SPE-195805-MS

Pore-Scale Characterization of Eagle Ford Outcrop and Reservoir Cores

with SEM/BSE, EDS, FIB-SEM, and Lattice Boltzmann Simulation

Sherifa Cudjoe, Siyan Liu, and Reza Barati, University of Kansas; Franciszek Hasiuk, Kansas Geological Survey;
Robert Goldstein, KICC - University of Kansas; Jyun-Syung Tsau, TORP - University of Kansas; Brian Nicoud, Kyle
Bradford, Amanda Baldwin, and David Mohrbacher, Chesapeake Energy

Copyright 2019, Society of Petroleum Engineers

This paper was prepared for presentation at the SPE Annual Technical Conference and Exhibition held in Calgary, Alberta, Canada, 30 Sep - 2 October 2019.

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Abstract
The objective of this work is to conduct pore-scale analysis of the pore systems in an Eagle Ford (EF)
outcrop sample and a Lower Eagle Ford (LEF) sample from a producing interval in the subsurface. After
characterization, we estimate bulk transport properties (such as tortuosity and permeability) within each pore
network model (PNM) using the lattice Boltzmann method (LBM). Comparing the two will evaluate the
degree to which outcrop samples of the EF are or are not applicable analogs to the subsurface for laboratory-
scale "huff-n-puff’ enhanced oil recovery experiments.
Grain types and pore systems of both samples were visualized and quantified at the micro- and nanoscale
using scanning electron microscopy/backscattered electron microscopy (SHM/BSH), energy- dispersive X-
ray spectroscopy (EDS), and focused ion beam-scanning electron microscopy (FIB-SEM). These methods
measure mineral content, elemental (mineral) analysis, size distribution of pores and pore throats in addition
to serving as the basis to develop pore network models (PNMs) for simulation. The LBM was then applied
to the extracted pores to estimate permeability for each medium.
The 2D SEM/BSE/EDS images of the EF outcrop sample showed that the microstructure of finegrained
inorganic matrix was modified by calcite neomorphic and passively precipitated microspar, spar, and
pseudospar altering the texture of the depositional matrix, low clay content with some of feldspar, solution-
enlarged microfractures, compactional fractures, coccolith debris, and calcite deformation (solution-
enlarged cleavages). There are abundant microfossils including foraminifer tests ("forams") filled with
either diagenetic calcite, quartz, organic matter or a mixture of these minerals; the organic matter in the
foram chambers mostly show cracks/shrinkage pores or lack pores in organic matter.
On the other hand, the LEF reservoir sample showed significantly different diagenetic alteration with
localized phosphate diagenesis, less calcite neomorphism, and better developed pores within the organic
matter infilling the foraminiferal tests as well as in depositional kerogen embedded within the inorganic
matrix. In addition, 3D FIB- SEM volumes showed the variation in tortuosity of each extracted PNM and
its impact on the diffusion coefficient during gas huff-n-puff recovery. The LBM enabled the estimation of
permeability at the molecular level from each extracted PNM.
2 SPE-195805-MS

Not surprisingly, the textural and compositional differences between the outcrop and subsurface samples
lead to different PNM and different behavior in huff-n-puff experiments. This work bridges a gap in the
literature by comparing and revealing the pore-scale heterogeneities of an outcrop sample to that of a
subsurface sample to measure the impact of the underlying mechanisms associated with gas huff-n-puff
recovery at the laboratory-scale, while estimating permeability within extracted pores with the LBM.

