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SPE 168840 / URTeC 1582182

Improved Data Analysis and Interpretation Method for Laboratory


Determination of Crushed-Sample Shale Gas Permeability
F. Civan, D. Devegowda, R. Sigal, University of Oklahoma
Copyright 2013, Unconventional Resources Technology Conference (URTeC)
This paper was prepared for presentation at the Unconventional Resources Technology Conference held in Denver, Colorado, USA, 12-14 August 2013.
The URTeC Technical Program Committee accepted this presentation on the basis of information contained in an abstract submitted by the author(s). The contents of this paper
have not been reviewed by URTeC and URTeC does not warrant the accuracy, reliability, or timeliness of any information herein. All information is the responsibility of, and, is
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Summary
Previously available interpretation methods developed for determination of gas permeability from crushed samples
are mostly applicable for conventional porous rocks of reasonably high permeability. This paper presents an
improved formulation which honors the relevant physics of fluid, transport, and shale-rock conditions for
determination of extremely-low nanodarcy gas permeability of shale by pressure-pulse transmission testing of
crushed shale-rock particles. The new method is demonstrated by means of typical simulated test conditions.
Assuming Darcian viscous flow instead of the nonDarcy flow yields almost twice the actual value of the intrinsic
permeability for this case.
Introduction
The intrinsic permeability of shale is only a characteristic of shale rock features, including its fabric and texture.
However, its value depends on the prescribed temperature and stress conditions as these conditions can alter the
shale-rock by deformation. In contrast, the apparent permeability measured by Darcys law is a property which
depends both on the shale rock properties, transport conditions, and fluid properties and behavior modified by poreconfinement effects. Thus, the permeability measured using a Darcy-type equation is the apparent permeability
depending on the prevailing conditions of fluid, transport, and shale, and not the intrinsic permeability. In fact, this
is the primary reason of contradictory values of permeability measured by different laboratories. Beskok and
Karniadakis (1999) expressed the difference between the intrinsic and apparent permeability for flow through a
single capillary tube by a conveniently simple correction factor based on the prevailing local conditions in shale
formations. Civan (2010) extended and generalized their formulation to a bundle of tortuous tubes representing the
gas transport paths in shale. A bundle of tubes is a special case of a more general porous media. Transport formulas
for a bundle of tubes differ from the more general case by the value of their formation factor (Sigal, 2002, Sigal,
2013). In terms of the cementation exponent for conventional reservoir rocks it is the transformation from m = 1 to
value closer to two.
Determination of the skeleton permeability in shale is very critical for improved reservoir management and plays a
key role in production forecasts, well placement, and configuration optimization. Although permeability estimates
may be obtained from production data analysis and history matching, such approaches are generally representative
of larger reservoir volumes and thus cannot capture high resolution heterogeneities. A more informative approach is
the use of core, crushed samples, or drill cuttings-based measurements obtained in the laboratory (Brace et al., 1968,
Hsieh et al., 1981, Neuzil et al., 1981, Dicker and Smits, 1988, Luffel et al., 1993, Wu et al., 1998, Egermann et al.,
2005, Cui et al., 2009, Barral et al., 2009, Civan et al., 2011, 2012, Profice et al., 2012, Xiong et al., 2012, and Tinni
et al., 2012).
However, these measurements need to be sufficiently representative of the in-situ conditions or alternatively,
interpretation models need to provide the means to correct for any deviations or errors, such as provided by Civan et
al. (2011, 2012). These measurements are typically acquired using core plugs, drill cuttings, or crushed sample

