Fuel xxx (2013) xxx–xxx

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Fuel
journal homepage: www.elsevier.com/locate/fuel

Characterization of oil shale pore structure before and after pyrolysis

by using X-ray micro CT
P. Tiwari a,1, M. Deo a,⇑, C.L. Lin b, J.D. Miller b
a
Department of Chemical Engineering, University of Utah, Salt Lake City, UT 84112, United States
b
Department of Metallurgical Engineering, University of Utah, Salt Lake City, UT 84112, United States

h i g h l i g h t s

" Effect of temperature on oil shale pyrolysis and product distribution.

" Pore structure analysis of raw and pyrolyzed shale.
" Heterogeneity in the sample and its effect on pyrolysis process.
" Permeability estimation using Lattice Boltzmann simulation.

a r t i c l e i n f o a b s t r a c t

Article history: The pyrolysis of oil shale to produce transportation fuels is a complex process. The organic matter in the
Received 23 August 2012 oil shale is tightly bound with a heterogeneous mineral matrix. Several physical changes occur during the
Received in revised form 29 December 2012 thermal conversion of kerogen in oil shale to produce hydrocarbon products. The creation of pore space
Accepted 3 January 2013
during pyrolysis is an important physical process which determines the flow behavior of the pyrolysis
Available online 21 January 2013
products and the ultimate recovery. In this paper, we report the effect of temperature (350–500 °C) on
oil shale pyrolysis and creation of pore volume during thermal treatment. One inch diameter oil shale
Keywords:
cores from different depths of a single drill hole in the Uinta Basin were used. Increase in the pyrolysis
Oil shale
Pyrolysis
temperature resulted in higher weight loss and a corresponding increase in the oil yield. Three-dimen-
Pore scale analysis sional X-ray micro tomography (XMT) was performed to characterize and to analyze the nature of the
Permeability pore network structure before and after pyrolysis. XMT scans of the cores at 42 lm voxel resolution dis-
played distinguishable features of reaction products and source rock. Unconstrained pyrolysis of organic
rich core produced large pore space during thermal treatment. The three-dimensional pore network
structure was established with pores as large as 500 lm developed after pyrolysis. Lattice Boltzmann
simulation of flow through the developed pore network structure suggested that permeabilities from
173 Darcy to 2919 Darcy can be expected.
Ó 2013 Elsevier Ltd. All rights reserved.

1. Introduction
Oil shale resources can be used primarily for producing trans-
portation fuels. The fuel production from these resources requires
an understanding of processes that occur over a wide range of
length and time scales. Pyrolysis of oil shale produces oil, gas
and coke. The reaction progress depends on the process time and
temperature. The products are formed and create a pore structure
in the shale. The fluid products, oil and gas, flow through the pore
channels while coke formation blocks pores. The fluid flow result-
⇑ Corresponding author.
E-mail address: Milind.Deo@utah.edu (M. Deo).
1
Present address: Department of Chemical Engineering, Indian Institute of
Technology, Guwahati, India.
ing from the kerogen decomposition is of interest in our current re-
search. The pore structure and the connectivity of the pore space
are important features which determine fluid flow. The pore struc-
ture created influences the reaction within particles and flow char-
acteristic of oil and gas products. Study of the nature of pores and
subsequent permeability are required. The nitrogen adsorption and
desorption isotherms on the Green River oil shale properties have
been reported [1]. The adsorption technique has also been used to
estimate pore properties from microwave retorting [2] and pore
structure changes during combustion [3] of Chinese oil shales
and eastern US oil shale [4]. The application of X-ray micro tomog-
raphy (XMT) to describe thermal cracking of Fussion oil shale un-
der different temperatures was reported [5]. Lee et al. [6]
reported the relation of bulk density of the rock to computed
tomography (CT) number and oil yields using X-ray tomography

0016-2361/$ - see front matter Ó 2013 Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.fuel.2013.01.006

