SPE-192666-MS

Three-Phase Flow Visualization and Characterization for a Mixed-Wet

Carbonate Rock

Alessio Scanziani, Amer Alhammadi, Branko Bijeljic, and Martin J. Blunt, Department of Earth Science and
Engineering, Imperial College London

Copyright 2018, Society of Petroleum Engineers

This paper was prepared for presentation at the Abu Dhabi International Petroleum Exhibition & Conference held in Abu Dhabi, UAE, 12-15 November 2018.

This paper was selected for presentation by an SPE program committee following review of information contained in an abstract submitted by the author(s). Contents
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Abstract
A novel method is presented to characterise in situ three-phase flow, including wettability, pore occupancy
and displacement mechanisms, at the pore scale. We used X-ray microtomography to obtain 3D images
of a carbonate reservoir rock saturated with crude oil and formation brine at subsurface conditions. The
sample had been aged with crude oil from the same reservoir to replicate the sunsurface wetting conditions.
The pore occupancy analysis shows that brine is non-wetting to oil and gas is non-wetting to brine with
a wettability order of oil-brine-gas from the most to the least wetting fluid. The waterflood recovery after
1 pore volume injected was only 14%, but this increased to 48% after further gas injection. New multiple
displacement mechanisms were observed, with gas displacing brine, which in turn displaces oil. The results
from this work can be used to improve the prediction accuracy of the three-phase network models and helps
in the design of gas injection processes.

Introduction
Three-phase flow is observed in many processes, such as enhanced oil recovery (Figuera et al., 2014;
Masalmeh et al., 2014; Rao, 2001), carbon geosequestration (Godec et al., 2011; Jessen et al., 2005), non
aqueous contaminant removal from aquifers, and fuel-cell optimization (Blunt, 2017). Field and centimetre
scale studies of three-phase flow are already present in literature, but a limited number of studies have been
performed at the pore scale. However, the miscroscopic fluid configurations control larger-scale properties
such as relative permeabilities and fluid saturations.
Relative permeability - the contribution that each phase give to the total flow - controls the prediction
of reservoir-scale models (Juanes et al., 2006). Relative permeability has been studied in three-phase flow
experiments at the core scale (Di Carlo et al., 2000; Iglauer et al., 2009; Oak, 1991; Shahverdi et al., 2011).
These core-scale studies showed how, in a water-wet medium, the relative permeabilities of brine and gas
depend only on their own saturations, while oil relative permeability depends also on the saturation of the
other two fluids. This behaviour has been explained through consideration of pore occupancy, related to
wettability: in a water-wet medium, water is the most wetting phase, and hence it was thought to occupy the
smallest pores, while gas - being the least wetting phase - should reside in the centre of the biggest pores.
2 SPE-192666-MS

Oil, instead, has an intermediate wettability and is displaced by the other phases into pores of intermediate
size: for this reason, its relative permeability is also influenced by the saturation of water and gas.
Recent studies have been performed on three-phase flow at the pore scale, using X-ray microtomography.
Some studies (Iglauer et al., 2016, 2013) focused on the analysis of the study of the optimal injection strategy,
highlighting differences in systems with different wettabilities. Other researchers (Khishvand et al., 2016)
studied the effect of local contact angles (i.e. wettability) on multiple displacement mechanisms.
To complement these studies, we have used pore-scae imaging to quantify pore occupancy, capture
double displacement processes and the trapping of oil and gas, relating these to the wettability of the system
(Scanziani et al., 2018). This suite of tools was applied on a water-wet carbonate rock sample, saturated
with model brine, oil and gas.
In this work, we present the application of this new methodology to a more representative system,
consisting of a carbonate sample extracted from a very large producing oil field that is saturated with
prepared formation brine and crude oil from the same reservoir. Nitrogen was used as a gas phase in a
three-phase immiscible displacement process at subsurface pressure and temperature. The rock, prior to
the experiment, was aged with crude oil to establish a mixed-wet wettability state that is known to exist in
hydrocarbon reserovirs (Alhammadi et al., 2017a).
Our study shows how different wettability conditions could lead to complex pore-scale processes, with
altered oil recovery, gas storage, phase connectivity, pore occupancy and displacement mechanisms.

