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Experimental Rock Physics under micro-CT

Nicola Tisato*, University of Texas at Austin, Jackson School of Geosciences, Texas, USA
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Qi Zhao, University of Toronto, Canada


Giovanni Grasselli, University of Toronto, Canada

Summary interior. This limitation could be overcome by employing X-


Ray tomography as lately it become a versatile, accessible
Geophysical methods rely on the accurate determination of and effective technique to image materials and their
physical and mechanical properties of rocks. These saturating phases (Ketcham and Carlson, 2001).
properties are intimately related to rock microscopic features
such as pore shape and distribution, grain orientations, and Here we report the design and the preliminary measurements
fluid distribution. The present contribution reports the of dynamic moduli and seismic wave attenuation in
preliminary results obtained with a newly conceived high Plexiglas and Berea sandstone that have been obtained by
pressure vessel which is paired with an X-ray micro-CT means of a new X-Ray transparent pressure vessel (ERDμ)
system to investigate the influence of fluid distribution and which can perform measurements inside the X-ray micro-CT
microstructural features on the physical and mechanical system installed at the University of Toronto (μCT). We also
properties of rocks, and in particular on seismic wave present CT-datasets for dry and partially saturated Berea
attenuation and dynamic moduli. sandstone, focusing on the estimation of the local saturation
through the analysis of the CT imagery.
Introduction
The improvement and the fine tuning of the machine
Geophysical methods rely on the effective rheological presented here will allow for measuring physical property
behavior of geo-materials. The macroscopic (i.e. apparent) changes in the sample (e.g. seismic wave attenuation) and,
rheology of rocks depends on microscopic features. For simultaneously, link them to saturation variations, or
instance, in granular porous media elasticity is not only precipitation-dissolution of minerals. This technological
affected by the grain-pore distributions and orientation, but development and the results obtained will improve our
also by the crack closures, and pore-fluid content and understanding of rock-physics, opening new avenues for
distribution. During laboratory tests none of these aspects exploration geophysics.
can be easily observed, and often, this is possible only
through destructive analyses. Materials and Methods

Among others, Tisato and Quintal (2013) demonstrated that The X-ray transparent vessel, which is mainly used to
the non-uniform distribution of liquid and gas in sandstones measure seismic wave attenuation, has a vertical
causes viscoelasticity, which in turn, subtracts a substantial electromechanical actuator, which applies the vertical stress
amount of energy from a propagating seismic wave (i.e., on the specimen. Such actuator is mounted in series with a
causes attenuation). However, the authors were unable to piezoelectric motor (PZT), which is controlled by a high
compare the calculated and the real fluid distribution as their voltage amplifier, and capable of generating a sinusoidal
apparatus lacked an “in-situ” analytical tool to visualize this variation of the vertical stress. This force oscillation is
aspect. Similarly, Tisato et al. (2015) demonstrated that necessary to estimate the complex Young’s modulus (E’),
microscopic bubbles dispersed in saturated porous media which is calculated according to the amplitudes of the
cause seismic velocity dispersion and attenuation. But again, sinusoidal stress and strain. In fact, a load cell placed
the authors were unable to image “in-situ” and “in- between the PZT and the sample (Fig. 1B) measures the
operando” the presence of such bubbles. sinusoidal force. The deformation across the sample is
measured by strain gauges which are directly glued on the
Many natural and anthropogenic activities cause specimen and connected to Wheatstone bridges. The
thermodynamic disequilibria in subsurface domains (i.e. machine can acquire deformations from two Wheatstone
physical property variations), which induce variations in the bridges, thus allowing us to measure extensional and
signals recorded by a contingent geophysical monitoring. transversal deformation. This can be achieved by gluing a
For instance, carbon sequestration is believed to cause the vertical and a horizontal strain gauge on the external surface
dissolution and/or precipitation of mineral phases in crustal of the sample, respectively. The sample is covered with thin
rocks (Adam et al., 2013). However, how these interactions layer of epoxy glue to avoid viscoelastic phenomena related
affect physical properties is still conjectural because of the to open-boundary conditions (Dunn, 1986), and isolated
inability of performing laboratory experiments and from the confining medium by means of a plastic jacket.
concurrently “see” the evolution and response of the sample

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SEG International Exposition and 86th Annual Meeting
The data acquisition system (i.e. amplifiers and analog-to- Reconstruction produced an image stack formed by 1024
digital converter) have been calibrated in order to easily grey scale images with dimensions of 1018 by 1018 pixels.
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convert the electric signals to strain/force signals. The


