Effect of Temperature and Pressure on
Contact Angle and Interfacial Tension
of Quartz/Water/Bitumen Systems
M. Rajayi and A. Kantzas, University of Calgary
Summary
Thermal-recovery methods (e.g., steam injection) are commonly
used to recover bitumen from oil sands. The injected steam contacts
the oil sand and forms an interface. The steam changes to water,
transferring its heat to bitumen across this interface. The heated bi-
tumen will have a lower viscosity, which allows for oil to be mobi-
lized and recovered from the reservoir.
Studies that explain hot-water/bitumen interfaces are crucial
for understanding thermal-recovery methods. The strength and en-
ergy of hot-water/bitumen interfaces are expected to play important
roles in the recovery of bitumen from oil sands. However, measure-
ments on hot-water/bitumen interfaces are scarce in the literature.
A relevant measurement would be the contact angle and interfacial
tension (IFT) of the water/bitumen interfaces at different tempera-
tures. In this paper, it has been attempted to reveal and present the
results of several water/bitumen contact-angle and IFT measure-
ments. The measurements cover a temperature range from ambient
to 100oC for a given pressure.
The experiments are run in X-ray transparent cells, and images
are taken using a microcomputed-tomography (microCT) scanner.
The results of contact angle and the IFTs of the hot-water/bitumen
interface are produced by using the axisymmetric drop shape-anal-
ysis (ADSA) method.
Introduction
Thermal recovery of bitumen causes numerous changes in oil-sand
reservoirs and in fluid properties (viscosity, density of each fluid,
and IFT and wettability of the aqueous/hydrocarbon and rock/fluid
interfaces). The changes in these properties affect the production of
the oil sand; therefore, it is important to study them.
Wettability measurement in the oil-recovery industry is quite
popular, and several different methods have been used to charac-
terize the wettability of different reservoirs. These methods are
reviewed in detail by Anderson (1986). They are generally catego-
rized in two major groups: qualitative and quantitative methods.
Common qualitative methods for wettability measurement are im-
bibition rates, microscope examination, flotation, glass-slide method,
relative permeability curves, permeability/saturation relationships,
capillary pressure curves, displacement capillary pressure, reservoir
logs, nuclear magnetic resonance (NMR), and dye adsorption.
Quantitative methods include contact angle, spontaneous and
forced imbibition (Amott), and USBM-wettability method. Ac-
cording to Anderson (1986), the contact-angle method is used to
measure the wettability of a certain surface, while the Amott and
USBM methods are used for core wettability measurements. Quan-
titative methods are more commonly used; nevertheless, there is no
single universally accepted method.
Contact angle (Θ) is the angle at which a fluid/fluid interface
meets the solid surface. The Θ is always measured relative to the
Copyright © 2011 Society of Petroleum Engineers. This paper (2009-195) was accepted
for presentation at the 10th Canadian International Petroleum Conference (the 60th
Annual Technical Meeting of the Petroleum Society), Calgary, 16–18 June 2009, and
revised for publication. Original manuscript received for review 31 March 2009. Revised
paper received for review 7 March 2011. Paper peer approved 22 March 2011 as SPE
paper 148631.
denser phase. In this work, water is the denser phase. The contact-
angle method is useful for wettability measurement when working
with clean surfaces and pure fluids. Typically, contact-angle mea-
surements are performed on oil/water/quartz-surface systems in
order to study the wettability variations under different tempera-
tures and pressures.
For the measurement of Θ, two immiscible fluids are placed on
a solid surface; Fluid 1 is the denser fluid. Θ can vary between 0
and 180°. If Θ is less than 75°, Fluid 1 is the wetting phase, and if
Θ is greater than 105°, Fluid 2 is the wetting phase. Θ between 75
and 105° defines what is known as neutral wettability, and indicates
that the surface does not have any preference to contact more with
any of the fluids.