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2 P. Tiwari et al. / Fuel xxx (2013) xxx–xxx

for Australian oil shales. A study on the characterization of oil shale

using X-ray tomography before and after pyrolysis has also been
reported in the literature [7].
We report results of the pyrolysis of the Green River oil shale at
different temperatures and provide a description of the pore struc-
ture created during pyrolysis. Cores of oil shale were pyrolyzed at
different temperatures. The effect of pyrolysis temperature on the
creation of pore space during the process was studied. Multiscale
three-dimensional (3D) high resolution X-ray micro tomography
(HRXMT) scanning was performed on the raw and pyrolyzed sam-
ples to understand the nature of the pore networks created during
thermal treatment. The Lattice Boltzmann method (LBM) was used Fig. 1. Green River core sections subjected to isothermal pyrolysis under different
on digitalized pore structure to estimate flow properties, such as temperatures.
absolute permeabilities for different pore network structures.

Table 3
Summary of GR core samples pyrolysis. The data were normalized based on initial
2. Materials and methods
weight.

The organic and inorganic compositions of oil shale vary from R core ID Temp. (°C) Weight loss (%)
one geological environment to another. To address this variability GR-1 1a 350 7.08
in resource composition and its effect on the pyrolysis product dis- 1b 425 25.91
1c 500 33.74
tribution, three fresh organic rich (Mahogany zone) samples from
GR-2 2c 350 2.84
core taken from the Uinta Skyline 16 well were used in this study. 2a 425 9.61
The samples were within the depth range of 461.1 to 548.9 feet. 2b 500 12.26
These samples were identified as GR-1 (461.1–462.1 feet), GR-2 GR-3 3b 350 2.54
(485.9–486.9 feet) and GR-3 (548.1–549.1 feet). 3c 425 18.40
3a 500 17.17

2.1. Elemental analyses

et al. [8]. The method at the University of Utah uses toluene rather
Uniformly mixed powdered (100 mesh) oil shale samples of GR- than benzene in the separation process.
1, GR-2 and GR-3 were used to perform materials characterization.
The crushed samples were dried for four hours at 100 °C to remove
moisture. There was no significant weight loss during drying, and 2.2. Pyrolysis of core samples
hence the samples were used as received after screening to
100 mesh. The samples had different appearances in color and The one-inch diameter cores from GR-1 (461.2–461.7 feet), GR-
were suspected to contain different amounts of organic matter. 2 (485.9–486.4 feet) and GR-3 (548.2–548.7 feet) were used for
Elemental analyses of the three core samples are shown in Table 1. pyrolysis. Each core (approximately, 600 long) was divided into
Elemental analyses were performed by a commercial laboratory three sections (Fig. 1) to perform the isothermal pyrolysis. The
(Huffman Laboratories, Inc.). Total carbon was determined fol- resulting cores were about two inches long and 30–60 g in weight.
lowed by acid-wash CO2, which provided the inorganic carbon. Continuous flow isothermal experiments at 350 °C, 425 °C and
The organic carbon was calculated by difference. The elemental 500 °C were conducted with hot N2 flow (approximately, 100 ml/
analyses of the isolated kerogens (KR), also performed at a com- min). The cores were packed into a reactor so that they would be
mercial laboratory are shown in Table 2. The demineralization able to expand both vertically and radially. A heating rate of
was carried out by a team at the University of Utah. It was a 100 °C/min was used to achieve the reaction temperature, where
nine-step procedure based on the method developed by Vandegrift the core was held for 24 h. The temperature of the reactor surface
was used to control the pyrolysis temperature. Temperature pro-
files were recorded at three points; reactor surface, core surface,
Table 1 and at the center of the core. The steady state temperature differ-
Elemental analysis of the shale samples from the three different cores. ence between reactor surface and center of the core was about
GR-1 GR-2 GR-3 50 °C. The condensable product was collected in a series of two
Hydrogen 2.71 1.52 2.19
condensers held at 6 °C. The weight loss results are shown in
Total carbon 25.44 17.66 20.25 Table 3. Cores with the highest organic content show the highest
Tot CO2 as C 5.17 7.33 4.79 losses as expected and weight loss increases with temperature.
Organic carbon 20.27 10.33 15.46 In experiments at the higher temperatures, weight loss exceeds
Nitrogen 0.73 0.34 0.65
the weight percent organic. The moisture content and bound water
Oxygen 16.94 21.85 16.46
Sulfur 0.83 0.29 0.95 in clays and minerals in the shale may have resulted in this
phenomenon.