URTeC 1582182

methods under transient-state pressure-pulse transmission conditions. Thus, we critically review and analyze the
relevant methodologies available for extremely-low skeleton permeability determination and compare those using
new improved formulations to model gas transport in shale. We also evaluate and compare the methodologies and
models used in the literature for raw data interpretation and correction and identify inherent shortcomings at the
same time.
Tinni et al. (2012) determined by pressure-pulse testing of various shale samples that the permeability values
obtained by the GRI method varied depending on the equilibrium pressure values attained in various tests because
the gas rarefaction and slippage effects diminish at high pressures but important at low pressures. However, because
the GRI permeability measurement method is usually applied at relatively low pressure values, Tinni et al. (2012)
resorted to the formulation of Fathi et al. (2012) in order to be able to analyze the test data by considering the gas
slippage effect. They reported that the permeability values obtained using different gases were not sensitive to the
type of gas used in the tests.
The work described here will enable the industry to design better experiments to determine several unknown
parameters that impact transport calculations, including adsorption, diffusion, and deviation from Darcy flow.
Adsorption effects if not accounted for properly can lead to overestimation of total hydrocarbon storage and
effective permeability (Sigal, 2013, Sigal et al., 2013). We also focus on the GRI method implemented by Luffel et
al., 1993, Cui et al. (2009), and Tinni et al. (2012) for skeleton permeability estimation from easily obtainable drill
cuttings and identify key weak points and address the corrections necessary to improve the reliability of the
measurements. Further, we describe modifications necessary for crushed sample methods for application to
extremely-low permeability shale rock by pressure-decay methods. These corrections include Knudsen diffusion and
pore proximity effects on fluid properties that are currently not available in existing simulation models. These results
are compared to existing interpretation approaches to delineate the significance of considering the accurate
formulations required for shale transport modeling. Finally, we present studies to assess the sensitivity of factors
such as the particle size thereby enabling the design of a more standardized approach for shale characterization using
cores or drill cuttings.
Improved Formulation
Consider the schematic of the crushed-samples pressure-pulse transmission testing system given in Figure 1 (after
Jahediesfanjani and Civan, 2007, and Cui et al, 2009). The method presented here is a direct extension and
combination of the transient-state formulations of Cui et al. (2009) and Civan et al. (2011, 2012) for purposes of
laboratory determination of shale gas permeability using crushed-samples. Our corrections include the Knudsen
diffusion and pore-proximity effects on gas properties which the current simulation models do not consider.

Gas
Supply
Tank

Crushed
Particles
Tank

Figure 1: Schematic crushed-samples pressure-pulse transmission testing system (after Jahediesfanjani and Civan,
2007, and Cui et al, 2009).
Let the density, volumetric flux vector, and viscosity of the flowing gas, be denoted by , u, and , respectively,
and the apparent permeability tensor of shale by Ka.
The gas mass balance equation is given by:
(1 ) q
( )
.
(1)
+ ( u ) =
t
t

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The term on the right denotes the loss of gas mass by adsorption per unit bulk volume of shale-rock and per unit
time. Neglecting the gravity effect the transport of gas through shale porous formation is given by a Darcy-type
equation as:
1
(2)
u = K a p

Thus, invoking Eq. (2) into Eq. (1) yields:


( ) (1 ) q

+
= K a p + K a 2 p .
t
t

(3)

The core-plug gas transport formulation of Civan et al. (2012) is now extended for application to transport of gas in
spherical-shape crushed rock samples. First, Eq.(3) is expressed in spherical radial direction as:
2
K a p
Ka
1 2 p
p
=
c1 + 2 =
r

t cT r r r r cT

p 2 p 2 p
+ + 2 , 0 r Rp , t > 0
c1
r r r r

(4)

where r and t indicate the radial distance from the center of spherical particle and time, respectively, c1 is the
coefficient of compressibility (a function of the fluid density and viscosity , and intrinsic core permeability K
variation depending on pressure p) by:

c1 = c ( p ) + cK ( p ) + c f ( Kn ) ( p ) c ( p )

(5)

cT is the coefficient of compressibility (a function of the fluid density and adsorbed gas amount q, and core
porosity depending on pressure p) by:

1 q
q
cT = c ( p ) + c ( p ) +
c ( p ) c ( p )

(6)

In Eqs. (5) and (6), the coefficients of variation of the fluid density, fluid viscosity, core porosity, permeability
correction or flow condition factor, and intrinsic permeability with pressure, are denoted by the subscripts of , , ,
f(Kn), and K, respectively.
The apparent gas permeability Ka and the intrinsic permeability K are related by (Beskok and Karniadakis, 1999):
(7)
K a = K f ( Kn)
Here, the correction factor f ( Kn) is determined by:

