Experimental Rock Physics under micro-CT
Nicola Tisato*, University of Texas at Austin, Jackson School of Geosciences, Texas, USA
Downloaded 10/18/16 to 189.122.24.58. Redistribution subject to SEG license or copyright; see Terms of Use at http://library.seg.org/
Qi Zhao, University of Toronto, Canada
Giovanni Grasselli, University of Toronto, Canada
Summary
Geophysical methods rely on the accurate determination of
physical and mechanical properties of rocks. These
properties are intimately related to rock microscopic features
such as pore shape and distribution, grain orientations, and
fluid distribution. The present contribution reports the
preliminary results obtained with a newly conceived high
pressure vessel which is paired with an X-ray micro-CT
system to investigate the influence of fluid distribution and
microstructural features on the physical and mechanical
properties of rocks, and in particular on seismic wave
attenuation and dynamic moduli.
Introduction
Geophysical methods rely on the effective rheological
behavior of geo-materials. The macroscopic (i.e. apparent)
rheology of rocks depends on microscopic features. For
instance, in granular porous media elasticity is not only
affected by the grain-pore distributions and orientation, but
also by the crack closures, and pore-fluid content and
distribution. During laboratory tests none of these aspects
can be easily observed, and often, this is possible only
through destructive analyses.
Among others, Tisato and Quintal (2013) demonstrated that
the non-uniform distribution of liquid and gas in sandstones
causes viscoelasticity, which in turn, subtracts a substantial
amount of energy from a propagating seismic wave (i.e.,
causes attenuation). However, the authors were unable to
compare the calculated and the real fluid distribution as their
apparatus lacked an “in-situ” analytical tool to visualize this
aspect. Similarly, Tisato et al. (2015) demonstrated that
microscopic bubbles dispersed in saturated porous media
cause seismic velocity dispersion and attenuation. But again,
the authors were unable to image “in-situ” and “in-
operando” the presence of such bubbles.
Many natural and anthropogenic activities cause
thermodynamic disequilibria in subsurface domains (i.e.
physical property variations), which induce variations in the
signals recorded by a contingent geophysical monitoring.
For instance, carbon sequestration is believed to cause the
dissolution and/or precipitation of mineral phases in crustal
rocks (Adam et al., 2013). However, how these interactions
affect physical properties is still conjectural because of the
inability of performing laboratory experiments and
concurrently “see” the evolution and response of the sample
© 2016 SEG
SEG International Exposition and 86th Annual Meeting
interior. This limitation could be overcome by employing X-
Ray tomography as lately it become a versatile, accessible
and effective technique to image materials and their
saturating phases (Ketcham and Carlson, 2001).
Here we report the design and the preliminary measurements
of dynamic moduli and seismic wave attenuation in
Plexiglas and Berea sandstone that have been obtained by
means of a new X-Ray transparent pressure vessel (ERDμ)
which can perform measurements inside the X-ray micro-CT
system installed at the University of Toronto (μCT). We also
present CT-datasets for dry and partially saturated Berea
sandstone, focusing on the estimation of the local saturation
through the analysis of the CT imagery.
The improvement and the fine tuning of the machine
presented here will allow for measuring physical property
changes in the sample (e.g. seismic wave attenuation) and,
simultaneously, link them to saturation variations, or
precipitation-dissolution of minerals. This technological
development and the results obtained will improve our
understanding of rock-physics, opening new avenues for
exploration geophysics.
Materials and Methods
The X-ray transparent vessel, which is mainly used to
measure seismic wave attenuation, has a vertical
electromechanical actuator, which applies the vertical stress
on the specimen. Such actuator is mounted in series with a
piezoelectric motor (PZT), which is controlled by a high
voltage amplifier, and capable of generating a sinusoidal
variation of the vertical stress. This force oscillation is
necessary to estimate the complex Young’s modulus (E’),
which is calculated according to the amplitudes of the
sinusoidal stress and strain. In fact, a load cell placed
between the PZT and the sample (Fig. 1B) measures the
sinusoidal force. The deformation across the sample is
measured by strain gauges which are directly glued on the
specimen and connected to Wheatstone bridges. The
machine can acquire deformations from two Wheatstone
bridges, thus allowing us to measure extensional and
transversal deformation. This can be achieved by gluing a
vertical and a horizontal strain gauge on the external surface
of the sample, respectively. The sample is covered with thin
layer of epoxy glue to avoid viscoelastic phenomena related
to open-boundary conditions (Dunn, 1986), and isolated
from the confining medium by means of a plastic jacket.
Page 3251
 The data acquisition system (i.e. amplifiers and analog-to-
digital converter) have been calibrated in order to easily