Materials and methods

Rock and fluids
The experiments were performed on a carbonate reservoir rock sample, with a diameter of 4.8 mm and
length of 14.6 mm. Table 1 shows that the rock is made mostly of calcite with minor quantities of kaolinite
and quartz. The mini-core was drilled from a cleaned carbonate reservoir core plug, in a location where the
plug presented a fairly uniform pore distribution without very large impereamble grains that could seal off
the flow or very large vugs that can result in non-represetative porosity and a fragile sample. To select a
representative drilling location, the whole core-plug was scanned at a resolution of 36 μm/voxel and the
distribution of pores and grains was investigated. A light crude oil (density 830 ± 5 kg/m3 at 21 °C) from
the same reservoir was used. The crude oil composition is shown in Table 1 and the crude oil was doped
with 20% by mass 1-iododecane (Sigma-Alddrich, UK) to increase the phase contrast allowing for effective
image segmentation. The doping percentage was selected based on contrast scans that were performed
before the experiment to select the optimal amount of dopant. The prepared formation brine (Alhammadi et
al., 2017b) was doped with 3% potassium iodide (Sigma-Alddrich, UK). The third phase was pure nitrogen,
immiscible with both brine and oil. The X-ray attenuation was lowest for nitrogen, followed by brine and
oil and was highest for rock, as shown in Figure 1.

Table 1—Mineralogical composition of the reservoir rock

Phase Phase proportion (weight %) Estimated error (weight %)

Calcite 98.1 1.0

Kaolinite 1.2 0.9

Quartz 0.7 0.3

Measured by the Natural History Museum, London.

SPE-192666-MS 3

Table 2—Crude oil composition

Weight %

Saturates 55.25

Aromatics 38.07

Resins 6.22

Asphaltenes 0.46

Measured by Weatherford Labs (UK), Birches Industrial Estate, East Grinstead RH19 1XZ.

Figure 1—2D slices of the reconstructed 3D images of the rock after gas injection (GI). The good contrast between the
four phases can be seen in both the images with resolution of 5μm (A) and 2μm (B and C) per voxel side. A. A horizontal
cross-sectoinal view of the whole sample. B. A cropped subvolume highlighting the three phases and C. The arrangement
of the three phases in a pore where contact angles between oil and water and gas and water have been measured.

Ageing and flow experiment

Prior to performing water flooding and gas injection, the rock was aged to replicate the native wettability
state of the reservoir. The ageing protocol of the mini-samples in a carbon fibre coreholder has been
developed by Alhammadi et al, (2017b) and is able to effectively alter the wettability of carbonate reservoir
rocks to establish a mixed-wet state (Alhammadi et al., 2017b; AlRatrout et al., 2018). The sample was first
scanned dry with an XRadia Versa XRM-520 micro-CT scanner to check the rock quality. The sample was
cleaned by a injecting solvent mixture of 50/50 by weight of methanol and toluene (Gant and Anderson,
1988). The sample was then dried under vacuum. After drying, the sample was placed in a carbon fibre
Hassler-type flow cell (Alhammadi et al., 2017a). After applying a confining pressure of 1.5 MPa, the
sample was flushed with CO2 at a low flow rate to remove any air in the pore spaces. The CO2 flush was
followed by the injection of 200 pore volumes of brine at a flow rate of 0.3 mL/min to fully saturate the rock
with brine: any trapped CO2 would dissolve in the brine. At this stage subsurface condtions were established
at a temperature of 76 ± 1 °C and a pore and confining pressure of 8.0 MPa and 9.5 MPa respectively.
Ageing was performed by oil injection (OI) at these subsurface conditions to establish the reservoir initial
conditions. The polar compounds of the crude oil with heavier mass fractions are known to interact with
the rock surfaces resulting in the adsorption of an organic layer onto the rock surfaces which alters the
rock surfaces from water-wet to be more oil-wet at the surfaces that are in direct contact with crude oil
(Alhammadi et al., 2017b; Buckley et al., 1998; Salathiel, 1973; Sayyouh et al., 1991).
OI was performed for a total of 20 pore volumes at 0.015 mL/min, and then the flow rate was reduced to
0.01 mL/min and dynamic aging was performed, injecting 10 PV of oil every day for 5 days, to continuosly
supply polar compounds to speed up the wettability alteration (Ferno et al., 2010). The sample was then left
in the oven for static ageing for further 3 weeks, with a total ageing period of 4 weeks.
4 SPE-192666-MS