4 Kn
f ( Kn) =
(1 + Kn ) 1 +

1
+ Kn

(8)

The pore-proximity effect on gas viscosity is accounted for by the first factor on the right of this equation. The poreproximity effect on real-gas deviation factor Z is accounted for the modification of the gas critical temperature and
pressure under pore confinement (Singh and Singh, 2011) according to the procedure proposed by Michel et al.
(2011a, b). This expression accounts for different gas transfer conditions such as the continuum fluid flow
(Kn 0.001), slip flow (0.001<Kn<0.1), transition flow (0.1<Kn<10), and free molecular flow (Kn 10) (Beskok
and Karniadakis (1999). It should be emphasized that the treatise of Beskok and Karniadakis (1999) is valid for gas
transfer occurring through a single straight capillary tube. Civan (2010) extended and generalized their approach for
a bundle of tortuous capillary tubes.
The dimensionless rarefaction coefficient is correlated by (Civan, 2010):

=
o 1 + B
Kn

(9)

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where o = 1.358, A = 0.1780, and B = 0.4348 are the empirical constants.


Let be the mean-free-path of molecules of a real gas and Rh the mean-hydraulic radius of narrow flow paths in
shale given, respectively, by (Carman, 1956, Civan, 2010):
Z Rg T
(10)
=
2M g
p

Rh = 2 2

(11)

where is the tortuosity, K is the intrinsic permeability, and is the porosity of porous media, is the viscosity
of gas, Rg is the universal gas constant, T is the absolute temperature, and Mg is the molecular weight of gas.
Then, the Knudsen number Kn is given by:

Kn =

Rh

(12)

The gas density is given by the real-gas equation of state, as:

Mp
(13)
ZRT
where Z is the real gas deviation factor, modified for pore confinement effect according to Michel et al. (2011).

The isothermal coefficient of variation of the rock and fluid properties F with pressure is expressed by:
1 F
(14)
cF =
F p
The Langmuir isotherm modified for mass of a real gas adsorbed per solid volume q is used as:
qL s M g
(15)
q=

pL
Vstd 1 +

p/Z

where s denotes the density of the shale skeleton, qL the Langmuir gas volume (standard volume per mass of
shale skeleton), pL the Langmuir gas pressure, and Vstd the standard molar volume of gas.
Thus, Eq. (4) can be written in a compact form as:
p
p
2 p
+=
Ua
Da 2 , 0 x L, t > 0 .
t
x
x
where the apparent convective flux U a and apparent transport coefficient Da are defined, respectively, as:

p 2
+
U a Da c1
r r
Ka
Da =
cT
The initial pressure of the gas inside the crushed sample particles is prescribed as:
=
p po , 0 r R p ,=
t 0

(16)

(17)
(18)

(19)

Following Cui et al. (2009), the shape of the crushed sample particles are represented as being spherical shapes.
Thus, the symmetry condition at the center of these particles is given by the following inner boundary condition:
p
(20)
= 0,=
r 0, t > 0
r
The rate of gas mass flow into a single particle at r = Rp is given by the following outer surface boundary condition:

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K p
(21)
m p =
Rp , t > 0
q =
Au =
( 4 R p2 ) a
,r =
r
Rp is the crushed particles grain radius. Consider that the continuous size distribution function of the crushed
samples is given by f(Rp). is the density of the test gas in the void space present in the gas and sample tanks,
assumed uniform but decreasing with time, measured as the pressure-pulse transmission test data. Assume there are
a total of N particles of various sized, loaded into the sample tank. Then, the mean grain radius is given by:

R pm = R p f ( R p ) dR p

(22)

The total mass of particles M is given by:

M = b R 3p Nf ( R p ) dR p
3

(23)

p and b denote the skeleton and bulk sample-particle densities, respectively. Following Cui et al. (2009) let Vr,
Vs, Vb, and Vc denote the volumes of the reference tank, sample tank, bulk of crushed sample particles, and total
open space occupied by gas, respectively (See Figure 1). Then, the following expression can be written, assuming
the compressibility of the crushed sample particles is negligible:
(24)
Vc =Vr + (Vs Vb )
Considering the volume occupied by the adsorbed gas, the mole of gas exchanged between the crushed sample
particles and the particle-free void space is given by:
V ( a ) po pe Vr pro pe (Vs Vb ) po pe
(25)
n = b
=
+

Rg T
Rg T Z o Z e
Z o Z e Rg T Z ro Z e
Rearranging yields:
p
p
p
p
Vr ro e + (Vs Vb ) o e
Z
Ze
Zo Ze
= a + ro
p
p
Vb e o
Z
Z
o
e

(26)

The corresponding equation of Cui et al. (2009) neglects pore volume occupied by adsorbed layer ( a = 0) assuming
the tests are conducted using non-adsorbing gases. Although Cui et al. (2009) also provide an expression for the
effective porosity, Civan et al. (2012) derived:
s M g (1 ) qL pL
.
(27)
a =
2
Vstd ( p ) ( p )( pL + p )
Civan et al. (2012) draw attention that the corresponding equation of Cui et al. (2009) missed the Mg term.
When the particle-size distribution is not a continuous function, Eq. (34) can be written as:
N
4

M = bi R 3pi Nf ( R pi )
3

i =1
If all the particles are approximately of the uniform size, then Eq. (36) simplifies as (Cui et al., 2009):
4

M = b R 3p N
3

The total bulk volume of particles Vb is given by:


M
Vb =

(28)

(29)

(30)

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The total rate of gas mass flow into all crushed particles N of size distribution is given by:

K p
2

m =
m
Nf
R
dR
Rp , t > 0
=
(
)
p
p
0 p
0 ( 4 Rp ) r Nf ( Rp ) dRp , r =
But, the isothermal coefficient of compressibility is given by:
1
c =
p
Thus,
(Vc )

p
p
=
= Vc = Vc = Vc c =
, r Rp , t > 0
m
t
t
p t
t
Equating Eqs. (31) and (33) yields the particle outer surface boundary condition as:

p
K p
2
Vc c , r =
Rp , t > 0
0 ( 4 Rp ) r Nf ( Rp ) dRp =
t
Or rearranging yields:

K p
p
2
Vc
Rp , t > 0
,r =
0 ( 4 Rp ) c r Nf ( Rp ) dRp =
t

When the particle-size distribution is not a continuous function, Eq. (34) can be written as:
N

p
Vc
Rp , t > 0
,r =
( 4 Rpi2 ) Kc pr Nf ( Rpi ) =

t
i =1

If all the particles are approximately of the uniform size, then Eq. (36) simplifies as:

dp ( t )
Vc
Rp , t > 0
,r =
( 4 Rp2 ) Kc pr N =
dt

(31)

(32)

(33)

(34)

(35)

(36)

(37)

Applying Eq. (32) to Eq. (37) yields the following expression given as the boundary condition by Cui et al. (2009):

d (t )
(38)
Vc
Rp , t > 0
,r =
( 4 Rp2 ) Kc r N =
dt

Assuming that the gas present in the gas tank can expand into the sample tank rapidly when the gas and sample
tanks are connected by opening the valve on the line connecting them the pressure of gas in the void space applied at
the particle outer surface:
(39)
=
p p=
Rp , t > 0
c,r
The void space pressure pc declines from an initial pressure value of pco until an equilibrium pressure pe is attained
and is measured vs. time as the pressure-pulse transmission test data.
Because the formulation given above yields a nonlinear partial differential equation, Eq. (16) cannot be solved
analytically. Therefore, we discretize it using an implicit finite-difference numerical scheme of the first-order time
accurate and second-order space accurate according to Civan (2007, 2009) and then solve numerically by an
iterative procedure as described in the Appendix of Civan et al. (2012). For this purpose, the coefficients of these
equations are first evaluated using the initial pressure at the start of simulation and then the pressures calculated at
subsequent time steps. We used 0.0025 seconds equal time increments, 101 equally spaced grid points, and a relative
deviation tolerance of 10-3 which led to satisfactory consistent and stable numerical solutions with around five
iterations.