vertical stress is calculated according to the force measured Sample 7v was saturated up to 80% injecting water through
by the load cell and the sample nominal cross-section. The its bottom surface. During such a process X-ray
attenuation related to the Young’s modulus (1/QE or simply radiographies were acquired with a frame rate of 2 FPS
1/Q) can be calculated as: 1/Q = tan(φ), where φ is the phase (frame per second) to capture the dynamic movement of the
shift between the sinusoidal stress and strain (Lakes, 2009). imbibition front in the sample (Fig. 2).
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).
Figure 1. A) ERDμ pressure vessel apparatus to measure dynamic
We measured attenuation and Young’s modulus of moduli and seismic wave attenuation inside the GE Phoenix
Aluminum alloy (not shown here) and Plexiglass (PMMA) v|tome|x CT-scan system installed at the University of Toronto. The
samples. Testing on these materials are meaningful to pressure vessel (3) is mounted on the CNC stage between the X-Ray
calibrate the system. We also measured attenuation and source (1) and the X-ray detector (2) (i.e. CCD and scintillator). B)
Young’s modulus of a Berea sandstone sample while dry and Berea Sandstone sample mounted between the sample holders
partially saturated with water. Measurements were acquired before jacketing and closure of the vessel. The sample is equipped
at Pc ranging between 0.7 and 2 MPa. The tested Berea with semiconductor strain gages to accurately measure the dynamic
shortening or strain. Below the sample and the bottom sample holder
sandstone sample (sample 7v) has permeability ~100 mD,
there is a load cell made of 17-4 PH stainless steel on which 4 strain
weight 8.456 g, porosity ~17%, length 34.03±0.02 mm and gages are mounted forming a Wheatstone bridge whose electric
diameter 11.99±0.05 mm. Weight, porosity and dimensions signal is used to estimate the force. Force and strain signals are
of the sample were measured by means of a 0.1 mg accuracy acquired by amplifiers and an analog-to-digital converter, which is
scale, a helium pycnometer and a 0.01 mm accuracy caliper, mounted on the control board indicated by (4) in panel A. Data are
respectively. The pore space volume of sample 7v is transferred to a PC, which is installed outside the CT cabinet,
Vpores~0.58 ml. through USB connection (see also Tisato et al., 2014).

CT-dataset were acquired employing the GE Phoenix After imbibition, the saturation profile was estimated
v|tome|x CT-scan installed at the Department of Civil comparing the CT-imagery acquired at wet conditions with
Engineering at the University of Toronto. ERDμ was that acquired at dry conditions. To correct for gray scale
mounted on a 5-axis rotation stage and irradiated with X- shifts, caused for instance by intrinsic µCT drifts, the gray
rays on its external curved surface by rotating it 360° in 1080 scale average of a volume of the datasets that did not change
equally spaced increments. At each angle, 5 projections were after imbibition (i.e. a volume outside the sample such as the
acquired and averaged to obtain a 2D 16-bit gray scale space between the sample jacket and the external surface of
projection. The chosen magnification of the specimens the vessel) were compared. In fact, the 16-bit gray scale
within the field of view corresponded to a voxel resolution dataset of the wet sample was shifted of -59, which
of 37 µm. Voltage, current and exposure time utilized during represents -0.09% of the gray scale full-scale. We assumed
acquisition were 100 kV, 250 μA and 800 ms, respectively. constant porosity along the vertical axis of the sample and
Image reconstruction was performed using the Pheonix X- no position shift between the two datasets (i.e. the same
ray datos—x-reconstruction software (v. 1.5.0.22). voxel was recorded at the same position during the two
acquisitions). Given such assumptions we subtracted the wet

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SEG International Exposition and 86th Annual Meeting
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%.
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(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 vessel, whose irradiated part is made of aluminum alloy
injection of water through the bottom sample holder. Acquisition (7075-T6), allows to effectively image the enclosed sample.
frame rate was 2 FPS. Images acquired at time t>0 sec are displayed In particular, there is no significant evidence of noise or
as difference between the frame acquired at time t and that acquired artefacts introduced by the high pressure vessel body. X-ray
at time t=0 sec to enhance any variation. Such a device allows radiographies, which were acquired during the saturation
observing the position of the imbibition front, here indicated by the process, show that the newly conceived apparatus allows
observing, in real-time, the imbibition process (Fig. 2 and 3).

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Especially in the bottom part of the sample, CT imagery estimated from: 1) the accuracy of the electronic circuits and
acquired for saturated conditions exhibit higher gray values 2) the electrical noise is ~0.001 rad for 1/QE and 0.01 GPa
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than that acquired for dry conditions, this allows estimating for Young’s modulus. Our calibration shows that ERDμ can
the saturation profile (Fig. 3). 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
Figure 4. A) Signals showing vertical stress-variation (σn) and strain properties. This achievement will aid the monitoring of
(ε), which are typically used to estimate the dynamic Young’s subsurface domains, for instance, to link the evolution of the
modulus (E) and the seismic wave attenuation (1/Q). B) elastic parameters to the observed changes in the internal
Measurements of E and 1/Q for dry (curve 1) and 80% water structure of the investigated sample (e.g. dissolution or
saturated Berea sandstone (curves 2 and 3). Confining pressure was precipitation of minerals caused by CO2 injection), to help
0.7 MPa for curves 1 and 2, and 2 MPa for curve 3. Curves 4 report inferring changes in subsurface domains that are imaged
measured E and 1/Q for Plexiglas (PMMA) in agreement with the
with geophysical methods.
literature (Lakes, 2009 and Tisato and Madonna, 2012).

Acknowledgments
Dynamic Young’s modulus and seismic wave attenuation
Our work has been supported by the Swiss National Science
Calibration of ERDµ was performed measuring Aluminum Foundation (SNSF) and Carbon Management Canada
alloy and Plexiglas. We collected five cycles of (CMC). We thank Jeff Sansome for technical support,
measurements for 45 frequencies logarithmically distributed Ronny Hoffman and Luca Duranti for helpful indications
between 0.1 and 100 Hz. The five repetitions are used to about the ERDµ design
estimate the repeatability error which is ~0.003 rad for
attenuation and ~0.1 GPa for Young’s modulus. The error

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SEG International Exposition and 86th Annual Meeting
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.

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