Introduction
The rise in petroleum production from fine-grained, "unconventional" deposits has demanded a greater
understanding of pore networks that govern migration, diagenesis, production, and enhanced oil recovery.
Outcrop samples of unconventional shales are typically thought to be poor analogs for subsurface shale
resources due to weathering at the surface [1,2]. Outcrop materials are used, however, when reservoir
(subsurface) cores are unavailable, when larger samples are needed, and to constrain stratigraphic variability
[3, 4, 5, 6]. As little is known about the pore-scale heterogeneities of outcrop samples in comparison to
subsurface samples, this study compares Eagle Ford Shale (EF) samples from the outcrop and subsurface,
to evaluate if their pore networks would lead to the same interpretations when used in laboratory-scale
studies of gas "huff-n-puff’ experiments. Hull'-n-pulf uses cyclic injection of a reservoir enhancement fluid,
soaking of that fluid to allow enough time to permeate into the ultra-tight matrix from the fractures, and
production of hydrocarbons in addition to the injected fluid.
The EF outcrop used in this study is present along US Highway 90 West in Val Verde County, Del Rio,
Texas, where the formation is known as Boquillas and presumed to be in the same depositional basin setting
as the Maverick Basin [7, 8]. A sample from this play was chosen to test the hypotheses that outcrop samples
are or are not good analogs for reservoir rock. The Boquillas formation is approximately 200 ft. thick in the
Val Verde County and described to be deposited during the Cenomanian-Turonian Oceanic Anoxic Event
[9]. The lowest member of the formation consists of breccias, slump folds, debris flows, turbidites, and
contourites, while the middle member (the member of interest) consists of black, organic- rich lithologies
[10, 11]. The middle member is regarded as a potential analog for source rock or unconventional reservoir
rock with high carbonate content and commonly described as intermixed marlstones or argillaceous lime
mudstones, that are largely recrystallized [9]. The total organic carbon (TOC) of the outcrop is reported
to fall in the range of 2 - 5.7 wt. % with an indication of an immature oil- prone Type I kerogen from the
hydrogen index (HI) versus oxygen index (OI) crossplot [6, 8]. The mean random vitrinite reflectance (Ro %)
value of samples from the Comstock West outcrop (US Highway 90, Val Verde County, Texas) is reported
as 0.53 %, determined to be matured with maximum temperature (Tmax) between 423°C and 429 °C [12].
Advanced imaging techniques such as scanning electron microscopy/backscattered electron microscopy
(SEM/BSE), energy-dispersive X-ray spectroscopy (EDS), and focused ion beam-scanning electron
microscopy (FIB-SEM) are commonly employed in pore-scale characterization to capture the in- situ
complexities and heterogeneities of fine-grained unconventional resource rocks ("shales"). Both SEM and
BSE provide high resolution 2D images of a sample's surface; SEM produces topographical information,
while BSE shows the contrast between elemental compositions of different minerals. EDS identifies and
quantifies the elemental composition of the SEM/BSE imaged areas from which the mineral composition
can be inferred. On the other hand, FIB-SEM produces iterative 2D slices, capable of being reconstructed
into a 3D volume to show pore connectivity and resolve nanometer-size pores. These advanced imaging
techniques have been applied extensively to Lower Eagle Ford (LEF) reservoir cores within the oil
window to characterize the sample heterogeneity prior to gas huff-n-puff [13, 14, 15]. Common grain
types found in the LEF subsurface samples from SEM/BSE and EDS analysis include detrital quartz, clay
minerals, foraminifera, coccoliths, and depositional kerogen. Diagenetic phases include calcite cement,
pyrite, kaolinite, albite, and migrated organic matter. Pore and pore throat size distributions have been
reported to be in the range of 13 nm to 500 nm and 5 nm to 400 nm, respectively, with geometric average
SPE-195805-MS 3

tortuosity between 1.5 and 2.0 for both organic and inorganic extracted pore network models (PNMs)
[13]. Little to no pore-scale characterization work has been published on EF outcrop samples to clarify the
feasibility of gas huff-n- puff recovery process. One of the objectives of this study is to carry out detailed
pore-scale characterization on an EF outcrop sample to compare with that from a LEF reservoir sample.
This project incorporates the Lattice Boltzmann model (LBM) to calculate fluid flow behavior through
pore networks, a mesoscopic fluid dynamics model that considers the trajectory of a group of particles rather
than that of individual particles in molecular dynamics, rendering it less computationally extensive [16, 17].
The LBM was developed as an improvement on the lattice gas cellular automata (LGCA) by replacing the
Boolean variables with distribution functions, f(x, t), assigned to a group of particles confined to a lattice
in space and time [18]. Thus, the LBM simply solves the Boltzmann equation, an analogue of the Navier-
Stokes equation at the molecular level.

Methods
Samples
A rock chips of 12 mm × 10 mm × 8 mm size are prepared from as-received uncleaned samples of an
EF outcrop with TOC in the range of 2 - 5.7 wt. % and vitrinite reflectance of 0.53 % [12] and a LEF
reservoir sample with total organic carbon (TOC) of 5.29 wt. % and a vitrinite reflectance (%Ro) of 0.98%,
respectively. The mineral composition and regional characterization of the LEF reservoir sample is detailed
in another phase of this study [13]. Both rock chips were ion-milled using the SEM Mill Model 1060 at the
NanoFab Laboratory (University of Utah, Provo, Utah, USA). Ion milling reduces the roughness of sample
surfaces while minimizing the chance of plucking, which plagues even the finest lapidary techniques, before
carrying out SEM and FIB-SEM scans. Argon million also increases the precision of EDS analysis by
reducing the scatter of the reflected X-ray beam.