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The number of tests which should be carried out should be greater than or equal to the number of unknown
parameters for unique estimation of the model parameters, including the permeability (Civan et al., 2012). This can
be accomplished by conducting sufficient number of pressure-pulse measurements on crushed shale particles under
different pressure conditions using different gases, such as He, N2, and CH4. We seek the best estimates of the
unknown parameters of the above formulation, listed in Table 1, in a manner to match the pressure gradient values
calculated by Eq. (37), rearranged as the crushed-particle outer surface boundary condition:
p ( t )
dp ( t )
Vc
(40)
=

,r =
c ( pd ( t ) )
Rp , t > 0
2
r
dt
( 4 Rp ) NK
Note that some parameter values can be acquired by direct measurements or property data.
Evaluation of Previous Data Analysis and Interpretation Methods

p
The model of Cui et al. (2009) is a simplified model because it neglects the term, assumes K, , and are
x
constant, and K , , h , and are zero. Then, Civan et al. (2012) have shown that Eqs. (16) and (18) simplify
2

to the following expressions of Cui et al. (2009):


p
2 p
Da 2
t
x
where
K
.
Da
( p ) + (1 ) K a

(41)

(42)

Analysis and Interpretation of Laboratory Tests


The pressure pulse-decay core tests are simulated using an assumed set of parameter values according to the
procedure described by Cui et al. (2009) considering the system shown in Figure 1. Initially, the gas is present in the
crushed samples tank at some prescribed pressure po. Suddenly, the high pressure nitrogen gas at pr present in the
gas supply tank is allowed to flow into the crushed sample tank, such that pr > po. The pressure pc of the crushed
sample tank void space is measured with time. The parameters of the present testing system of crushed-samples and
the best estimate values of the unknown model parameters, including the intrinsic permeability at the reference state of
1 atm pressure, are reported in Table 1. The measured downstream gas pressure vs. elapsed time was simulated
assuming an exponential decay with a decay rate constant of 0.05 s-1.
0.77
(43)
pc =
( atm ) 20exp 0.05 ( t ,sec )
Figure 2 shows the pressure profiles obtained over the radial distance in small spherical particles at different times
and a comparison of the calculated and measured spherical particle near-outer surface gas pressure gradients
assuming nonDarcy flow leading to an intrinsic permeability estimation of Ko = 7.7E-06 Darcy with a high-quality
match of data. Figure 3 presents the similar results but assuming Darcy flow leading to an intrinsic permeability
estimation of Ko = 1.5E-05 Darcy with a poor-quality match of data. As can be seen, assuming Darcian viscous flow
leads to a (1.5E-05/7.7E-06) = 1.9 times larger intrinsic permeability determination.
TABLE 1- Parameters of the data analysis model.
Parameters
Crushed-sample particle radius, Rp (cm)
Crushed-sample mass, M (g)
Crushed-sample bulk density, s (g/cc)
Crushed-sample porosity, (fraction)
Test conditions
Gas
Temperature, T (oC)

Values
0.2
35
2.5
0.05
Nitrogen
20

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Crushed-sample Initial gas pressure, po (atm-abs)


Applied initial void space gas pressure, pco (atm-abs)
Gas supply reservoir volume, Vr (cc)
Crushed-sample reservoir volume, Vs (cc)
Estimated parameters
Intrinsic permeability at 1 atm-abs, Ko (Darcy)
Langmuir pressure, pL (atm)
Langmuir volume, qL (cm3/g)
Tortuosity, o (dimensionless) at 1 atm-abs
(atm-1)

7.7E-06
45
7.5
2.3
1.0x10-6

K (atm-1)

4.0x10-6

(atm-1)

-2.0x10-6

200

15

Time, sec.
0.075
0.15
0.225
0.3
0.375
0.45
0.525
0.6

10

5
0
0.00

dp/dr, calculated (atm/cm)

Pressure, p, atm

20

1
20
45
45

150

100
50

Diagonal
Best match

0.05

0.10

Distance, r, cm

0.15

0.20

50

100

150

200

dp/dr, measured (atm/cm)

Fig. 2: Pressure profiles over the radial distance in a spherical crushed shale particle (left figure) and comparison of
the calculated and measured crushed particle gas pressure gradients (right figure) assuming nonDarcy flow leading
to an intrinsic permeability estimation of Ko = 7.7E-06 Darcy with a high-quality match of data.

