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SPE-174968-MS

Measurement of Key Shale Petrophysical Properties


Mehrdad Zamirian, Kashy Aminian, and Samuel Ameri, West Virginia University

Copyright 2015, Society of Petroleum Engineers

This paper was prepared for presentation at the SPE Annual Technical Conference and Exhibition held in Houston, Texas, USA, 28 –30 September 2015.

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Abstract
Even though the advances in hydraulic fracturing and horizontal well technology have unlocked consid-
erable reserves of hydrocarbon contained in shale formations, quantification of the key petrophysical
properties in shale reservoirs still remain challenging. The unconventional formations such as shales
typically have permeability values in nano-Darcy range. It is not practical to measure the permeability of
the shale samples by conventional steady state techniques because of very low flow rates and length of
time required to reach the steady state condition. Therefore, unsteady state methods such as GRI and
pressure pulse decay which have been extensively used to estimate permeability of the shale samples.
However, the measured permeability values for similar samples by these techniques can differ by 3 orders
of magnitudes. This large margin of uncertainty and non-uniqueness of the results can be attributed to the
interpretations of the data obtained from transient techniques and reproducibility problems. Furthermore,
the unsteady-state measurements are not performed under the reservoir effective in-situ stress and
temperature which introduces more limitations.
This paper describes the design, construction, and application of a laboratory set up and test protocols
for accurate and repeatable measurements of the rich organic shale porosity, permeability and sorption
characteristics under reservoir stress conditions. The near steady-state measurements can be performed in
minutes up to hours, depending on the characteristics of the sample. This allows the permeability
measurements to be performed as many time as need to produce repeatable results. Furthermore, the
absolute permeability of the sample can be calculated by applying the gas slippage (Klinkenberg) and/or
gas double-slippage corrections. The monitoring of the flow rate during the experiment allows to
determine when the sample is fully saturated (adsorbed or desorbed). Therefore, there is no need for gas
sorption correction.
The paper also present the results of measurements on several Marcellus shale sample which clearly
indicate that shale’s porosity and permeability to a larger extent, are sensitive to stress and the stress
impact on permeability is non-reversible. This could be attributed to flow of gas through micro-fractures,
which do not contribute to porosity significantly. In addition, the analysis of the measurement results
indicated that only gas double-slippage corrections can provide reliable values for the absolute permea-
bility of the sample. The sorption characteristics, although not the primary objective of the measurements
with laboratory setup, are compatible with published values.
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Introduction
Shale gas is a promising secure source of energy. According to the U.S. Energy Information Adminis-
tration’s, The 56% increase in total natural gas production from 2012 to 2040 results from increased
development of shale gas, tight gas, and offshore natural gas resources. Shale gas production is the largest
contributor, growing by more than 10 TCF, from 9.7 TCF in 2012 to 19.8 TCF in 2040. The shale gas
share of total U.S. natural gas production increases from 40% in 2012 to 53% in 2040. Among shale gas
producing plays, Marcellus shale has the highest contribution which is growing daily due to advances in
horizontal drilling and hydraulic fracturing techniques. On the contrary of conventional or tight reservoirs
which have permeability values in ranges of mill-darcy to micro-darcy, shales have extremely low
permeability values in order of nano-darcy. These extreme low permeability values are due to the
microstructure of the shales. These micropores which are only a few nanometers in diameter disrupt the
application of classic fluid flow equations. Moreover, these micropores alongside the organic material in
the shales, kerogen, have a significant adsorption capacity (Ambrose et al. 2010). Therefore, better
understanding of the petrophysical properties of shale plays can improve the production, simulation and
future prediction. Shale characterization can be investigated from three aspects of permeability measure-
ment, adsorption measurement, and pore size characterization.