Table 2
Elemental analysis of isolated kerogens from GR samples. KR-1, KR-2 and KR-3 are the kerogens separated from GR-1, GR-2 and GR-3.

Sample ID C (%) H (%) N (%) S (%) O (%) Ash (%) Drying loss (%) H/C (molar) O/C (molar)
KR-1 73.27 9.27 2.62 1.9 7.64 5.3 0.77 1.52 0.08
KR-2 73.96 9.49 2.45 1.87 7.64 4.6 0.39 1.54 0.08
KR-3 73.22 9.14 2.43 3.57 7.78 3.87 0.54 1.50 0.08

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 P. Tiwari et al. / Fuel xxx (2013) xxx–xxx 3

2.3. Multiscale X-ray micro tomography
X-ray micro computed tomography (XMT) is the best non-inva-
sive non-destructive method to characterize complex pore struc-
tures. The cone beam XMT system provides 3D visualization,
characterization and analysis of multiphase systems at a voxel
(volume element) resolution of 10 lm which corresponds to the
ability to describe mineral structure and composition of multi-
phase particles having a size on the order of 100 lm [10]. Tradi-
tional XMT systems use microfocus X-ray source to achieve a
small source spot size combined with a minimal distance between
sample and source. The high-resolution X-ray micro tomography
(HRXMT) system from Xradia (model micro XCT-400) employs an
X-ray detector with sub-micron resolution combined with a micro
focus X-ray source which corresponds to a voxel resolution of 1 lm
and with advanced X-ray optics is able to describe particles having
a size on the order of 10 lm. In this system the working distance
between source, sample and detector is typically around
100 mm. Full tomography for larger samples can be achieved. In
this way 3D pore network structures of cores before and after pyro-
lysis have been characterized non-invasively using the HRXMT
imaging technique [11].
2.4. Lattice Boltzmann method (LBM)
The Lattice Boltzmann method (LBM) has received attention in
order to simulate fluid flow in porous media [12,13]. The LBM has
become an emergent mathematical technique able to handle the
complex boundary conditions for flow in porous structures such
as oil shale samples in a reasonable amount of time. This method
incorporates molecular level interactions and structure which
facilitates code parallelization. It is also becoming popular for its
capabilities to incorporate additional physical complexities such
as multicomponent and multiphase flow [14]. The LBM [15–21]
is based on a ‘bottom-up’ approach where constructed kinetic
models incorporate microscopic model interactions and mesoscop-
ic kinetic equations so that the macroscopic averaged properties of
the flow obey the desired macroscopic equations. The resulting
macroscopic dynamic behavior is the result of the collective behav-
ior of the microscopic particles in the system. The use of computer
simulation allows the calculation of macro variables, such as abso-
lute and relative permeabilities of the flow [22]. Videla et al. [22]
describe in detail the fundamentals aspects of LBM and its applica-
tion for the analysis and determination of permeability for packed
particle beds of limestone, sand, and rock particles. The same
methodology was used in this work to examine the effect of oil
shale core pore structure on fluid flow. HRXMT images were used
for the Lattice Boltzmann simulations to calculate permeabilities
generated due to pyrolysis of organic matter.
3. Results and discussion
3.1. Characterization of oil shale
The differences in organic carbon (please see Table 1) in the
three samples highlight the level and nature of heterogeneity in
the samples. GR-1 has almost twice the organic carbon as GR-2
and about 1.33 times that of GR-3. GR-2 has the lowest sulfur con-
tent possibly due to the low organic content. The hydrogen to car-
bon ratios of the kerogen samples are remarkably similar in the
1.5–1.54 range. These ratios are consistent with extensive data
on Green River oil shale that is available in the literature [9]. Sulfur
appears concentrated in the kerogens. High sulfur content in KR-3
is consistent with the high sulfur content seen in the core GR-3.
3.2. Pyrolysis of core samples
The purpose of this paper is to discuss porosity changes due to
pyrolysis. More detailed pyrolysis results are available elsewhere
[23]. In general, the weight loss increased with temperature.