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200

15

Time, sec.
0.075
0.15
0.225
0.3
0.375
0.45
0.525
0.6

10

5
0
0.00

dp/dr, calculated (atm/cm)

Pressure, p, atm

20

150

100
50

Diagonal
Best match

0
0.05

0.10

0.15

0.20

Distance, r, cm

50

100

150

200

dp/dr, measured (atm/cm)

Fig. 3: Pressure profiles over the radial distance in a spherical crushed shale particle (left figure) and comparison of
the calculated and measured crushed particle gas pressure gradients (right figure) assuming Darcy flow leading to an
intrinsic permeability estimation of Ko = 1.5E-05 Darcy with a poor-quality match of data.
Conclusions
We presented an improved interpretation and analysis method for the pressure-pulse decay tests. Our approach
yields accurate determination of intrinsic permeability compared with the earlier methods, including by Cui et al.
(2009), which are subject to the inherent limitations of the Darcy viscous flow equation. Our example demonstrated
that the assumption of Darcian flow yields twice the actual value of the intrinsic permeability that is obtained by
considering the prevailing nonDarcy flow conditions. Our method essentially determines the fixed values of the
variable-parameters at a reference condition, such as the standard conditions. Nevertheless, these values can be
subsequently substituted into the improved formulation presented in this paper in order to predict their values,
including the apparent permeability, at varying shale-gas reservoir conditions in presently available simulators.
Future studies are recommended for validation of the proposed interpretation model with a variety of experimental
data.
Acknowledgments
The authors gratefully acknowledge the funding from RPSEA (The University of Oklahoma Subcontract No. 0912211 (Sigal et al., 2010)) which provided support for the work done here, and from a consortium of service and
operating companies that also provided support for this work.
Nomenclature

c1

coefficient of variation with pressure (atm-1)

c f ( Kn )

coefficient of variation of permeability correction factor with pressure (atm-1)

cT
c

total coefficient of variation with pressure (atm-1)

coefficient of variation with pressure for fluid viscosity (atm -1)

coefficient of variation with pressure for porosity (atm -1)

cK
Da

coefficient of variation with pressure for intrinsic permeability (atm -1)

coefficient of variation with pressure for fluid density (atm -1)

apparent hydraulic diffusivity (cm2/s)

f ( Kn) flow condition function (dimensionless)

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F
K
Ka
Kn
M
Mg
p
po
pc
pL
q
qL
Rh
Rg
Rp
t
T
Vr
Vc
r
Z

10

rock or fluid property


intrinsic permeability (Darcy)
apparent permeability of gas (Darcy)
Knudsen number (dimensionless)
crushed-sample mass (g)
molecular weight of gas (g/mol)
absolute gas pressure (atm)
crushed-sample initial gas pressure (atm)
applied initial void space gas pressure (atm)
Langmuir gas pressure (atm)
mass of gas adsorbed per solid volume (g/cc)
Langmuir gas volume expressed in standard volume per mass of shale skeleton (cc/g)
hydraulic flow radius (cm)
universal gas constant (82.1 atm.cc/mol/K)
crushed-sample particle radius (cm)
time (sec)
absolute temperature (K)
gas-supply reservoir volume (cc)
crushed-sample reservoir volume (cc)
radial distance from the crushed-particle center (cm)
real gas deviation factor (dimensionless)

Greek

porosity of porous media (fraction)


mean-free-path of molecules (cm)
tortuosity of porous media (dimensionless)
gas density (g/cc)
crushed-sample bulk density (g/cm3)
dynamic viscosity of gas (cp)

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