Permeability Measurement Methods


It is not practical to measure the permeability of the shale samples by steady state techniques because of
very low flow rates and length of time required to reach the steady state condition. Therefore, unsteady
state methods such as GRI and pressure pulse decay which are faster and can measure permeability values
as low as 1nD have been extensively used to estimate permeability of the shale samples. GRI is a common,
fast, and inexpensive method for permeability measurements on crushed samples (Luffel et al., 1993;
ResTech, 1996; Egermann, et. al, 2005; Profice et al., 2011). This method cannot be applied under stress
conditions. This popular method, however, has major drawbacks which limit its reliability. Recent studies
have shown inconsistent results on the same samples from different laboratories. This inconsistency is
contributed to factors such as the size of the crushed particles, equilibrium pressure, and volume
conditions of the test (Tinni et al. 2012). Pulse decay method which utilizes a core plug can be performed
under stress conditions. The interpretation of the results is complicated and is very sensitive to pore
volume and compressibility measurements. Over decades many researchers (Hsieh et al., 1981; Bourbie
and Walls, 1982; Dicker and Smits, 1988; Ning et al. 1993; Jones, 1997; Akkutlu and Fathi, 2012) have
tried to optimize the solution for pulse decay method. However, it has been reported that the permeability
values estimated by the pulse decay are 2 to 8 times higher than values measured by steady-state
techniques (Rushing et al., 2004; Carles et al., 2007).
Adsorption Measurement
Volumetric method is the most common technique for measurement of sorption characteristics of the
shales and coals. This technique can be applied to crushed or plug samples. The analysis data requires an
equation of states to calculate the amount of gas adsorbed at a series pressure stages. The results are
presented in the form of the sorption isotherm which can be used for estimation of the gas in place,
prediction of the released gas during reservoir depletion, or the potential for carbon dioxide sequestration.
The most popular sorption isotherm model used for coals and shales is known as Langmuir model.
Pore Size Characterization
Mercury injection capillary pressure (MICP) and nuclear magnetic resonance (NMR) methods are two
common methods for pore size characterization in shales. In mercury injection method, the amount of
mercury intruded into the sample at different pressures is measured and the pore size is calculated as a
function of applied pressure. The smallest pore size that can be measured by MICP is 1.8 nm (Curtis
2011). NMR relaxation spectroscopy senses the hydrogen atoms inside the pores and relates it to the pore
SPE-174968-MS 3

radius. MICP and NMR studies on Barnett shale samples suggested that the pore throat radii ranges
between 1.8-36 nm and 5-150 nm, respectively (C. A. Sondergeld 2010). Scanning electron microscopy
(SEM) and scanning transmission electron microscopy (STEM) techniques image the microstructure
pores directly. SEM can image small pores but some shales contain pores that are smaller than the
maximum resolution of the equipment. STEM can image pores as small as 2-3nm in diameter (Curtis
2011). Difficulties to image or measure pores in micropore category (⬍2 nm), necessitates other
approaches for pore size distribution. Low temperature (77° K) Nitrogen adsorption experiments allow to
access to these smaller micropores. Typically Brunauer, Emmett and Teller (BET) combined with t-plot
method yields the micropore surface area and Horvath-Kawazoe (H-K) method is used for micro pore size
distribution. For mesopore size distribution and pore volumes Barret, Joyner, and Halenda (BJH) method
is used. Also, density function theory (DFT) method is used for micropore-mesopore distribution
(Adelola, 2011).

Methodology

Objective of this research is to develop and evaluate a new technique which allows petrophysical
properties like porosity, permeability, formation compressibility, and sorption parameters to be measured
more accurately and faster than commonly used techniques. The impact of the adsorption/desorption by
different gases on these petrophysical properties will be also investigated. The laboratory set-up, referred
to as Precision Petrophysical Analysis Laboratory (PPAL) here, is designed, constructed, and assembled
for accurate and repeatable measurements of the rich organic shale petrophysical properties including
porosity, permeability and sorption characteristics under reservoir stress conditions. The detailed descrip-
tion of the system and complete sample preparation as well as the porosity and permeability measurements
procedures are available elsewhere (Zamirian et al., 2014a, 2014b). This multitasking machine is inspired
by CORAL (Computer Operated Rock Analysis Laboratory) designed at the Institute of Gas Technology
where it was used to measure porosity and permeability of tight sandstones of Mesaverde (Randolph
1983).
Preparing a complete and accurate report on petrophysical properties of a sample requires different
tests, with different gases, and at different pressure or temperature conditions. Thus, it is imperative to
have a detailed protocol to optimize the time needed to perform the tests and to minimize the damages to
the plug sample during the experiments. A stepwise procedure has been prepared here to run a full set of
tests on a sample is presented below:
1. Cut the core plug and dry it in humidity oven at 60 °C and 45% humidity until its weight stabilizes.
This temperature and humidity removes all the free water except one or two layers of water on the
clays. This prevents the minerals deformation due to drying (Bush 1970, Soeder 1988).
2. Load the sample in the core holder and apply 500 psia confining pressure. This pressure preserves
the sample from geomechanical changes due to net stress effects. It will also reveal any possible
problem with the water leak from the gas lines. If no water leak is observed, then the core holder
can be connected to the gas system.
3. Pressurize the system to 200 psia gas pressure. (If this is the first time, use a non-adsorbate gas
such as Helium).
4. Isolate PPAL from room, and set the temperature and monitor the temperature until the system
temperature reaches the set value. It may take up to 72 hours for the temperature to stabilize
depending on the temperature of the water used for confining pressure.
5. Isolate all the PPAL gas sections by closing all the valves, and monitor the pressure over time to
detect any gas leakage.
6. Repair or replace the leaking sections and repeat the monitoring until no gas leakage is observed
4 SPE-174968-MS