Fig. 2. Photographs of the spent shales from pyrolysis of the three Green River shale samples. Core 1 corresponds to the GR-1 sample, core 2 to GR-2 and core 3 to GR-3. The
core richest in the organic content (GR-1) essentially crumbles due to the decomposition of the organic matter. The leanest of the core (GR-2) remains intact and retains its
original appearance. The core with the intermediate organic content (GR-3) displays intermediate characteristics with respect to deformation as well.

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Fig. 3. Tri-planar image of GR-1 sample (core 1b). The pyrolysis was performed at 425 °C. This sample contained about 20% organic matter. Large amounts of kerogen are
converted and pore space is generated. The pore space generated is patchy and is consistent with the initial kerogen distribution along the bedding in the core. The pore space
measured was 26%.

Weight loss at 350 °C was minimal and in some experiments at the Table 4
highest temperature of 500 °C, the weight loss exceeded the organ- Comparison of calculated porosities and those measured using the X-ray micro
ic content in the core. The oil quality improved as the temperature tomography (XMT). The GR-1 core had the highest amount of organic matter at about
20%.
increased (oil produced was lighter).
Photographs of the spent shales from isothermal pyrolysis of Porosity Calculated Experimental
the different sections of the three cores are shown in Fig. 2. The Conversion 60% 80% 100% GR-1b GR-1c
cores of higher organic content (GR-1) during high temperature Porosity 20% 28% 36% 26% 21%
(500 °C) pyrolysis showed more deformation than the cores

Fig. 4. Effect of the pyrolysis (425 °C) on GR-1 (core 1b) sample. Based on the relative position of mineral grains inside the core 1b, three slice pairs from 3D CT images were
identified at the same positions along the core before and after pyrolysis at 425 °C.