The experiment then consisted of a sequence of injections of the three fluids, scanning the sample
after each injection, with the flow stopped, using both a resolution of 3.5 μm/voxel side covering the
full field of view, and a zoomed-in scan at a resolution of 2 μm/voxel side covering a cylindrical field
of view with a diameter of 2 mm at the centre of the sample. The confining pressure and temperature
were kept constant at 10 MPa and 60°C during the whole water injection and gas inection experiment,
using the pumps (Teledyne Isco, Lincoln, NE, USA) and a heating jacket dynamically controlled using
a proportional-integral-derivative (PID) controller and a thermocouple placed in the core holder, next to
the sample. The first scan sequence was performed at the end of ageing (oil injection, OI), then brine was
injected (waterflooding, WF) at a flow rate of 0.01 mL/min, corresponding to a capillary number of 10-7,
ensuring a capillary-dominated regime. One pore volume of brine was injected and then the system was left
to reach equilibrium over 2 hours to avoid interface relatxation and fluid rearrangement during scanning.
Gas injection (GI) was then performed at the same flow rate, for a total of 8 PV followed by scanning.

Image analysis
Example 2D slices of the 3D images obtained can be seen in Figure 1. The good contrast between the four
phases (gas, brine, rock and oil) can be observed, along with the details provided by the higher resolution
images.
The images were processed using a non-local-means filter to increase the signal to noise ratio (Buades et
al., 2008), then the voxels of the images were assigned to the four phases employing image segmentation.
Seeded watershed (Jones et al., 2007) and machine learning WEKA (Arganda-Carreras et al., 2017) methods
were used for segmentation depending on the dimension of the images, as WEKA is more precise in
segmenting the interfaces but processing large images requires excessive computer memory. Segmented
images were used to obtain the saturation of the four phases after each injection step for the whole
sample using watershed segementation, while to visualise displacement in the higher-resolution images we
employed WEKA segementation.
Pore occupancy - the relationship between the dimension of the pores and the phase in their centre -
was computed using the segmented images. The methodology for obtaining pore occupancy is described in
Scanziani et al. (2018) and consists of using a maximum ball (MB) algorithm (Raeini, et al., 2017) to obtain
a set of spheres representing the centre of the pores, then computing the median value of the voxels defined
by each sphere. This allows to associate each sphere to a phase and hence obtain a relationship between the
dimension of the pores (defined as the equivalent radius of the MBs) and the phase residing in its centre.

Results
Wettability
A closer look at the images of Figure 1 can give an indication of the wettability of the aged rock. The
curvature of the brine/oil interface at the location zoomed in Figure 1C shows how, at least in that pore,
oil and brine are wetting and non-wetting phase respectively, as the interface bulges into the oil phase. The
same consideration can be made looking at the interfaces between gas and brine: in the same pore, the
curvature of the gas/brine interface bulges into the brine phase, meaning that gas is non-wetting to brine
for that pore. This leads to a wettability order of oil-brine-gas, with the oil being the most wetting phase,
brine the intermediate and gas the most non-wetting phase. According to Blunt (2017), this behaviour is
typical of a weakly oil-wet system.
A more precise characterization and quantification of wettability can be obtained with the direct
measurement of contact angles. We first performed manual measurements (Andrew et al., 2014) as shown in
Figure 1C. The contact angle of 112° between oil and water (measured through the water) confirms a weakly
oil-wet system and the contact angle of 35° between brine and gas (measured through the brine) confirms
that brine is wetting to gas. In other locations we see locally regions that appear more water-wet. A complete
SPE-192666-MS 5

quantification of wettability has been obtained using the automatic method developed by Scanziani et al.,
(2017): in Figure 2, the distribution of contact angles measuered through water after OI are both above and
below 90°, with a mean value of 103°. Hence, we will describe this system as being mixed-wet.

Figure 2—Probability density function of the contact angle between oil and water (θow) computed
with the method described in (Scanziani et al., 2017) from a subset of the high resolution image
after oil injection (OI). The average contact angle is indicated at the top-left side of the graph.

Saturations
Segmented images were used to compute the saturation of each phase, after each injection step. The
saturations were computed dividing the number of voxel assigned to the selected phase by the total number
of voxels assigned to the pore space. Table 1 shows the saturations after each injection step. One pore volume
of brine injection gave only 14% oil recovery, while 8 pore volumes of gas injection increased it to 48%.
This shows how gas injection may be an effective enhanced oil recovery strategy for mixed-wet systems.
In the water-wet system studied in Scanziani et al., (2018), the oil recovery after GI was 51%.