Several methods have been used to measure the contact angle
[capillary rise, tensiometric, cylinder, vertical rod, captive bubble,
Wilhelmy plate, tilting plate, pendant drop, sessile drop as de-
scribed by Adamson and Gast (1997), single-crystal sessile drop,
and dual-drop-dual-crystal (DDDC)]. Details can be found in the
works of Vijapurapu and Rao (2004), Vijapurapu et al. (2002), Rao
(1999, 1996), and Rao and Girard (1996).
For measuring IFT and surface tension (ST) of two fluids on
a solid substrate, there are several different methods that are ex-
plained in detail in the books of Adamson and Gast (1997) and
Erbil (2006). The most commonly used methods are categorized
into shape methods and force methods. The shape methods include
the sessile-drop, pendant-drop, and spinning-drop methods. They
are based on the analysis of the deformation of a drop or bubble
in another fluid. Force methods measure the force exerted on an
object by the meniscus of a liquid. The Du Nouy-ring method and
the Wilhelmy-plate method are examples of force methods. Some
other methods not placed in these two categories are also used to
measure IFT and ST. They are the capillary-rise, drop-weight, and
maximum-bubble-pressure methods.
Of all the methods for measuring IFT and contact angle, the ses-
sile-drop and pendant-drop methods are the most general experi-
mental methods that are applicable for measurements of both IFT
and Θ simultaneously in numerous research areas. In early works
for determining IFT and Θ from the shape of the drops, the sessile
and pendant drops were analyzed and discussed separately. In order
to be able to calculate the IFT and Θ, numerous series of tables
containing the shape parameters were generated by Bashforth and
Adams (1893) for sessile drops, and by Fordham (1948) for pen-
dant drops. The tables were suitable for a certain range of size and
shape of drops. More tables were generated by Padday (1969) and
also by Hartland and Hartley (1976). Malcolm and Paynter (1981)
used another analytical method to calculate the IFT and Θ of non-
wetting sessile drops (Θ>90°). Maze and Burnet (1971, 1969)
started the development of a numerical method to calculate the IFT
and Θ for sessile drops. Their method needed reasonable initial es-
timates of the drop-shape and -size parameters. They used the ta-
bles of Bashforth and Adams (1893) for the initial estimates.
Rotenberg et al. (1983) proposed a new computational proce-
dure for determining values of the IFT and Θ from the shape of
axisymmetric fluid interfaces (ADSA). The development of this
method was a great achievement in surface sciences. No particular
June 2011 61

Fig. 1—The Skyscan 1072 device.
Fig. 3—An image of the microcell taken by the microCT scanner.
values are required for any parameters (i.e., the surface tension, the
radius of curvature at the apex, and the coordinates of the origin)
because they are calculated in the program. This numerical method
combines and unifies both the sessile-drop and pendant-drop tech-
niques without using any of the previously generated tables.
In their later works, Neumann and his collaborators improved
and modified the ADSA technique and produced different versions
for various applications. The modified versions are ADSA diam-
eter (del Río and Neumann 1997), ADSA contact diameter (Li et
al. 1992; Skinner et al. 1989), automatic digitization technique in
ADSA (Hansen 1993; Cheng et al. 1990), ADSA maximum dia-
meter (Moy et al. 1991), ADSA height and diameter (del Río and
Neumann 1997), ADSA contact or equatorial diameter (Amirfazli
et al. 2000), ADSA captive bubble (Zuo et al. 2004a, 2004b; Prokop
et al. 1998), ADSA electric field (Bateni et al. 2005, 2006), ADSA
profile (del Río and Neumann 1997; Li et al. 1992; Cheng and Neu-
mann 1992), ADSA imperfect profile (Kalantarian et al. 2009),
theoretical image fitting analysis (Cabezas et al. 2004, 2005), and
ADSA for nearly-spherical-shaped drops (Hoorfar and Neumann
2006; Hoorfar et al. 2005).