Scanning/Backscattered Electron Microscopy (SEM/BSE)

High resolution SEM/BSE images were acquired for both samples using the Hitachi 8230 instrument at the
Microscopy and Analytical Imaging Lab at the University of Kansas (Lawrence, Kansas, USA). It employs
a cold field emission gun with a resolution of 0.8 nm for selected voltage and current at 10 kV and 15.2 |iA,
respectively. SEM/BSE images were acquired at various magnifications to resolve grains, OM, and pores
in addition to diagenetic phases.

Energy-Dispersive X-ray Spectroscopy (EDS)

The Hitachi 8230 is connected to the silicon drift EDS detector (Oxford Instruments, X-MaxN, UK), which
enables the identification of different elements within the regions of interest (ROIs) selected on the SEM/
BSE images of either samples from which the mineral composition of the samples at the pore-scale can be
inferred. The elemental mapping and energy spectrums were acquired with Aztec tools (Oxford Instruments,
UK). A table is presented in another study, which lists the various elements and their corresponding inferred
minerals [13].

Focused Ion Beam-Scanning Electron Microscopy (FIB-SEM)

The FEI Helios Nanolab 650 at the Utah NanoFab lab was used for high resolution imaging. The FIB- SEM
system is capable of resolving the organic pores at the nanometer scale. It involves acquiring a series of 2D
slices on Argon ion milled surfaces with a milling depth of approximately 10 nm. The resulting 2D slices
are then reconstructed into a 3D volume from which digital rock analysis can be carried out to generate
PNMs and simulate bulk transport properties. More than 200 2D slices were acquired for each sample at an
ion beam current of 0.79 nA, an acceleration voltage of 30 kV, and a working distance of 4 mm but only
100 slices were used in the analysis to limit computational complexity [13].
4 SPE-195805-MS

Image Processing and Segmentation. The resulting FIB-SEM images were processed with PerGeos
software (Thermo Fisher Scientific) through steps such as: geometry correction to compensate stage tilt,
alignment, removal of bad slices, reduction of curtaining artifacts, reduction of noise, and shear and shading
correction of the images. Subsequently, a marker-based watershed segmentation algorithm was applied to
segregate and quantify the relative abundance of component phases (e.g., mineral, organic matter, and pores)
in the grayscale images. This has been explained in detail in previous work [13].
Tortuosity. Although it is not easily measured, the tortuosity of fluid flow pathways plays a significant
role in enhanced oil recovery (EOR) through gas huff-n-puff in shale oil reservoirs due to its correlation to
the diffusion coefficient because injected gas requires enough time to permeate the shale matrix from the
matrix-fracture interface. It also impacts permeability estimations. As such, an estimation through digital
rock analysis is currently the method that yields the best proxy for an in-situ measurement. This study
considers the geometric method, which describes the physical tortuous pathways of the extracted pores
through segmentation, without relying on the diffusivity or conductivity of the medium. It is defined as the
ratio of the geodesic distance (LG) to the Euclidean distanced (LE) [19].

(1)

While the geodesic distance (LG) is described as the shortest path possible in the presence of an obstacle
(or another phase), the Euclidean distance (LE) is the assumed shortest distance in the absence of any
interfering structure, i.e., a straight-line [19].

Lattice Boltzmann Simulation

The LBM comes in different dimensions with varying speeds and this study employed the variant called
"D3Q19" for 3D volumes ("D3") in space with 19 velocity vectors ("Q19") as shown in Figure 1 The D3Q19
was applied to the segmented pores of both the outcrop and reservoir samples to simulate single phase
fluid flow and estimate permeability using the open source Lattice Boltzmann Methods for Porous Media
(LBPM) developed by James McClure at Virginia Tech [20]. It allows the input of segmented pores from
the FIB-SEM images ("3D tiff images") to be used as the simulation domain. In addition, a bounce- back
boundary condition is applied at the pore walls with a fixed pressure gradient between the inlet and outlet
planes; we varied the pressure gradient between 0.01 and 0.05 lattice units. The velocity field is initialized
at zero and the particles are driven by the linear pressure drop between the inlet and outlet using a single
relaxation time of 1. To determine the steady state for permeability estimation, the coefficient of variation
(CV) parameter is used, which is defined by dividing the standard deviation of the velocity distribution by
the average velocity over the flow medium.
SPE-195805-MS 5

Figure 1—Schematic diagram of a D3Q19 model showing the flow direction of our simulation after Wang [21]

The smaller the CV value, the easier for the simulation to converge; a threshold value of 0.001 was
used in this work. Subsequently, the macroscopic fluid properties (such as velocity, density, and kinematic
viscosity) were resolved through the collective behavior of the microscopic particles at steady state and the
permeability is estimated based on Darcy's equation
(2)
where, uavg is the average velocity, v is the kinematic viscosity expressed in terms of the relaxation time, L
is the length along the direction of flow, and Δp is the pressure gradient.

