Article

pubs.acs.org/jced

Eects of Four Important Factors on the Measured Minimum

Miscibility Pressure and First-Contact Miscibility Pressure
Yongan Gu,* Pengcheng Hou, and Weiguo Luo
Petroleum Technology Research Centre (PTRC), Petroleum Systems Engineering, Faculty of Engineering and Applied Science,
University of Regina, Regina, Saskatchewan S4S 0A2, Canada

ABSTRACT: The vanishing interfacial tension (VIT) technique is

applied to determine the minimum miscibility pressures (MMPs) and
rst-contact miscibility pressures (Pmax) of ve light crude oilCO2
systems from the measured equilibrium interfacial tensions (IFTs) at
dierent equilibrium pressures. The equilibrium IFTs are measured under
various experimental conditions by applying the axisymmetric drop shape
analysis technique for the pendant drop case. It is found that in each IFT
test, the measured equilibrium IFT is reduced almost linearly with the
equilibrium pressure in two pressure ranges. The MMP of each light
crude oilCO2 system is thus determined from the measured equilibrium
IFTs in range I by applying the VIT technique. The rst-contact
miscibility pressure (Pmax) of each light crude oilCO2 system is
extrapolated from the measured equilibrium IFTs in range II. Moreover,
the test temperature, crude oil composition (dead/live oil), gas
composition (pure/impure CO2), and initial gasoil ratio (GOR) are studied to examine their specic eects. The experimental
data show that the measured MMPs and Pmax values of ve light crude oilCO2 systems increase linearly with the temperature.
The presence of CH4 in the CO2 phase results in substantially higher MMP and Pmax. An increased initial GOR leads to
marginally higher MMP and Pmax.

INTRODUCTION
For a long time gas injection has been used to displace the
residual oil, reduce the oil viscosity, induce the oil-swelling
eect, and maintain the reservoir pressure1,2 in an eective
enhanced oil recovery (EOR) method. During the gas injection
process, the interfacial mass transfer occurs across the interface
between the residual oil phase and the injected gas phase until
they reach an equilibrium state. As a result, the physicochemical
properties of the displacing gas and displaced oil become
similar, leading to an ecient displacement process.3 The
concept of miscibility is introduced and used for a gas injection
process when the interfacial tension between the two phases of
interest (i.e., the oil and gas phases) approaches zero and there
is not an interface formed between these two phases. The
minimum miscibility pressure (MMP) is dened as the lowest
operating pressure at which the injected gas and the residual
oil-in-place (ROIP) become miscible after a dynamic multi-
contact process at the reservoir temperature.4 At a pressure
higher than the MMP, miscibility can be achieved through a
vaporizing process, a condensing process, or a combination of
the two.5,6 To ensure a miscible gas ooding process with a
high oil recovery factor, accurate determination of the MMP is
important in the design and implementation of a gas injection
EOR project in a eld application.
Among many gas injection projects, the carbon dioxide
(CO2) ooding process is often applied under the miscible or
near-miscible ooding conditions to enhance the oil recovery.
In comparison with the other solvents used for the gas ooding
processes, CO2 in its supercritical state can enter the oil-bearing
zones that are not swept by the previously injected water and
thus displace the trapped oil. Besides, a large fraction of the
injected CO2 can be stored underground, which is benecial to
the environment.7 During and after the CO2 injection process,
the injected CO2 and the residual crude oil interact with each
other. At a reservoir pressure close to or higher than the MMP,
the injected CO2 is dissolved into the crude oil to dilute it and
reduce its viscosity. Meanwhile, the light-hydrocarbons (HCs)
in the crude oil can be extracted by CO2. After the rst contact
of CO2 and crude oil, the light-HCs enriched CO2 advances to
contact the fresh crude oil due to its high mobility and becomes
even more enriched. After adequate and multiple contacts,
ultimately, the light-HCs enriched CO2 becomes miscible with
the fresh crude oil at the displacement front. If the injection
pressure is suciently high, in principle, the injected CO2 can
become miscible with the residual oil at the rst contact and
this pressure is referred to as the rst-contact miscibility
pressure.8
Several experimental methods for determining the MMP
have been developed and described in the literature. The slim-
tube test method is considered to be a standard method for
measuring the MMP in the petroleum industry.9,10 The major
component of the experimental apparatus for the slim-tube test
Received: February 1, 2013
Accepted: March 28, 2013
Published: April 8, 2013