Table 3—Saturations at the end of each injection.

OI WF GI

Oil 59.8% 51.5% 31.1%

Brine 40.2% 48.5% 10.1%

Gas - - 57.8%

Measured with image analysis.

Pore occupancy
Pore occupancy was investigated using the procedure described in the methods section. The results are
shown in Figure 3. In this mixed-wet case, brine occupies the centre of the largest pores, while oil resides
in the smallest ones, with an opposite behaviour to what happens for the Ketton water-wet rock studied in
Scanziani et al., (2018). This is a confirmation of the successful alteration of the wettability during ageing,
leading to a change in the nature of the WF process, now becoming a drainage process, with a non-wetting
phase invading the sample where capillary barriers prevent entry into the smallest pores, as shown in an
example in the next section.
6 SPE-192666-MS

Figure 3—Histograms showing how the phases are distributed in pores as a function of pore diameter (pore occupancy).
Solid green, dashed blue and point-dotted red lines are associated respectively to oil, brine and gas. The left figure
shows the occupancy after waterflooding (WF), while the right figure shows the occupancy after gas injection (GI).

The results after GI give an indication of the wettability to gas, and it is clear how, as in water-wet
rocks, gas resides in the centre of biggest pores, consisitent with the measurement of contact angle. Brine
is pushed by the invading gas and, moving towards smaller-sized pores, in turn displaces oil, allowing for
its production, with the double displacement described in the next section.

Pore-scale displacement events

To better understand displacement processes, we cut a small subset from the high resolution images and
improved its segmentation using the machine learning WEKA algorithm which accurately captures the
shape of the trapped phases. We then obtained 3D visualisations of the pore space and the arrangement of
the three phases within it after OI, WF and GI (Figure 4). These images are useful to see how water invades
some of the larger pores in WF as the non-wetting phase, leaving connected oil retained in the majority
of the pore space. It is likely that recovery would improve on further brine injection. An interesting event
occurred in the circled throat, which was occupied by oil after OI, and hence is likely to have experienced
a wettability alteration. The oil is not displaced from the throat with WF, as the non-wetting brine phase
has insuffiicent capillary pressure to invade it. It can also be seen how the 3D curvature of the oil/brine
interface confirms oil as the wetting phase.

Figure 4—3D renderings of gas (red), brine (blue) and oil (green) phases after OI,
WF and GI, inside a small subvolume extracted from the high resolution images.
SPE-192666-MS 7

After GI the 3D images show a multiple displacement mechanism: in this system, gas has displaced brine
which has displaced oil, consistent with their wettability order. Gas competes with brine for the centre of
bigger pores, as shown in Figure 3, and hence directly contacts brine, which is pushed towards the smaller
pores, occupied by oil, with a consequent double displacement mechanism of gas displacing brine displacing
oil. As indicated by the dashed circle in Figure 4, some brine remains in the smaller pores after OI and
remains there throughout the displacement, forming a layer between oil and gas.

Conclusions
We have imaged three-phase flow in situ at the pore scale in a mixed-wet carbonate reservoir rock at
subsurface conditions. We characterised the mixed-wet sample in terms of saturation, pore occupancy and
wettability order. We observed that: (i) oil is the most wetting phase in most of the pore space, residing in the
smallest pores, with a negative curvature with brine, and a contact angle between oil and brine, measured
through the brine, that is higher than 90°; (ii) gas is the most non-wetting phase, residing in the largest
pores, with a positive curvature with brine, and a contact angle between gas and brine, measured through
brine, that is lower than 90°; and (iii) brine is the intermediate phase, as it resides in the largest pores in the
presence of oil and brine only but still competes with oil for the smallest pores when gas is injected.
This wettability state has consequences for oil recovery, which is low (14%) after the injection of 1 PV of
brine and increases to 48% with the injection of 8 PV of gas. The wettability order also influences the pore
scale displacements, which differ from those observed in a water-wet system as now gas directly contacts
brine instead of oil, and the main double displacement observed is gas displacing brine displacing oil. This
work is useful for a further development of pore-network models and aids in the understanding and design
of enhanced oil recovery processes.
Future work will study a wider variety of rocks and wettabilities, and employ automatic contact angle
measurement methods to obtain the full distribution of angles in the pore space (AlRatrout et al., 2017;
Scanziani et al., 2017).

Acknowledgements
We thank Abu Dhabi National Oil Company (ADNOC) for funding this work and permission to publish
this paper.

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