Downloaded 10/18/16 to 189.122.24.58. Redistribution subject to SEG license or copyright; see Terms of Use at http://library.seg.org/
convert the electric signals to strain/force signals. The
vertical stress is calculated according to the force measured
by the load cell and the sample nominal cross-section. The
attenuation related to the Young’s modulus (1/QE or simply
1/Q) can be calculated as: 1/Q = tan(φ), where φ is the phase
shift between the sinusoidal stress and strain (Lakes, 2009).
On the other hand, the Poisson’s ratio can be estimated
computing the ratio between the horizontal and vertical
strain.
As the apparatus is equipped with a hydraulic circuit, it is
possible to vary the confining pressure (P c) between 0 and
30 MPa, the pore pressure between 0 and 20 MPa, and inject
in the sample precise fluid volumes (V in). The primary
objective is to measure attenuation before and after injection
of brine and CO2, which will cause dissolution and/or
precipitation of mineral phases, to better understand the
impact of microstructural and saturation variations on the
rock viscoelasticity. For instance, we could relate the fluid
distribution with the variation of attenuation measured
between dry and saturated conditions gaining insights in the
Wave-Induced-Fluid-Flow (WIFF) theory (Müller et al.,
2010).
We measured attenuation and Young’s modulus of
Aluminum alloy (not shown here) and Plexiglass (PMMA)
samples. Testing on these materials are meaningful to
calibrate the system. We also measured attenuation and
Young’s modulus of a Berea sandstone sample while dry and
partially saturated with water. Measurements were acquired
at Pc ranging between 0.7 and 2 MPa. The tested Berea
sandstone sample (sample 7v) has permeability ~100 mD,
weight 8.456 g, porosity ~17%, length 34.03±0.02 mm and
diameter 11.99±0.05 mm. Weight, porosity and dimensions
of the sample were measured by means of a 0.1 mg accuracy
scale, a helium pycnometer and a 0.01 mm accuracy caliper,
respectively. The pore space volume of sample 7v is
Vpores~0.58 ml.
CT-dataset were acquired employing the GE Phoenix
v|tome|x CT-scan installed at the Department of Civil
Engineering at the University of Toronto. ERDμ was
mounted on a 5-axis rotation stage and irradiated with X-
rays on its external curved surface by rotating it 360° in 1080
equally spaced increments. At each angle, 5 projections were
acquired and averaged to obtain a 2D 16-bit gray scale
projection. The chosen magnification of the specimens
within the field of view corresponded to a voxel resolution
of 37 µm. Voltage, current and exposure time utilized during
acquisition were 100 kV, 250 μA and 800 ms, respectively.
Image reconstruction was performed using the Pheonix X-
ray datos—x-reconstruction software (v. 1.5.0.22).
© 2016 SEG
SEG International Exposition and 86th Annual Meeting
Reconstruction produced an image stack formed by 1024
grey scale images with dimensions of 1018 by 1018 pixels.
Sample 7v was saturated up to 80% injecting water through
its bottom surface. During such a process X-ray
radiographies were acquired with a frame rate of 2 FPS
(frame per second) to capture the dynamic movement of the
imbibition front in the sample (Fig. 2).
Figure 1. A) ERDμ pressure vessel apparatus to measure dynamic
moduli and seismic wave attenuation inside the GE Phoenix
v|tome|x CT-scan system installed at the University of Toronto. The
pressure vessel (3) is mounted on the CNC stage between the X-Ray
source (1) and the X-ray detector (2) (i.e. CCD and scintillator). B)
Berea Sandstone sample mounted between the sample holders
before jacketing and closure of the vessel. The sample is equipped
with semiconductor strain gages to accurately measure the dynamic
shortening or strain. Below the sample and the bottom sample holder
there is a load cell made of 17-4 PH stainless steel on which 4 strain
gages are mounted forming a Wheatstone bridge whose electric
signal is used to estimate the force. Force and strain signals are
acquired by amplifiers and an analog-to-digital converter, which is
mounted on the control board indicated by (4) in panel A. Data are
transferred to a PC, which is installed outside the CT cabinet,
through USB connection (see also Tisato et al., 2014).
After imbibition, the saturation profile was estimated
comparing the CT-imagery acquired at wet conditions with
that acquired at dry conditions. To correct for gray scale
shifts, caused for instance by intrinsic µCT drifts, the gray
scale average of a volume of the datasets that did not change
after imbibition (i.e. a volume outside the sample such as the
space between the sample jacket and the external surface of
the vessel) were compared. In fact, the 16-bit gray scale
dataset of the wet sample was shifted of -59, which
represents -0.09% of the gray scale full-scale. We assumed
constant porosity along the vertical axis of the sample and
no position shift between the two datasets (i.e. the same
voxel was recorded at the same position during the two
acquisitions). Given such assumptions we subtracted the wet
Page 3252
 and dry datasets creating a dataset resembling the gray scale red arrow in each frame. The injected volume of water was Vin~0.23
shift caused by the presence of water in the pore space ml, making the total saturation Sw~40%.
Downloaded 10/18/16 to 189.122.24.58. Redistribution subject to SEG license or copyright; see Terms of Use at http://library.seg.org/