2013 American Chemical Society 1361 dx.doi.org/10.1021/je4001137 | J. Chem. Eng. Data 2013, 58, 13611370
Journal of Chemical & Engineering Data Article

is a long (2 to 40 m) coiled slim tube packed with proper in Table 1. The mass fraction of asphaltene content of the
packing materials (e.g., the Ottawa sands or glass beads). After cleaned light crude oil was measured to be wasp = 0.0026
the coiled slim tube is saturated with the crude oil to be tested,
CO2 is injected through it to displace the crude oil at dierent Table 1. Physical and Chemical Properties of the Pembina
injection pressures and at the actual reservoir temperature. At Cardium Light Crude Oil (9-11-48-9W5), Where oil and oil
the end, the measured oil recovery factor is plotted versus the Are the Oil Density and Viscosity; (SG)oil, (MW)oil, and wasp
injection pressure, and then the MMP is determined to be the Are the Oil Specic Gravity, Molecular Weight, and
break-over pressure, above which the oil recovery factor almost Asphaltene Content in Mass Fraction, Respectively
reaches its maximum value.11 This method simulates the
multiphase uid ow through the porous media under the oileld Pembina Cardium
crude oil light
actual reservoir conditions. However, it is extremely time-
oil @ 300.15 K/(gcm3) 0.835 0.001
consuming and expensive as well. Alternatively, a series of high-
oil @ 300.15 K/(mPas) 5.53 0.01
pressure CO2 coreood tests can be used to measure the MMP
(SG)oil/(API) 37.96 0.01
in a similar manner.12
(MW)oil/(gmol1) 212.1 0.1
The third experimental method for determining the MMP
wasp 0.0026 0.0001 (normal-pentane insoluble)
uses the rising-bubble apparatus (RBA), which is commonly
used as a fast and cost-eective alternative to the slim-tube
method.13 In this method, a gas (such as CO2) bubble is (normal-pentane insoluble) by using the standard ASTM
injected into a thin transparent column of the crude oil at a D2007-03 method and lter papers (Whatman No. 5, England)
dierent pressure each time. The MMP is inferred from the with a pore size of 2.5 m. The compositional analysis result of
pressure dependence of the rising-bubble behavior (e.g., size, the light crude oil was obtained by using the standard ASTM
shape, or color of the gas bubble) inside the oil column. In D86 and is given in Table 2. Carbon dioxide was purchased
general, the MMP is determined to be the pressure at or above
which the rising-gas bubble ultimately disappears in its rising Table 2. Compositional Analysis Result of the Pembina
process. The RBA method is fast and requires a small amount Cardium Light Crude Oil (9-11-48-9W5) with the Analysis
of the crude oil, in comparison with the slim-tube or coreood Uncertainty of 0.0001 in Mole Fraction
test. However, the RBA method simulates the vaporizing Cn mole fraction Cn mole fraction
process alone in the miscibility development process and C1 0.0000 C27 0.0107
neglects the condensing process. This leads to an overestimated C2 0.0000 C28 0.0094
MMP of some crude oilCO2 systems, in which the C3 0.0020 C29 0.0089
condensing process also contributes to the miscibility develop- C4 0.0117 C30 0.0064
ment. C5 0.0367 C31 0.0068
More recently, an experimental method called the vanishing C6 0.0501 C32 0.0059
interfacial tension (VIT) technique has been used to determine C7 0.1067 C33 0.0046
the MMP.1416 In experiment, the equilibrium interfacial C8 0.0720 C34 0.0038
tensions (IFTs) between an oil phase and a gas phase can be C9 0.0761 C35 0.0054
accurately measured at dierent equilibrium pressures and at C10 0.0695 C36 0.0047
the actual reservoir temperature by applying the axisymmetric C11 0.0575 C37 0.0030
drop shape analysis (ADSA) technique for the pendant drop C12 0.0501 C38 0.0027
case. Thus the MMP is determined by applying the VIT C13 0.0459 C39 0.0037
technique, which is based on the concept that the equilibrium C14 0.0397 C40 0.0028
interfacial tension between the two phases approaches zero C15 0.0374 C41 0.0027
when they become miscible. In the literature, it is also proven C16 0.0298 C42 0.0022
that the zero interfacial tension is a necessary condition for the C17 0.0308 C43 0.0022
miscibility development.17,18 Each MMP determination by C18 0.0309 C44 0.0020
using the VIT technique can be accomplished in (4 to 6) h, C19 0.0201 C45 0.0020
whereas the slim-tube test usually takes (4 to 6) weeks.9 C20 0.0207 C46 0.0015
In this paper, the VIT technique is applied to determine the C21 0.0196 C47 0.0014
MMPs and the rst-contact miscibility pressures (Pmax) of ve C22 0.0114 C48 0.0013
dead/live crude oilpure/impure CO2 systems at dierent C23 0.0155 C49 0.0013
experimental conditions. The following four important factors C24 0.0128 C50+ 0.0335
are experimentally studied to evaluate and compare their C25 0.0127 total 1.0000
detailed eects on the measured MMP and Pmax: the test C26 0.0114
temperature, oil and gas compositions, and initial gasoil ratio
(GOR) in volume.

