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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

subject to corrections by the author(s). Any person or entity that relies on any information obtained from this paper does so at their own risk. The information herein does not

necessarily reflect any position of URTeC. Any reproduction, distribution, or storage of any part of this paper without the written consent of URTeC is prohibited.

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

URTeC 1582182

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

( ) (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)

URTeC 1582182

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)

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:

URTeC 1582182

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)

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

M

Vb =

(28)

(29)

(30)

URTeC 1582182

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.

URTeC 1582182

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

p

2 p

Da 2

t

x

where

K

.

Da

( p ) + (1 ) K a

(41)

(42)

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

URTeC 1582182

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

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

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.

URTeC 1582182

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

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

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

c f ( Kn )

cT

c

cK

Da

URTeC 1582182

F

K

Ka

Kn

M

Mg

p

po

pc

pL

q

qL

Rh

Rg

Rp

t

T

Vr

Vc

r

Z

10

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

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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