Results & Discussion

Grain Types and Pore Systems
The matrix of both the outcrop and the subsurface samples are dominated by calcite with significant
contributions of quartz, clay minerals, pyrite, and traces of dolomite. In the outcrop, the calcite is
observed to grow outwards from calcitic nuclei and invade or replace matrix minerals (neomorphism and
cementation). Moreover, the clay content in the outcrop samples is very low or non-existent compared
to that of the subsurface sample. The porosity in the mineral matrix in the outcrop sample is much
more significant with solution-enlarged cleavage fractures in calcite, solution-enlarged micro-fractures,
compactional microfractures as well as parallel nanofractures.
On the other hand, inorganic pore types observed in the subsurface sample were mostly interparticle
pores between matrix grains (clay, quartz and calcite) and intraparticle pores (chambers) within forams,
with some intercrystalline pores and solution-enlarged fractures. Most of the interparticle and intraparticle
pores were filled with migrated OM (solid bitumen), itself containing pores of various morphologies as
observed in the BSE images below.
Organic matter (OM) distribution, either embedded in the matrix or infilling the chambers of forams was
observed in both the outcrop and subsurface samples, but the organic matter in the subsurface sample is
riddled with abundant circular pores, likely from thermal maturation. In contrast OM in the outcrop samples
show cracks/shrinkage pores, likely related to devolatilization [15].
In addition, the subsurface sample and the outcrop sample show contrasting diagenetic fabrics and
histories. For the subsurface sample, kaolinite, calcite, pyrite and quartz are common cements within forams.
Hydrocarbons generated at the onset of oil generation to within the gas generation window are thought to
6 SPE-195805-MS

migrate into remaining inter- and intraparticle pores following the formation of authigenic minerals [22].
In so doing, the paragenetic sequence of diagenesis in a foraminiferal mudstone was thought to start with
authigenic pyrite, followed by calcite, then quartz, the kaolinite/pyrite cementation, bitumen, fractures, and
organic porosity [22]. The presence of compactional brecciation in the calcite cement observed in the BSE
images of the subsurface (Figure 6 and Figure 7) postdates the calcite and predates the migrated OM.
LEF Reservoir (Subsurface) Sample. Figure 2 (A) and Figure 3 (A) show BSE images of the subsurface
sample at varying magnifications, with distributions of foraminifera tests reduced by cements (kaolinite,
pyrite, quartz, and calcite) and migrated organic matter identified through EDS analysis (below each image).
The matrix is dominated by calcite (Ca map), quartz (Si map), a phosphate mineral (P map), organic matter
(C map), and clay minerals (Al and Si maps), with traces of pyrite (S), albite (Na), and dolomite (Mg).
The presence of interstratified phosphatic intervals are believed to represent diagenetic replacements of
carbonate minerals and depositional phosphate [24].

Figure 2—A) BSE image of the LEF reservoir sample showing abundant kaolinite cement (white arrows)
and calcite cement (yellow arrows) in intraparticle pores in foraminifera. B) Elemental maps from EDS
analysis with distributions of Al (kaolinite), Ca (calcite), Si (quartz and other silicates), and P (phosphate).
SPE-195805-MS 7

Figure 3—A) BSE image of the LEF reservoir sample with distributions of non-detrital phosphate (P
map), calcite (Ca map), quartz (Si map), and traces of dolomite (Mg map). Calcite (yellow arrows) and
kaolinite (white arrows) cement and organic matter (blue arrow) infill foram chambers. B) Elemental maps
from EDS analysis with distributions of Ca (calcite), Si (quartz and other silicates), and Mg (dolomite)