from Praxair (Canada) and normal-pentane was purchased

EXPERIMENTAL SECTION
Materials. In this study, the original light crude oil was
collected from the Pembina Cardium oileld in Alberta,
Canada. The obtained original crude oil was cleaned by using
a centrifuge (Allegra X-30 Series, Beckman Coulter) in order to
remove any sands and brine. Some major physical and chemical
properties of the Pembina Cardium Crude oil sample are listed
1362
from VWR International (Canada). Four hydrocarbon solvents,
methane, ethane, propane, and normal-butane, were all
purchased from Praxair (Canada). The purities of these six
solvents used in this study are listed in Table 3.
Reconstitution of Live Oil Sample. The live oil was
reconstituted by saturating the dead oil with the produced
hydrocarbon (HC) gas. The actual produced gas composition is
listed in Table 4, which was provided by PennWest Exploration.
dx.doi.org/10.1021/je4001137 | J. Chem. Eng. Data 2013, 58, 13611370
Journal of Chemical & Engineering Data Article

Table 3. Purities of Six Solvents Used in This Study

solvent purity (mole fraction)
CO2 0.99998 0.00001
normal-C5H12 0.9976 0.0001
CH4 0.9997 0.0001
C2H6 0.99 0.01
C3H8 0.995 0.001
normal-C4H10 0.995 0.001