Since the development of ADSA, numerous researchers in nu-
merous different areas of science have used it to obtain the IFT and
Θ of sessile drops, pendant drops, and captive bubbles in a variety
of fluid/fluid/solid systems. Application of this method for the cal-
62 Journal of Canadian Petroleum Technology
Fig. 2—The microcell and its position inside the microCT scanner.
culation of IFT and Θ can be found in polymer sciences (Wulf et
al. 1999; Regismond et al. 1999; Kwok et al. 1998a; del Río et al.
1998; Welzel et al. 2002; Liu and Tomasko 2007; Zschoche et al.
2007), monolayers (Wege et al. 1999), surface and chemistry sci-
ences (Kwok et al. 1996, 1998b; Susnar et al. 1994, 1996; Li et al.
1996; Noordmans and Busscher 1991; Li and Neumann 1990; Hol-
gado-Terriza et al. 1999; Lam et al. 2001a, 2001b, 2002; Serrano-
Saldaña et al. 2004; Vrânceanu et al. 2007), the oil and gas industry
(Nobakht et al. 2008; Askvik et al. 2005; Vijapurapu and Rao 2004;
Rao and Lee 2002, 2003; Gu 2001), road construction (Rodríguez-
Valverde et al. 2002), biological sciences (Moy et al. 1991, Kalan-
tarian et al. 2009, Aguilar-Mendoza et al. 2008; Mikhaylova et al.
2007; Acosta et al. 2007; Wege et al. 2002; Lu et al. 2002; Grundke
et al. 1999; Alvarez et al. 1999; Amirfazli et al. 1998; Lin et al.
1993; Voigt et al. 1991; Duncan-Hewitt et al. 1989), and air-strip-
ping and wastewater-treatment processes (Mak et al. 2004).
The IFT and contact-angle values in the aforementioned methods
are measured either by looking directly at the sample interfaces or
by looking at a photograph of the contact area. Therefore, in the ex-
periments, the transparent phase (water or gas) should always play
the bulk-fluid role and oil is the drop phase. Therefore, with these
techniques, it is impossible to study the contact angle of a drop of
water or a bubble of gas inside the oil phase; however, with use of
a microCT scanner, it is possible to see through the oil as the bulk
fluid and investigate the IFT and contact angle of the water as a ses-
sile drop on a quartz plate. The images taken by the microCT scan
can detect the drop of water inside the bitumen (oil) phase.
In this study, the experiments are run at elevated pressures and
temperatures and the images are processed by use of the comput-
erized-ADSA method to determine the IFTs and contact angles of
bitumen/water systems on a quartz surface from the drop profile.
Experimental Procedure and Setup
The microCT scanner used for imaging the contact angle is a Sky-
scan 1072 (Fig. 1). In order to measure the contact angle, a micro-
model containing the quartz crystal was designed and constructed.
The micromodel is an aluminum cell, and its size is 10 mm in di-
ameter and 20 mm in height. Fig. 2 shows the cell inside the mi-
croCT scanner, and Fig. 3 is an image of the microcell taken by
the microCT scanner. The quartz plate is 6 mm in diameter and 1
mm in thickness. The cell was connected to a microvalve through
1.59-mm (1/16-in.) tubing for pressure control. The height and di-
ameter of the entire system inside this scanner cannot be more than
85 and 50 mm, respectively. Aluminum was chosen as the cell-body
material because of its X-ray transparency characteristics and the
ability to withstand the elevated pressure at the experiment tem-
peratures. The maximum temperature that can be reached in the
cell is 393 K (120°C) under the experimental pressure. The cell was
placed in a conventional oven to reach the temperature and inserted
in styrofoam insulation to maintain the temperature during the
scanning process. The microvalve and the connected tubing were
wrapped in glass-wool insulation. The advantage of styrofoam over
glass wool is the better X-ray transparency of the former, which

Fig. 4—A sample image of the water/bitumen/quartz contact
area taken by the microCT sanner.
produces clearer CT images. Therefore, for the cell that undergoes
the scanning process, it is recommended to use styrofoam instead
of glass wool. But, in the nonscanning part, which is the micro-
valve and the tubing, glass wool has the priority of usage because
it is more flexible and occupies less space. Therefore, it prevents
exceeding the maximum height available in the microCT-scanner
chamber. The temperature was measured using a thermocouple at-
tached to the body of the cell.
