plot Matrix