(saturation dataset). Finally, we i) isolated from the

saturation dataset a portion of the rock sample (i.e. 31.45 mm
in length and 11 mm in diameter) and ii) divided such sub-
volume in N=85 vertical subdomains. For each subdomain,
which was penny shaped (i.e. 370µm in thickness and 11
mm in diameter), we calculated the average of the gray scale
shift producing a gray scale shift vertical profile (GSS(z)),
where z is the number of vertical subdomain (i.e. 1≤z≤85).
Assuming the overall saturation, 𝑆𝑤𝑡 = 𝑉𝑖𝑛 ⁄𝑉𝑝𝑜𝑟𝑒𝑠 and
𝑆𝑤(𝑧) ∝ 𝐺𝑆𝑆(𝑧) (Landis and Keane, 2010), we can write:
𝑆𝑤𝑡 = 𝑎 ∑𝑁 𝑧=1 𝐺𝑆𝑆(𝑧)⁄𝑁, which allows calculating the
constant a and the vertical saturation profile as: 𝑆𝑤(𝑧) =
𝑎 𝐺𝑆𝑆(𝑧) (Fig. 3).

Figure 3. X-Ray imagery showing the gray levels of the dry (A) and
wet (B) Berea sandstone. The injected volume of water for the wet
dataset was Vin~0.23 ml, making the total saturation Sw~40%.
Longitudinal sections are shown in panels 3 and 6, while transversal
sections are shown in panels 1, 2 and 4, 5. Notice that after
imbibition the bottom part of the sample exhibits higher increase of
gray levels into respect the upper part of the sample (i.e. compare
the increase of gray level between panel 1 and 4 versus that between
panel 2 and 5). Panel 7 shows the estimated saturation profile.