Table 4. Compositional Analysis Results of the Actual,

Nominal, and Synthetic Produced Gas Samples with the
Analysis Uncertainty of 0.0001 in Mole Fraction
actual (mole nominal (mole synthetic (mole
component fraction) fraction) fraction)
C1 0.6650 0.6650 0.7020
C2 0.1141 0.1141 0.1002
C3 0.1139 0.1139 0.1026
Figure 1. Measured equilibrium pressure of the Pembina Cardium live
crude oilproduced gas mixture versus its volume data at T = 294.15
iso-C4 0.0183
K.
normal-C4 0.0390 0.1070 0.0906
iso-C5 0.0068
normal-C5 0.0086 Preparation of Two Impure CO2 Samples. In this study,
C6 0.0055 two dierent impure CO2 samples were prepared by mixing
C7+ 0.0054 pure CO2 with pure CH4 at a predetermined approximate
N2 0.0148 0.0046 composition of 0.8 CO2 + 0.2 CH4 or 0.9 CO2 + 0.1 CH4 in
CO2 0.0086 mole fraction. For example, the rst impure CO2 sample with
the composition of 0.8 CO2 + 0.2 CH4 was prepared as follows.
The actual produced gas composition was simplied as the First, two cylinders (500-10-P-316-2, DBR, Canada) with the
nominal composition in Table 4 by lumping the HCs whose volume of 1000 cm3 each were cleaned and vacuumed at the
carbon numbers are equal to or larger than 4 (i.e., C4+) and the room temperature T = 294.15 K. Pure CO2 was injected into
non-HCs together as normal-C4. The man-made or synthetic one of the two cylinders by using a displacement pump until its
produced HC gas was prepared in laboratory to reconstitute the pressure reached P1 = 3.06 MPa. Second, pure CH4 was
live oil and its composition is given in Table 4. injected into another cylinder by using a displacement pump
With the synthetic produced HC gas sample, the live oil was until its pressure reached P2 = 0.67 MPa. These two respective
reconstituted by using the actual gasoil ratio (GOR) of 15:1 pressures were calculated by using the PR EOS so as to
in volume under the standard conditions. The detailed prepare the rst impure CO2 sample with the targeted
experimental procedure for reconstituting the live oil sample composition of 0.8 CO2 + 0.2 CH4. Third, pure CH4 in the
is described below. First, a high-pressure cylinder (500-10-P- second cylinder was injected into the rst CO2 cylinder, which
316-2, DBR) with the volume of 1000 cm3 was cleaned and was then further pressurized to P3 = 10.00 MPa to ensure that
kept inside an air bath at T = 326.15 K. A total of 500 cm3 dead such a prepared CO2CH4 mixture was in a homogeneous
oil sample was injected into the cylinder by using a high- phase. Thus the rst impure CO2 sample with the targeted
pressure displacement pump. Second, the synthetic produced composition of 0.8 CO2 + 0.2 CH4 was obtained. The second
gas was injected into another cleaned and vacuumed cylinder impure CO2 sample with the targeted composition of 0.9 CO2
with the volume of 500 cm3 until the gas pressure inside the + 0.1 CH4 was prepared in a similar way. After each impure
cylinder reached P1 = 1.50 MPa. This pressure was calculated CO2 sample was prepared, the CO2CH4 gas mixture was
by applying the PengRobinson equation of state (PR sampled and stored in a miniature sample cylinder (SS-4CS,
EOS)19 so as to reach the actual GOR of 15:1 in volume for the Swagelok, Canada). The gas sample was then analyzed by
live oil. Third, the produced HC gas was compressed and applying GC. The actual compositions of these two impure
injected into the oil cylinder to saturate the dead oil. Finally, the CO2 samples are found to be 0.7487 CO2 + 0.2513 CH4 in
high-pressure cylinder containing the dead oilsynthetic mole fraction for the rst impure CO2 sample and 0.8406 CO2
produced gas mixture was kept rotating continuously for at + 0.1594 CH4 in mole fraction for the second impure CO2
least 7 d to fully mix the dead oil with the synthetic produced sample, respectively.
gas. The saturation pressure of such reconstituted live oil was IFT Measurement. Figure 2 shows a schematic diagram of
determined to be Psat = 2.03 MPa at 294.15 K from two linear the experiment setup used for measuring the dynamic/
regression lines of the measured equilibrium pressure of the live equilibrium IFT between the dead/live crude oil and pure/
oilproduced HC gas mixture versus its volume data in two impure CO2 by applying the axisymmetric drop shape analysis
dierent regions, as shown in Figure 1. After the live crude oil (ADSA) technique for the pendant drop case.20 The major
was reconstituted, the live crude oilproduced gas mixture component of this experimental setup was a see-through
inside the high-pressure cylinder was further compressed until windowed high-pressure IFT cell (IFT-10, Temco) with a net
its pressure reached P2 = 3.50 MPa, which was far above the volume of Vcell = 49.5 cm3. A stainless steel syringe needle was
measured saturation pressure in order to eliminate the HC gas installed at the top of the IFT cell and used to form a pendant
cap. The live oil sample cylinder was positioned vertically for oil drop. The light crude oil and CO2 were stored in two
the live oilCO2 IFT measurement. transfer cylinders (500-10-P-316-2, DBR), heated to a