The brine (aqueous phase) used for this study is a 10.0 wt%
CaCl2 solution. The bitumen is from the Athabasca pool. The den-
sity and viscosity of this particular bitumen is 1000.4 kg/m3 and
14.7 Pa∙s (14,700 cp), respectively, at 298 K (25°C). The use of a
quartz plate in the experiments corresponds to a good representa-
tion of sandstone.
In order to more realistically simulate the conditions of the res-
ervoir in the microcell, the quartz plate was immersed in the brine
for 24 hours before each experiment. This time allows the surface
of the quartz to reach equilibrium with the brine. In the next step,
the drop of bitumen was placed on the surface, which was in equi-
librium with the brine, and the cell was closed. The entire system
was left for 72 hours to allow the bitumen/brine/quartz interface to
reach equilibrium as well. Previously, the contact angle of the bi-
tumen/brine/quartz system had been measured at several time inter-
vals, and it had been observed that the changes in the contact angle
are negligible after 72 hours.
When the system reached the equilibrium conditions, the main
part of the experiments began. The valve and tubing parts of the
system were wrapped in the glass-wool insulation, and the cell
was placed in the oven until it reached the desired temperature at
the desired pressure. Then, the cell was placed inside the styro-
foam insulation, delivered to the microCT scanner, and placed in
the X-ray chamber before scanning began. Fig. 4 shows a sample
image of the water/bitumen/quartz contact area taken by the mi-
croCT scanner. The device had been previously warmed up and
prepared for scanning.
Density and viscosity of the bitumen were carefully measured at
different temperatures. Density of the brine was also measured at
different temperatures. The value of each of the fluid-density mea-
surements was used to calculate the IFT of the brine and bitumen
on the quartz system.
The IFT and contact angle for the system of quartz/water(brine)/
bitumen were determined at different temperatures and pressures
using the ADSA numerical method.
Results and Discussion
Methodology Used for IFT and Contact-Angle Determination.
In this work, an X-ray transparent cell has been prepared to study
the bitumen/water(brine)/quartz interfacial properties. The system
has been aged to reach equilibrium. The IFT and contact angle for
the system of quartz/water(brine)/bitumen were determined at dif-
ferent temperatures at ambient pressure, 1.724 MPag (250 psig),
3.447 MPag (500 psig), 5.171 MPag (750 psig), and 6.895 MPag
(1,000 psig) using the ADSA numerical method and a Skyscan
1072 microCT scanner. The ambient pressure and temperatures
during the experiments were approximately 101 kPa(a) and 22°C,
respectively. In this study, all the measured pressures are reported
in gauge units.
We assumed that the drops at different pressures and tempera-
tures are axisymmetric; therefore, we could use the ADSA tech-
nique to calculate the IFT from the shape of the axisymmetric drop.
In order to determine the IFT, random points from the drop inter-
face, representing the drop profile, were selected and used to gen-
erate the calculated curve that has the minimum distance from the
measured drop shape. On the basis of the calculated curve, the
place of the apex of the drop, the radius of the drop at the apex, β
(the shape factor or bond number), and, consequently, the IFT of
bitumen/water were all determined. Also, by integrating the curve
from the apex to the contact point, the contact angle of the bitumen/
water interface was calculated. The results of the IFT calculations
are shown in Figs. 5 and 6 and the results for the calculated contact
angles are shown in Figs. 7 and 8.
IFT Results. From the results of IFTs (Figs. 5 and 6), it is apparent
that a general trend exists when the pressure increases. The IFT for
the system tends to increase with the pressure for these experiments.
By considering each individual test, a less-apparent trend ap-
pears. At a given pressure, the IFT tends to decrease with an in-
crease in temperature.