Results

CT-data

The X-ray datasets collected show that the newly designed

Figure 2. X-Ray radiographies of the Berea sandstone sample during
injection of water through the bottom sample holder. Acquisition
frame rate was 2 FPS. Images acquired at time t>0 sec are displayed
as difference between the frame acquired at time t and that acquired
at time t=0 sec to enhance any variation. Such a device allows
observing the position of the imbibition front, here indicated by the
vessel, whose irradiated part is made of aluminum alloy
(7075-T6), allows to effectively image the enclosed sample.
In particular, there is no significant evidence of noise or
artefacts introduced by the high pressure vessel body. X-ray
radiographies, which were acquired during the saturation
process, show that the newly conceived apparatus allows
observing, in real-time, the imbibition process (Fig. 2 and 3).

© 2016 SEG Page 3253

SEG International Exposition and 86th Annual Meeting
 Especially in the bottom part of the sample, CT imagery
acquired for saturated conditions exhibit higher gray values
Downloaded 10/18/16 to 189.122.24.58. Redistribution subject to SEG license or copyright; see Terms of Use at http://library.seg.org/
than that acquired for dry conditions, this allows estimating
the saturation profile (Fig. 3).
Figure 4. A) Signals showing vertical stress-variation (σn) and strain
(ε), which are typically used to estimate the dynamic Young’s
modulus (E) and the seismic wave attenuation (1/Q). B)
Measurements of E and 1/Q for dry (curve 1) and 80% water
saturated Berea sandstone (curves 2 and 3). Confining pressure was
0.7 MPa for curves 1 and 2, and 2 MPa for curve 3. Curves 4 report
measured E and 1/Q for Plexiglas (PMMA) in agreement with the
literature (Lakes, 2009 and Tisato and Madonna, 2012).
Dynamic Young’s modulus and seismic wave attenuation
Calibration of ERDµ was performed measuring Aluminum
alloy and Plexiglas. We collected five cycles of
measurements for 45 frequencies logarithmically distributed
between 0.1 and 100 Hz. The five repetitions are used to
estimate the repeatability error which is ~0.003 rad for
attenuation and ~0.1 GPa for Young’s modulus. The error
© 2016 SEG
SEG International Exposition and 86th Annual Meeting
estimated from: 1) the accuracy of the electronic circuits and
2) the electrical noise is ~0.001 rad for 1/QE and 0.01 GPa
for Young’s modulus. Our calibration shows that ERDμ can
measure extensional attenuation between 0.01 and 0.1 rad
with a total error ~0.004, and dynamic Young’s modulus
between 3 and 70 GPa with an error ~0.1 GPa (Fig. 4). In
particular, the measurement of attenuation for the PMMA
agrees with the data published by Lakes (2009) and Tisato
and Madonna (2012) that were acquired with independent
apparatuses.
Attenuation measurements performed in sample 7v do not
show frequency dependence and significant difference
between dry and wet conditions (Fig. 4). We speculate that
the high permeability and small dimension of the sample
would cause frequency dependent attenuation related to
wave induced fluid flow at much higher frequencies than
those tested during our tests (Müller et al., 2010). In
additions, measurements above 25 Hz (not shown here) were
affected by a resonance which drastically decreased the
measurement precision. Such a resonance was probably
generated by sample wobbling which can be solved by
improving the sample preparation (e.g. improving the end-
faces parallelism). Nevertheless, measurements of dynamic
Young’s modulus show i) decrease after imbibition, which
is typical for sandstones and often attributed to the
intergranular cement softening (Mavko et al., 2009), and ii)
increase as confining pressure increases (Fig. 4).
Conclusions
ERDµ allows i) observing and estimating water saturation in
Berea sandstone samples and concurrently ii) measuring
dynamic Young’s modulus and seismic wave attenuation.
However, fine tuning is still necessary to obtain improved
results. ERDµ will help investigating further the
relationships between saturation and effective elastic
properties. This achievement will aid the monitoring of
subsurface domains, for instance, to link the evolution of the
elastic parameters to the observed changes in the internal
structure of the investigated sample (e.g. dissolution or
precipitation of minerals caused by CO2 injection), to help
inferring changes in subsurface domains that are imaged
with geophysical methods.
Acknowledgments
Our work has been supported by the Swiss National Science
Foundation (SNSF) and Carbon Management Canada
(CMC). We thank Jeff Sansome for technical support,
Ronny Hoffman and Luca Duranti for helpful indications
about the ERDµ design
Page 3254
 EDITED REFERENCES
Note: This reference list is a copyedited version of the reference list submitted by the author. Reference lists for the 2016
SEG Technical Program Expanded Abstracts have been copyedited so that references provided with the online
metadata for each paper will achieve a high degree of linking to cited sources that appear on the Web.