Foraminifers make up a substantial portion of the matrix grains in the Eagle Ford subsurface sample and
are commonly filled with diagenetic calcite, kaolinite, quartz, pyrite, and migrated organic matter. Forams
in the Eagle Ford are described having multiple chambers and including sizes up to hundreds of microns,
making approximately 10 - 80% of the depositional matrix Schieber et al [15]. Figure 4, 6, and 7 show
BSE images of authigenic minerals in the chambers of foraminifer tests. In Figure 4 (outlined by the white
square on the left), a foram chamber is predominantly filled with authigenic kaolinite in addition to traces
of organic matter in the kaolinite's intercrystalline pores. A higher resolution of the authigenic kaolinite in
Figure 5 shows minor crystals of pyrite (blue arrow) and feldspar (Al + Si minerals) (yellow arrow), and
later migrated organic matter filling kaolinite intercrystalline pores with triangular openings similar to those
described by Schieber et al [15].
8 SPE-195805-MS

Figure 4—A) BSE image of the LEF reservoir sample showing both calcite-filled (light gray) and calcite, kaolinite, and
organic matter filled foraminifer tests. B) Shows an enlargement of the calcite, kaolinite, and organic matter filled
foraminifer test outlined by the white box on the left and C) the elemental distribution maps from the field of view in (B).

Figure 5—Phyllosilicate intercrystalline pores (white arrows) observed within diagenetic kaolinite infilling foraminifer tests
SPE-195805-MS 9

Figure 6—A) BSE image of the LEF reservoir sample showing the distribution of foraminifer tests within the matrix,
some of which are fully occluded by calcite cement and B) an enlargement of the calcite cement, organic matter-
(dark) and pyrite-filled (white) foraminifer test. Note that the calcite cement in the foram has been brecciated
before infill with organic matter (yellow arrows). C) The elemental distribution maps from the field of view in (B).

Figure 7—A) BSE image showing various diagenetic minerals within foraminifer tests. Some are dominated
by calcite and others are dominated by kaolinite. B) This is an enlargement of the foraminifer test outlined by
the white square in (A). It initially is partially cemented by calcite, then that calcite is autoclastically brecciated
(yellow arrows), and then organic matter migrates in but only partially fills some of the pores. Notice the pores
on the upper right and base are fully occluded by organic matter. Those happen to be two pores with extensive
autoclastic brecciation of calcite. In contrast the pore in the upper left was not occluded by organic matter. This
cement in this pore happens to show less autoclastic brecciation. C) Element maps of (B) showing calcite (Ca
map), migrated and depositional organic matter (C map), depositional silicates (Si and Al map), and pyrite (S map).

In other fields of view, foraminiferal tests (Figure 6) show initial reduction by calcite cement, possibly
followed by framboidal pyrite. The forams and calcite cement show microbrecciation fabrics (yellow
10 SPE-195805-MS

arrows) consistent with compactional deformation of grains and cement. This is followed by migrated OM
filling the foram chambers and breccia pores. Pores in the organic matter (white arrows) range from ~ 40
nm to as large as ~ 200 nm and vary in 2D shape from circular to polygonal. Circular-shaped organic pores
in the chambers of the forams are reported to be indicative of gas bubbles originally formed in a liquid phase
[15]. In another part of the sample, a multi-chambered foram (Figure 7) showed infills of diagenetic calcite,
brecciation of that calcite (yellow arrows), and then migration of OM, but some of the original intraparticle
pore space is preserved.
Kerogen was observed (Figure 8 A) as depositional particles surrounded by matrix consisting of calcite,
pyrite, clay minerals, quartz, traces of dolomite, and albite. OM pores in kerogen are related to either
kerogen, solid bitumen or pyrobitumen [25]. An enlargement of a section of the kerogen (Figure 8 B) shows
organic pores (white arrows) ranging from approximately 100nm to 300nm.

Figure 8—A) Structured kerogen (OM) in matrix with depositional calcite (Ca map), pyrite (Fe map),
clay minerals (Al and Si map), quartz (Si map), OM (white arrows; C map) depositional grains and
between mineral pores. B) Shows an enlarged section of the kerogen with organic pores (white arrows)

EF Outcrop. BSE imaging of an outcrop sample (Figure 9) showed abundant calcite cement and
neomorphic microspar in addition to significant quartz content, low clay content, and dolomite from EDS
analysis. The diagenetic alteration observed in the outcrop sample is characterized by either depositional
fabrics or highly altered fabrics with diagenetic calcite cements and neomorphic microspar replacing
surrounding matrix minerals (Figure 9). Non-porous, depositional kerogen (white arrows in Figure 10 A)
in some cases contains micro-scale grains and crystals of clay, quartz, and carbonate grains and in other
cases is only organic matter. Most of the interparticle pores, ranging from ~ 70 nm - 200 nm, are filled with
organic matter, some of which may be depositional kerogen and some of which may be migrated organic
matter. Distinguishing between these two sources of organic matter is difficult at this scale (e.g. [26]). Other
interparticle pores remain empty. Patches of neomorphic spar and cement (blue arrows -Figure 11 A) are
observed to dominate the matrix of the outcrop in addition to solution-enlarged fractures (white arrows -
Figure 11 A andFigure 11 B), which tend to provide permeability pathways through the low permeability
patches.
SPE-195805-MS 11