The scatter of the results can be attributed to the interpretation of
the image taken by the microCT scanner. Any small deviation from
the actual drop shape can cause the ADSA algorithm to converge
to a suboptimal curve. Experimental error in preparing the samples
also influences the calculations.
The IFT trends are smoother at lower pressures. As shown in
Fig. 5, at ambient pressure the IFT ranges from 0.7 to 2 mN/m, but
as the pressure increases, the range of IFT changes is larger; there-
fore, in Fig. 6, the IFT range for 6.895 MPa (1,000 psi) is from 3.5
to 12.2 mN/m.
The accuracy of the results can be attributed to the interpreta-
tion of the image taken by the microCT scanner. Any small devia-
tion from the actual drop shape can cause the ADSA algorithm to
converge to a suboptimal curve. Experimental error in preparing
the samples also influences the calculations. The error estimated in
these experiments was less than ±0.5 mN/m, shown as error bars
in Figs. 5 and 6. Because the ADSA method is accurate in deter-
mining IFT and contact-angle values, the error in the experiment is
dominant because of image inaccuracy. Therefore, by deviating the
data points of the interface to the maximum possible coordinates,
the experimental error is estimated. This procedure also takes tem-
perature- and pressure-measurement inaccuracy into account.
Contact-Angle Results. Figs. 7 and 8 illustrate the results of con-
tact-angle measurement at different temperatures and pressures.
These graphs show that, generally, the contact angle of the bitumen/
water interface increases as the temperature increases. At lower tem-
peratures, the system is more water-wet, the wettability of the sys-
tem changes toward neutral wettability as the temperature increases.
Also, comparing Figs. 7 and 8, it is found that the contact angle
of the bitumen/water interface decreases as the pressure increases.
The exception occurs at 3.447 MPa (500 psi) onward, which shows
a higher contact-angle average compared with ambient-pressure
and 1.724-MPa (250-psi) experiments. The trend of contact-angle
decrease with pressure increase continues as the pressure reaches
higher than 3.447 MPa (500 psi).
Similar to IFT, the contact-angle curves show a smoother trend
at higher temperatures at each level of experimental pressure. Also,
the contact-angle curves are smoother in higher pressures. As is ap-
parent in Fig. 7 (ambient pressure), the contact-angle range is more
than 40°; but as the pressure increases, the range of the contact
angle narrows to 20° at 6.895 MPa (1,000 psi), as shown in Fig. 8.
June 2011 63
 IFT vs. Temperature at Ambient,
1.7 MPa (250 psi), and 3.4 MPa (500 psi)
12
Interfacial Tension, mN/m
10
8 8
6 P =1.7
4 4
2 2
0
30 40 50 60 70 80
Temperature, °C
Fig. 5—IFT of bitumen/water on the quartz surface at different
temperatures at ambient pressure [101 kPa(a)], 1.7 MPa (205 psi),
and 3.4 MPa (500 psi).
Contact-angle values can deviate from the real values because
of some experimental faults. The error can be a consequence of
the cell movement from the oven to the microCT scanner, unclear
images taken by the microCT scanner, and inaccurate temperature
and pressure indication. Some tests have been performed to eval-
uate the value of the error in contact-angle measurements. These
tests showed a total error of ±3° in the contact-angle values. The
experimental error is estimated by deviating the data points of the
interface to the maximum possible coordinates. This also takes
temperature- and pressure-measurement inaccuracy into account.
Conclusions
• Comparison between the results of IFT shows that the IFT of the
bitumen/water system under study decreases as the temperature
increases at each experimental pressure.
• The results show that, generally, the IFT increases as the pressure
of the system increases.
• The IFT curves show a smoother trend at lower pressures. At am-
bient pressure, the IFT ranges from 0.7 to 2 mN/m, but as the
pressure increases, the range of IFT changes is larger; there-
fore, at 6.895 MPa (1,000 psi), the range is between 3.5 and
12.2 mN/m.