REFERENCES
Downloaded 10/18/16 to 189.122.24.58. Redistribution subject to SEG license or copyright; see Terms of Use at http://library.seg.org/

Adam, L., K. Van Wijk, T. Otheim, and M. Batzle, 2013, Changes in elastic wave velocity and rock
microstructure due to basalt-CO2-water reactions: Journal of Geophysical Research: Solid Earth,
118, 4039–4047, http://dx.doi.org/10.1002/jgrb.50302.
Dunn, K.-J., 1986, Acoustic attenuation in fluid-saturated porous cylinders at low frequencies: The
Journal of the Acoustical Society of America, 79, 1709–1721,
http://dx.doi.org/10.1121/1.393232.
Ketcham, R. A., and W. D. Carlson, 2001, Acquisition, optimization and interpretation of X-ray
computed tomographic imagery: Applications to the geosciences: Computers and Geosciences,
27, 381–400, http://dx.doi.org/10.1016/S0098-3004(00)00116-3.
Lakes, R. S., 2009, Viscoelastic materials: Cambridge University Press,
http://dx.doi.org/10.1017/CBO9780511626722.
Landis, E. N., and D. T. Keane, 2010, X-ray microtomography: Materials Characterization, 61, 1305–
1316, http://dx.doi.org/10.1016/j.matchar.2010.09.012.
Mavko, G., T. Mukerji, and J. Dvorkin, 2009, The rock physics handbook: Tools for seismic analysis of
porous media (2nd ed.): Cambridge University Press,
http://dx.doi.org/10.1017/CBO9780511626753.
Müller, T. M., B. Gurevich, and M. Lebedev, 2010, Seismic wave attenuation and dispersion resulting
from wave-induced flow in porous rocks — A review: Geophysics, 75, no. 5, 75A147–75A164,
http://dx.doi.org/10.1190/1.3463417.
Tisato, N., and C. Madonna, 2012, Attenuation at low seismic frequencies in partially saturated rocks:
Measurements and description of a new apparatus: Journal of Applied Geophysics, 86, 44–53,
http://dx.doi.org/10.1016/j.jappgeo.2012.07.008.
Tisato, N., and B. Quintal, 2013, Measurements of seismic attenuation and transient fluid pressure in
partially saturated Berea sandstone: Evidence of fluid flow on the mesoscopic scale: Geophysical
Journal International, 195, 342–351, http://dx.doi.org/10.1093/gji/ggt259.
Tisato, N., B. Quintal, S. Chapman, C. Madonna, S. Subramaniyan, M. Frehner, E. H. Saenger, and G.
Grasselli, 2014, Seismic attenuation in partially saturated rocks: Recent advances and future
directions: The Leading Edge, 33, 640–646, http://dx.doi.org/10.1190/tle33060640.1.
Tisato, N., B. Quintal, S. Chapman, Y. Podladchikov, and J.-P. Burg, 2015, Bubbles attenuate elastic
waves at seismic frequencies: First experimental evidence: Geophysical Research Letters, 42,
3880–3887, http://dx.doi.org/10.1002/2015GL063538.

© 2016 SEG Page 3255

SEG International Exposition and 86th Annual Meeting