Figure 9—A) BSE image of an EF outcrop sample composed mostly of "patches" of calcite surrounded by
matrix with calcite, quartz, clay minerals, and dolomite. B) EDS maps of Si (quartz and clays), Ca (calcite
and dolomite), Mg (dolomite), and Al (clay minerals) of the entire area in (A). Note that paches of calcite
do not show as only calcite in EDS maps. Thus, patches are poikilotopically including minerals other
calcite and likely neomorphically altering depositional calcite grains and cementing open pore space.

Figure 10—A) BSE image showing non-porous wispy seam of kerogen and particle of kerogen (white arrows)
embedded within mineral matrix grains (light gray). Note large patch of calcite consists of interlocking
crystals of calcite, each ~ 5-10 microns in size. Curved surface in bottom center of mass (black arrow) is
probably remnant of foram test. B) Shows an enlargement of the outlined white box showing the distribution
of calcite depositional grains, infills of organic matter, clay minerals, pyrite, and interparticle pores
12 SPE-195805-MS

Figure 11—A) BSE image showing solution-enlarged fractures (white arrows), microfractures (yellow arrow), and cemented
patches of neomorphic spar (blue arrows). B) Shows Shows an enlargement of the outlined white box showing the solution-
enlarged fractures (white arrows), pyrite framboid (black arrow), as well as organic matter filled foram (green arrow).

Some chambers in forams (Figure 12) were first partially cemented with calcite, then fractured, and then
occluded with OM. Structure of pores in this migrated organic matter differs markedly from that in the
subsurface sample. It contains crack-like shrinkage pores. The sample has traces of diagenetic quartz but
no diagenetic kaolinite. BSE image (Figure 12 A) shows a two-chambered foram, where the left chamber
shows compactional crushing or breakage before and after organic matter migration as a viscous fluid, and
then organic matter shrinkage.

Figure 12—A) Shows a two-chambered foram with the left chamber partially dissolved or abraded (white
arrows) and the right chamber filled with OM with a shrinkage pore. B) A single chambered foram with particles
of calcite filling the shrinkage pores. C) shows a two-chambered foram; left chamber is filled with OM and
calcite cement, while right chamber is almost fully filled with calcite cement and neomorphic microspar
replaces matrix. D) Shows a single foram containing organic matter, calcite cement, and shrinkage pores.

Doubly terminated quartz microcrystals were also observed within depositional kerogen (Figure 13)
suggesting that quartz crystal formation preceded bitumen migration into primary pores in depositional
kerogen.
SPE-195805-MS 13

Figure 13—Non-porous depositional kerogen containing euhedral quartz microcrystals, calcite, and
clay grains. Si map on the right is blow up of quartz microcrystals within the depositional kerogen

Reconstructed 3D Volumes
Approximately 106 slices were used to reconstruct 3D volumes (Figure 14). The darkest features represent
the lowest intensity areas (pores), dark features represent intermediate intensity phases (e.g., OM), and the
gray to lightest gray features represent the highest intensity mineral phases (e.g., calcite, quartz, pyrite).

Figure 14—Reconstructed 3D volumes of both the outcrop (left) and reservoir sample (right), respectively

Pore space analysis. A surface representation of the segmented pores, OM and matrix was used to calculate
the volume and surface area of each phase (Figure 15). The pores in the outcrop are made up of both organic
and inorganic pores, while the pores in the reservoir sample are mainly organic in origin. The segmented
organic pores in the reservoir sample appear mostly spherical in shape, whereas the segmented pores of the
outcrop come in varying shapes from tabular to fractures (Figure 15).
14 SPE-195805-MS

Figure 15—Surface view of a network of triangles representing segmented pores from both outcrop and reservoir sample

Specific surface area (SSA) was calculated as the ratio of the surface area (SA) to its bulk volume and is
given as 6.059 × 104 mm-1 for the subsurface sample and 3.122 × 104 mm-1 for the outcrop sample (Table 1).
SSA contributes to the adsorption of gas molecules in shales and also impacts the permeability. Assuming a
kerogen density of 1.3 g/cm3 [25], SSA is converted to the interface area per unit mass (IAPUM), which is
comparable to nitrogen (N2) Brunaeur-Emmett-Teller (BET) measurements [26]. The IAPUM of the outcrop
is estimated as 24.02 m2/g and that of the reservoir sample was twice as much as that of outcrop at 46.6 m2/g.