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 P. Tiwari et al. / Fuel xxx (2013) xxx–xxx
Fig. 5. 3D views of LB simulated flow along x-axis through the reconstructed
HRXMT image of core 1b samples at a reaction temperature of 425 °C with
transparent solid phase to reveal flow channels (pore network structure after
pyrolysis).
pyrolyzed at lower temperatures (350 °C) and organic lean cores
(GR-2). The core with the highest organic content crumbles while
the leanest one stays close to its original. The overall patterns are
consistent with those observed by Duvall et al. [24].
3.3. Porosity changes within core geometry
Selected pieces of these nine GR samples were scanned using
HRXMT. Characterization of the texture change during pyrolysis
was analyzed based on the comparison of the same sections of
cores before and after pyrolysis. Fig. 3 shows the tri-planar image
for pyrolyzed core-1b (pyrolysis temperature 425 °C). Large
amounts of pore space are generated as evidenced by the dark
patches observed in the images. The pore space generated is un-
even however and corresponds as expected to the original distribu-
tion of kerogen in the core.
Fig. 6. Tri-planar image of GR-1 sample (core 1c). The pyrolysis was performed at 500 °C. The pore space created in locations where kerogen existed. The porosity measured
was 21%.
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5
It is possible to estimate to amount of porosity generated and
compare the values with those measured using the HRXMT. This
comparison is shown in Table 4. The porosity values in Table 4
were calculated for core GR-1 at three different possible kerogen
conversion values. Density of the inorganic matter in the shale
was assumed to be 2.65 g/cc, the density of kerogen was consid-
ered to be 0.98 g/cc and the coke density used was 1.2 g/cc. For
each conversion value, it was assumed that 60% was converted to
liquid, 20% to coke and 20% to gas. It was assumed that all of the
coke formed deposited in the pore space created by the reacting
kerogen. The cores undergo thermal expansion. Duvall et al. [24]
describe the linear expansion of oil shale cores in great detail. They
show that it is difficult to establish the exact amount of expansion
because of the settling and crumbling of the oil shale cores. This is
particularly true of the richer shales. It is even more difficult to
establish the relative increase in porosity due to thermal expan-
sion. Most of the normalized thermal expansion values for cores
of a variety of grades ranged from 3% to 5% in the data shown by
Duvall et al. [24]. In Table 4, a relative increase in porosity of 1%
is assumed at 425 °C and 3% at 500 °C. Comparison of the porosities
in Table 4 show that the calculated and measured porosities are
similar in magnitude. The porosity at a higher pyrolysis tempera-
ture of 500 °C is expected to be higher than at 425 °C, but is mea-
sured to be lower. This was primarily due to the settling of the core
as large amounts of organic matter are removed. The settling was
observed visually. The uncertain aspects of how and where the
coke deposition actually take place also might affect these
porosities.
As expected, pores were generated along the kerogen-rich lay-
ers. Based on the relative position of mineral grains inside core
GR-1b, as shown in Fig. 4, three slice pairs from the 3D images
were identified at the same positions along the core before and
after pyrolysis at 425 °C. Before pyrolysis, the distance between
the top (7 4 7) and bottom (6 9 8) layers was 49 voxels or
2041.83 lm (voxel resolution 41.67 lm). After pyrolysis, the dis-
tance between the top (2 7 8) and bottom (2 2 2) layers increased
to 56 voxels or 2333.52 lm (voxel resolution 41.67 lm due to
creation of pores during pyrolysis, the length of core increased
by 291.69 lm with a corresponding 14.3% increase in length.
6 P. Tiwari et al. / Fuel xxx (2013) xxx–xxx

Before Pyrolysis- Core 1c After Pyrolysis- Core 1c

227 123

235 143

Fig. 7. Effect of the pyrolysis (500 °C) on GR-1 (core 1c) sample. Based on the relative position of mineral grains inside the core 1c, two slice pairs from 3D CT images were
identified at the same positions along the core before and after pyrolysis at 500 °C.