in the system.
7. Set the upstream and downstream pressures to 150 and 50 psia respectively, and perform porosity
and permeability tests. The porosity test usually takes 10 to 15 minutes, while the permeability test
depending on the permeability, TOC of the sample, and the type of gas might take few minutes
to couple of hours. It is recommended that the permeability test be repeated at least 30 times to
determine if the tests results are reliable and the sample is completely saturated (adsorbed/
desorbed).
8. Increase the upstream and downstream pressures for the next set of measurements. During these
measurements, as the gas pressure is increased, the confining pressure should be increased such
that the net stress to remain constant. The main purpose here is to measure the effect of gas type
and its pressure on permeability. When a non-adsorbate gas such as helium is used, the porosity
is not expected to change. Therefore, there is no need to measure the porosity every time the
permeability is measured. However, it is recommended to measure the porosity randomly at higher
pressures to validate the initial measurement. When an adsorbate gas such as Carbon Dioxide or
Methane is used, the pore volume changes due to the adsorbed layer thickness at pressures above
3000 psi (Santos, 2012). Since these tests are performed at low pressures it is not recommended
to measure porosity at every pressure. Our results in the next section illustrate this better.
9. Repeat the permeability test for at least four different mean gas pressures by increasing the
pressure from 100 to 400 psia. This will provide sufficient data for application of the gas slippage
correction.
10. Repeat the permeability tests by decreasing the mean pressure from 400 to 100 psia when an
adsorbate gas is used. This will capture the hysteresis during adsorption and desorption.
11. If it is desired to evaluate the effect of different gases on the measured properties, proceed to step
12, otherwise go to step 13 to perform adsorption measurements, or go to step 14 for evaluation
of the geomechanical effects.
12. If the sample exhibited adsorption with the previous gas, take it out of core holder, vacuum it for
12 hours and put it in the humidity oven until its weight stabilizes. Replace the gas in the system
with the desired gas and repeat steps 2-10.
13. Perform volumetric adsorption test in successively higher pressure levels at desired temperature
and stress condition,
14. Measure the permeability and porosity at a low net stress and repeat the measurements by
increasing the confining pressure in 500 psia increment up to the limit of the system (9,000 psia
or permeability less than 1 nD).
15. Measure the permeability and porosity by decreasing the confining pressure in 500 psia steps to
evaluate the geomechanical hysteresis effects on these properties.
16. Finally, crush the sample, sieve it, perform the low temperature adsorption test, and measure the
pore size distribution.
Results and Discussion
A Marcellus shale sample with 0.8% TOC was acquired for the experiments. After preparation and
loading it, the first set of experiments was performed to evaluate the effects of the gas type and the gas
pressure on the permeability. The permeability measurement was conducted by Helium and was repeated
at successively higher pressure steps (during adsorption) and then it was repeated at successively lower
pressure steps (desorption). The procedure was repeated with Nitrogen and Carbon Dioxide.
Figure 1 illustrates the results of permeability measurement at constant net stress for various gases. As
it can be observed, the permeability measurements did not exhibit any hysteresis with Helium and
Nitrogen which can be related to the low TOC of the sample. However, the permeability measurements
with Carbon Dioxide clearly exhibit hysteresis between adsorption and desorption. At higher pressure, the
SPE-174968-MS 5

permeability values measured by Helium and Nitrogen are very close. However as the mean gas pressure
decreases, the difference between the two sets increases. The permeability values measured using Carbon
Dioxide exhibit lower permeability values at all the gas pressures. These differences in the measured
permeability values by different gases can be contributed to the gas slippage effect.

Figure 1—The Effect of Gas Type and Gas Pressure on Gas Permeability Measurements

Klinkenberg (1941) demonstrated that the permeability of porous media to gases is a linear function of
the reciprocal pressure. His theory suggests that the momentum carried by the gas molecules hitting the
pore walls, gas slippage, results in higher gas velocities. For shales which have average pore sizes smaller
than 10 nm (Akkutlu and Fathi 2011, Adesida et. al, 2011), the Klinkenberg theory is not valid because
it ignores the momentum that gas molecules can carry to the bulk fluid. Fathi et al (2012) incorporated
the momentum carried by bouncing back molecules that lead to a linear relation between permeability and
reciprocal of the square of pressure. This is referred to as the double-slippage correction. Figure 2
illustrates the results of the application of double-slippage correction to the permeability measurements for
different gases. As it can be observed, the absolute permeability values for the Helium or Nitrogen data
sets are identical. This is consistent with definition of absolute permeability which is an intrinsic rock
property independent of the gas type. Moreover, it is important to note that while the absolute permeability
for Carbon Dioxide data sets are the same, but lower than the absolute permeability values for Helium or
Nitrogen. This can be explained by the higher affinity of Carbon Dioxide. The tendency of Carbon
Dioxide molecules to attach to the pore surface can cause a reduction in open pore-throat size (swelling
effect) and therefore a reduction in the permeability.
6 SPE-174968-MS