Table 1—Pore surface estimations for the outcrop and reservoir samples

Samples Surface Area (µm2) Volume (µm3) Porosity (vol. %) OM (vol. %)

EF Outcrop 99.9 3.2 3.6 8.3

LEF Reservoir 102.4 1.69 2.11 13.2

Pore and Pore Throat Size. The size of the pores and pore throats in the outcrop sample are larger than
that of the reservoir sample with considerable hydraulic length for flow (Table 2). This was understandable
since the generated PNM of the outcrop sample was a mixture of organic and inorganic pores, while the
PNM of the reservoir sample was predominantly organic pores, textures and mineral composition between
the two samples differed, and diagenetic fabrics differed.

Table 2—Statistics of pore network modeling for resampled pores of the outcrop and reservoir samples

Pore diameter Throat diameter

Samples Number of Pores Number of Throats Hydraulic length (nm)
range (nm) range (nm)

EF Outcrop 18,488 13,862 20 - 385 19 - 258 0.0000222 - 1246

LEF Reservoir 18,452 11,295 20 - 280 19 - 193 0.0000243 - 679

Pores identified in the 3D volumes of each sample were converted to PNMs where pores were represented
with spheres of similar diameter or size, while the throats are represented with rods of similar size (Figure
16).
SPE-195805-MS 15

Figure 16—Generated PNMs of the outcrop and reservoir sample, respectively. Pores are represented
by spheres, scaled by the volume of the pores, and color coded by the range of pore radius. Throats
are presented by rods, scaled by the hydraulic length and color coded by the radius of the throats

Aspect Ratio (AR). Aspect ratio is defined as the ratio of the pore size to the throat size; it controls
the distribution of fluids within a porous medium. It is related to the capillary trapping, where a non-
wetting phase may be trapped and becomes discontinuous in a pore space due to snap off resulting from
capillary forces. This phenomenon is favored by high aspect ratios as observed in both samples, but more
so the outcrop (Table 3). NMR 2D T1-T2 maps generated for the reservoir and outcrop samples to evaluate
gas huff-n-puff recovery, indicated trapped gas within the bound region (micro-pores) of both samples in
addition to gas adsorption onto the organic pores (meso-pores) as a result of these large aspect ratios [27].

Table 3—Pore-throat aspect ratio for both the reservoir and outcrop samples

Samples Min Max Mean

LEF Reservoir 1 14.63 1.706

EF Outcrop 1 20.01 1.749

Tortuosity. To calculate tortuosity at every point within the 3D volume using the geometric method, each
voxel was assigned a value depending on the distance to the nearest object boundary.Figure 17 shows
the tortuosity map estimated from the geodesic and Euclidean distance maps of the outcrop. The range of
tortuosity of the outcrop sample listed in Table 4 is from ~ 1.04 to 1.67.
16 SPE-195805-MS

Figure 17—Geometric tortuosity using the geodesic and Euclidean distance maps of the EF outcrop

Table 4—A range of geometric tortuosity variation in the x (flow direction) - and y- directions, respectively

Samples Tortuosity

Outcrop 1.04 - 1.67

Subsurface 1.04 - 2.36

On the other hand, the ratio of distance maps for the reservoir sample resulted in the tortuosity calculation
at every voxel (Figure 18) to range from 1.04 - 2.36 also listed in Table 4.

Figure 18—Geometric tortuosity estimated from the geometric

method applied to the segmented pores of the LEF reservoir sample
SPE-195805-MS 17

LBM Permeability
The 3D segmented pores of both the outcrop and reservoir samples with dimensions of 109 × 832 × 1466
voxels and 106 × 658 × 1222 voxels in the x, y, and z directions, respectively, were used as input for the
simulation domain in the LBPM. The predefined CV criteria of 0.001 was reached after 56,520 iterations
for the reservoir pore system and that of the same CV criteria was reached after 48,250 iterations for the
outcrop sample. Small pores with few voxels capable of creating spurious velocity were managed by creating
additional nodes. The resulting geometric permeability, which is dependent on only the geometry input for
both the outcrop and subsurface samples are 1.27 |iD and 0.71 |iD, respectively. This matches the lower
tortuosity range observed in the direction of flow for the outcrop.Figure 19 shows the velocity magnitude in
lattice units (lu) for both the outcrop and subsurface sample, whereby the outcrop shows a greater average
velocity (1.8e-5 lu/ts or 0.0107 m/s) than that of the subsurface (1e-5 lu/ts or 0.0059 m/s) due to significant
inorganic connecting pathways attributed to solution-enhanced microfractures.