• At a certain pressure level in the experiment, the contact angle
of the bitumen/water interface increases as the temperature in-
creases. At lower temperatures, the system is more water-wet;
and the wettability of the system changes toward neutral wetta-
bility as the temperature increases.
• The contact angle of the bitumen/water interface decreases as the
pressure increases. The exception occurs at 3.447 MPa (500 psi)
onward, which shows a higher contact-angle average compared
with ambient pressure and 1.724 MPa (250 psi). The trend of
contact-angle decrease with pressure increase continues as the
pressure goes higher than 3.447 MPa (500 psi). Lower contact
angles at higher pressures indicate that the system shows more-
water-wet properties as it undergoes higher pressures; but gener-
ally speaking, there is no apparent effect of pressure on contact
angle.
• The contact-angle curves show a smoother trend at higher temper-
atures at each level of experimental pressure. Also, the contact-
angle curves are smoother in higher pressures.
Nomenclature
β = shape parameter (Bond number)
Θ = contact angle
Acknowledgements
The contributions and support of Juan M. Montelongo, Sergey
Kryuchkov, and David Moon are greatly appreciated. Financial
64 Journal of Canadian Petroleum Technology
IFT vs. Temperature at 5.2 MPa (750 psi),
and 6.9 MPa (1,000 psi)
12
Interfacial Tension, mN/m
10
Ambient
Pressure P =5.2
Mpa
6 P =6.9
Mpa
Mpa
P =3.4
Mpa
0
90 100 30 40 50 60 70 80 90 100
Temperature, °C
Fig. 6—IFT of bitumen/water on the quartz surface at different
temperatures at 5.2 MPa (720 psi) and 6.9 MPa (1,000 psi).
support from the sponsoring companies of the Canada Research
Chair (CRC) in Energy and Imaging (PetroCanada, Suncor, Nexen,
Shell, ConocoPhillips, Laricina, ET-Energy, Schlumberger, Para-
mount, CMG Foundation, Canadian Natural, and Devon Canada),
the CRC program, and Natural Sciences and Engineering Research
Council of Canada is gratefully appreciated. JCPT
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110
100
Contact Angle, °
90 P=5.2
Mpa
80
70 P=6.9
Mpa
60
50
40
30 40 50 60 70 80 90 100
Temperature, °C
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Authors

Maryam Rajayi is currently working for

WorleyParsons Canada. Before completing
her graduate studies in Canada, Rajayi
worked for 1 year as a chemical engineer in
an engineering and consulting company in
Iran. Her research interests are in solvent
and thermal recovery of oil sands and heavy
oil, properties of oil-sands reservoirs, and
enhanced oil recovery. Rajayi holds a BS de-
gree in chemical engineering from Sharif
University of Technology in Iran, as well as an MS degree in chem-
ical engineering from the University of Calgary.

Apostolos Kantzas is currently a professor

at the University of Calgary, holder of a
Canada Research Chair in Energy and Im-
aging, and the director of the Tomographic
Imaging and Porous Media Laboratory. Be-
fore his appointment at the university,
Kantzas held a senior research-engineer po-
sition in the Pipeline and Oil Technologies
department at NOVA Research and Tech-
nology Corporation. He led a 40-person re-
search group that was involved in research related to problems of
flow through porous media, enhanced oil recovery, soil remedia-
tion, reactor design, and tomographic imaging. Kantzas has au-
thored or coauthored more than 300 technical papers and more than
200 technical reports. He holds a Dipl. Eng. in chemical engi-
neering from the Aristotle University of Thessaloniki in Greece and
MASc and PhD degrees in chemical engineering from the Univer-
sity of Waterloo. Kantzas is a member of the Association of Profes-
sional Engineers, Geologists, and Geophysicists of Alberta; SPE;
the Chemical Institute of Canada; the American Institute of Chem-
ical Engineers; the Canadian Well Logging Society; and the Society
of Core Analysts.

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