This increase is higher than the ones reported by Duvall et al. [24] Fig. 8 shows the 3D views of LB simulated flow along the x-axis
except for their richest sample perpendicular to the bedding plane. through the reconstructed HRXMT image of core GR-1c samples.
The percentage increase for that sample was about 20%. Fig. 4 also The estimated permeability after pyrolysis at 500 °C was about
shows the heterogeneous distribution of the organic matter in the 1.71  106 cm2 or 173 Darcy. The estimated permeability is some-
shale which corresponds to the pore space created in the core. The what consistent with the visual observation of pore space for this
absolute permeability was determined based on coupling with LB sample. With the generation of higher amount of oil, one may have
simulation using the HRXMT data subset obtained for regions con- expected higher permeability generation for this sample, which is
taining more cracks from core GR-1b. Fig. 5 shows the 3D views of not the case. The flow channels do appear better connected in this
LB simulated flow along the x-axis through the reconstructed case, however.
HRXMT image of core GR-1b samples. Once the solid phases are re- Figs. 9 and 10 show the tri-planer images for the high temper-
moved, the right panel of Fig. 5 shows the nature of the flow chan- ature (500 °C) pyrolysis of GR-2 and GR-3 samples respectively.
nels. The velocity scale is color-coded as shown by the color bar The organic lean (or mineral rich) GR-2 samples showed a small
(lattice unit) in Fig. 5. The estimated permeability after pyrolysis extent of pore generation even at the highest temperature of
at 425 °C was about 2.88  105 cm2 or 2919 Darcy.
Fig. 6 shows the tri-planar image for pyrolyzed core GR-1c
(pyrolysis temperature 500 °C). The pore space generated is ob-
served to be patchy despite the higher pyrolysis temperature.
The two slice pairs from the 3D images were identified at the same
positions along the core before and after pyrolysis at 500 °C (Fig. 7).
Before pyrolysis, the distance between the top (2 3 5) and bottom
(2 2 7) layers was 8 voxels or 333.36 lm (voxel resolution
41.67 lm). After pyrolysis, the distance between the top (1 4 3)
and bottom (1 2 3) layers was 20 voxels or 833.4 lm (voxel resolu-
tion 41.67 lm). The length of the core increased by 500.04 lm dur-
ing the pyrolysis. This corresponds to an increase in length of 24%
which is consistent with the observations of Duvall et al. [24] for
the richest sample perpendicular to the bedding plane. The fact
that we see a larger thermal expansion is consistent with our
expectation of higher thermal expansion at higher temperatures.
Qualitatively, there is no significant difference between the images
at 500 °C and at 425 °C. One would expect to observe higher
amount of pore space based on the higher amount of oil generated
Fig. 8. Three-dimensional views of LB simulated flow along x-axis through the
at 500 °C, but that is really not the case. At this temperature the reconstructed HRXMT image of core GR-1c samples at a reaction temperature of
coke formed might be obscuring the pore space or the start of 500 °C with transparent solid phase to reveal flow channels (pore network structure
the mineral decomposition process may also have an effect. after pyrolysis).

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 P. Tiwari et al. / Fuel xxx (2013) xxx–xxx 7

Fig. 9. Tri-planar image of GR-2 sample (core 2b). The pyrolysis was performed at 500 °C. This was the leanest of the samples containing about 10% organic matter. The pore
space created is not easily visible.

Fig. 10. Tri-planar image of GR-3 sample (core 3a). The pyrolysis was performed at 500 °C. This sample contained about 15% organic matter. Concentration of the organic
matter in certain locations and thus creation of localized pore space in those locations are observed.

500 °C. In the GR-3 samples (intermediate organic content) direc-
tional cracks were created during pyrolysis. It is important to note
the non-uniformity of the pore space created and the resultant
unconnected permeability.
4. Conclusions
The results show that the samples within a single core had sig-
nificant variations in composition. During pyrolysis different sec-
tions of cores released different amounts of organic matter,
creating different amounts of void space. The channels formed dur-
ing the pyrolysis are also likely to affect the ultimate product for-
mation and distribution. Characterization of the textural change
during pyrolysis was accomplished from HRXMT analysis and
based on comparison of the same core sections before and after
pyrolysis for kerogen-rich cores (GR-1b and GR-1c) at different
reaction temperatures (425 °C and 500 °C). Porosities of 20–25%
were measured using the XMT. Absolute permeabilities of the re-
acted cores, GR-1b and GR-1c (kerogen-rich) for Skyline 16 core
samples after pyrolysis reactions at different temperatures were
calculated based on the pore network structure from HRXMT

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8 P. Tiwari et al. / Fuel xxx (2013) xxx–xxx
analysis coupled with LB simulation. Pyrolysis of organic rich core
at high temperature produced larger pore space during thermal
treatment. The HRXMT scans of these cores at 42 lm voxel resolu-
tion allowed for reaction products and source rock to be distin-
guished and spatially resolved. The porosity created was highly
patchy and depended on the distribution of kerogen in the shale.
The resultant flow channels created may not be fully connected.
Acknowledgements
The authors would like to acknowledge financial support from
the U.S. Department of Energy, National Energy Technology Labo-
ratories (US DOE Award Number: DE-FE0001243). Support from
various members of the Institute for Clean and Secure Energy
(ICSE) and the Petroleum Research Center (PERC) at the University
of Utah is also gratefully acknowledged.
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