Figure 19—3D view of LBPM simulated velocity distribution for both the outcrop (A) and the subsurface sample (B). White
arrows point to the pores with higher magnitude of velocity compared to small or isolated pores with little or no flow

Moreover, the resulting permeability from the LBM simulation was comparable to the pulse decay
permeability measurement provided by Chesapeake for the as-received LEF reservoir sample at 0.65 μD.

Conclusions
• The diagenetic history and dominant diagenetic textures of the outcrop sample differ from those
of the subsurface sample, leading to a differing pore systems.
• The outcrop sample shows calcite cement and quartz cement, and common compactional and
solution- enlarged microfractures, as well as isolated dolomite crystals. The calcite microspar is
nucleated in and around the foraminifera. It grows as cement in pores and as neomorphic microspar,
replacing the matrix poikilotopically. Organic matter migrates into primary pores after calcite
cementation and compactional fracturing. Organic matter develops shrinkage pores after migration.
After microfractures, solution enlargement enhances and opens the fractures.
• The subsurface sample has calcite cement, pyrite, authigenic kaolinite, quartz cement and
phosphatization. Compactional microfractures postdate calcite cementation and predate migration
of organic matter. After migration, organic matter develop pores of various types.
• Porosity in organic matter differs between the outcrop and subsurface sample. Porosity in organic
matter is better developed and more heterogeneous in the subsurface sample. This is ascribed to
18 SPE-195805-MS

the higher thermal maturity of the subsurface sample. Whereas, the organic pores in the forams
of the reservoir sample were typically circular in shape, those occurring in the outcrop samples
are tabular in shape.
• Multiple pore types observed in both samples include interparticle pores between the matrix grains,
intercrystalline pores within diagenetic kaolinite in the subsurface sample, intraparticle pores
within forams, and pores within OM.
• Digital rock analysis carried out on FIB-SEM reconstructed volumes and enabled the calculation of
SSA from the segmented pores represented with a network of triangles. SSA is known to contribute
to fluid adsorption in organic-rich shales and also impacts the estimated permeability. The interface
area per unit mass for the surface of reservoir pores is 46.6 m2/g, which is twice that of the outcrop
(24.02 m2/g). In addition, the pore size distribution of the generated PNMs is found to range from
~20 nm - 280 nm for the organic pores in the reservoir sample and ~ 20 - 385 nm for both the organic
and inorganic pores of the outcrop. Aspect ratio, defined as the ratio of the pore and the pore throat
size was calculated as 15:1 for the reservoir and 20:1 for the outcrop samples, respectively. These
differences are ascribed to the different diagenetic histories of the two samples and the different
thermal maturity.
• Tortuosity, which influences permeability and the diffusion of gas into the matrix at the matrix-
fracture interface, was estimated using the geometric method, where the outcrop has a lower range
(1.04 to 1.67) than the reservoir sample (1.04 to 2.36).
• The estimated permeability from LBPM shows the outcrop with less tortuous pathways to be more
permeable (1.27 pD) and with a greater average velocity of 0.0107 m/s than the reservoir sample
(0.7 pD, 0.0059 m/s) with isolated patches of organic pores. The higher permeability and greater
average velocity observed in the outcrop is attributed to significant solution-enlarged fractures
within compacted neomorphic spar and cement creating additional permeability pathways.

Acknowledgement
The authors would like to thank Chesapeake Energy for funding this work and providing the core plugs
and fluid samples, corresponding core data, and continuous feedback during the course of this project. Our
acknowledgement is extended to Kansas Interdisciplinary Carbonates Consortium (KICC) for providing
a platform for collaboration and for partially funding this project. We would like to thank Prem Thapa
(KU Imaging Lab) and Randy Polson (Utah NanoFab Lab) for their assistance in acquiring BSE/SEM/EDS
and FIB-SEM images, respectively. Thermofisher Scientific donated a one year license for PerGeos with
support and training. The open-source LBPM was developed by James McClure under the Open Porous
Media (OPM) platform.

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