Figure 2—Determination of Absolute Permeability by Double-Slippage Correction

To investigate the effect of stress on porosity and permeability, a second set of experiments were
performed by maintaining the gas pressure while increasing the confining pressure from 700 to 7,900 psia.
To capture the hysteresis the experiments were repeated by decreasing the confining pressure from 7,900
to 700 psia. Figure 3 illustrates the effect of stress on the porosity measurements which exhibit a
non-linear trend. The hysteresis appears to be insignificant which suggests that the larger pores (major
contributors to porosity) are elastic. Figure 4 illustrates the effect of stress on the permeability measure-
ments. Contrary to porosity, permeability exhibits a significant hysteresis suggesting the irreversibility of
the permeability. According to Figure 4, permeability values drop faster at lower stress than at high stress.
This observation can be explained by the presence two pore system, i.e. fracture and matrix. At low stress,
the fractures contribute significantly to the total permeability are open. As stress increase, these fractures
tend to close causing a reduction in permeability. After all the fractures are closed, the only contributor
to permeability is the matrix which is less sensitive to stress than fractures. To evaluate this hypothesis,
we applied Walsh’s theorem (Walsh, 1984) to the measured permeability values. According to Walsh the
fracture closure pressure can be estimated by plotting (k/k0)1/3 vs. In(p/p0) where k is the measured
permeability at confining stress of, p and k0 is the permeability at lowest confining stress, p0. Figure 5
illustrate this plot for the measured permeability values. On this plot, two straight lines are present. The
first straight line represents the stress values when the fractures are open and the second straight (change
in the slope of the line) represents the stress values when the fractures are closed. Figure 5 suggests that
fractures are closed above 4,700 psia.
SPE-174968-MS 7

Figure 3—Impact of the Stress on Porosity

Figure 4 —Impact of the Stress on Permeability


8 SPE-174968-MS

Figure 5—Estimation of the Fracture Closure by Walsh Method

To investigate adsorption/desorption isotherms and pore size characterization, the third set of exper-
iments were performed. These measurements performed by Micromeritics accelerated surface area and
porosimetry (ASAP) 2020 and the results were matched with BET, t-plot, BJH, and H-K methods. These
measurements are necessary to determine the pore size distribution of the sample, average pore size, shape
of the pores, and possible hysteresis during adsorption and desorption. The pore size distribution and the
average pore size are necessary to confirm the need for double-slippage correction. Also, knowing the
hysteresis during adsorption and desorption would provide a better understanding of the pore structure.
Figure 6 demonstrating the results of the sequential adsorption/desorption tests with Nitrogen. The shape
of the adsorption curve on this figure is consistent with type II isotherm according to IUPAC classifica-
tion. Type II isotherm are typically associated with multilayer adsorption. In addition, the hysteresis
observed on the desorption curve suggests slit-like pores (hysteresis loop type H3 according to Sing et al.,
1985). BET method combined with t-plot was used for the micropore (0.7 to 2 nm) characterization and
BJH method was used for mesopore (2 to 50 nm) characterization. Table 1 summarizes the results from
each method and demonstrates that the average pore size in micropores and mesopores are 0.848 and 6.48
nm, respectively. Furthermore, 21% of the pore volume is associated with the micropores. These results
provide a good justification for the application of double-slippage correction.
SPE-174968-MS 9

Figure 6 —N2 Adsorption/Desorption Isotherms

Table 1—Pore size characterization results

Conclusions
1. Permeability of shales can be measured under steady-state conditions. This method is fast,
repeatable, and does not require a complicated interpretation or adsorption correction like pulse-
decay or GRI methods.
2. In tight formations double-slippage correction results in consistent and plausible value for the
absolute permeability.
3. Adsorption and desorption cause hysteresis in permeability during adsorption and desorption. The
amount of adsorption depends on the type of the gas and TOC of the formation. The adsorption
of CO2 resulted in the pore size and permeability reduction.
4. Permeability is very sensitive to stress while porosity is impacted by stress to a lesser extent. Also,
the impact of stress on permeability is an irreversible process.
10 SPE-174968-MS

5. Non-linear behavior of permeability with respect to stress is contributed to the different response
of the fracture and matrix to the stress which can be successfully verified with Walsh theory. This
theory can determine the pressure at which the fractures are closed and the flow occurs only in the
matrix.
6. Nitrogen low temperature adsorption/desorption results suggest multi-layer adsorption and slit-like
pores for Marcellus shale samples. Also, these pore characterization tests confirm that the high
percentage of micropores and small average pore size for the mesopores.

Acknowledgements
The authors with like to thank USDOE/NETL and URS corporation for providing financial and technical
support for design and construction of PPAL Apparatus. The technical support provided by Mr. Daniel
Soeder and Mr. Josh Dalton were instrumental in successful operation of the laboratory set up.

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