1363 dx.doi.org/10.1021/je4001137 | J. Chem. Eng. Data 2013, 58, 13611370
Journal of Chemical & Engineering Data
Figure 2. Schematic diagram of the experimental setup used for measuring the dynamic/equilibrium interfacial tension (IFT) between a pendant
dead/live light crude oil drop and pure/impure CO2 by applying the axisymmetric drop shape analysis (ADSA) technique for the pendant drop case.
prespecied constant test temperature, and injected into the
IFT cell to reach a prespecied initial GOR in volume at a
targeted equilibrium/test pressure. The detailed IFT exper-
imental procedure will be described below. After the injected
light crude oil and CO2 reached an equilibrium state, the light
crude oil was introduced from its transfer cylinder to the
syringe needle to form an extremely small pendant oil drop for
the IFT measurement. A light source and a glass diuser (240
341, DynaLume) were used to provide uniform and sucient
illumination for the pendant oil drop. A monochrome
microscope camera (MZ6 Leica) was used to observe and
capture the sequential digital images of the dynamic pendant oil
drop inside the IFT cell at dierent times. The high-pressure
IFT cell was positioned horizontally between the light source
and the microscope camera. The entire ADSA system and the
IFT cell were placed on a vibration-free table (RS4000,
Newport). The digital image of the dynamic pendant oil drop
surrounded by CO2 at any time was acquired in a tagged image
le format (TIFF) by using a digital frame grabber (Ultra II,
Coreco Imaging) and automatically stored in a DELL desktop
computer.
Prior to each IFT measurement, the high-pressure cell was
rst cleaned with kerosene, then ushed with nitrogen, and
nally vacuumed. It was preheated to an elevated test
temperature by using a heating belt with an autotransformer
(3PN1010B, STACO Energy Products Co.) and a thermom-
eter (type K, DDT2, Supco.). After the temperature inside the
high-pressure cell reached the prespecied constant test
temperature, CO2 was injected slowly into the IFT cell from
its bottom port by using a manual displacement pump (PMP-
500-1-10-HB-316-MO-CO, DBR) to reach a high pressure.
Then a certain amount of the light crude oil was injected into
the IFT cell through the syringe needle at its top port to reach a
targeted initial GOR in volume by using a programmable
syringe pump (100DX, ISCO Inc.). An extremely low oil
injection rate of 6.0 cm3h1 was used so that the oil and gas
phases inside the IFT cell could interact with each other over a
1364
Article
suciently long period (e.g., 1 h) and reach their equilibrium
state, which was indicated by the constant equilibrium pressure
at the prespecied constant test temperature. It is worthwhile
to note that in this study, the ratio of the initial gas phase
volume (Vgas) to the initial oil phase volume (Voil) inside the
high-pressure IFT cell was dened as the initial gasoil ratio
(GOR) in volume, i.e., Vgas:Voil, prior to each IFT test. In the
case for the highest initial GOR of 4000:1, for example, no oil
was preinjected before the IFT test. Thus the entire high-
pressure IFT cell was occupied by pure/impure CO2 in this
special case, i.e., Vgas = Vcell = 49.5 cm3. If the average pendant
oil drop size was assumed to be Voil = 12.375 103 cm3, the
initial GOR was approximated to be Vgas:Voil = 4000:1 in
volume. In the case for the lowest initial GOR of 3:1, for
instance, the light crude oil with the volume of 0.25Vcell (i.e.,
Voil = 0.25Vcell) was injected into the high-pressure IFT cell.
The remaining IFT cell space (i.e., Vgas = 0.75Vcell) was
occupied by pure/impure CO2 in this case so that the initial
GOR was equal to Vgas:Voil = 3:1 in volume.
After the injected crude oil and CO2 phases inside the IFT
cell reached an equilibrium state, a pendant oil drop was
generated at the tip of the syringe needle and surrounded by
pure/impure CO2. The dynamic IFT measurement was
commenced. Once a well-shaped pendant oil drop was formed,
the sequential digital images of the dynamic pendant oil drop at
dierent times were acquired and stored automatically in the
personal computer. The time interval for the sequential digital
image acquisition was set to be smaller at the beginning and
larger when the pendant oil drop and surrounding CO2 were
close to an equilibrium state. Finally, the ADSA program for the
pendant drop case was executed to analyze the digital image of
the dynamic pendant drop. This program requires the local
gravitational acceleration and the density dierence between
two immiscible phases as the input data. The output data
include the dynamic IFT, the prole, volume, and surface area
of the dynamic pendant liquid drop at any time.
dx.doi.org/10.1021/je4001137 | J. Chem. Eng. Data 2013, 58, 13611370
Journal of Chemical & Engineering Data Article

Before the pendant oil drop and the surrounding CO2 Table 5. Summary of 15 IFT Tests for Five Dead/Live Light
reached an equilibrium state, the measured dynamic IFT Crude OilPure/Impure CO2 Systems at Dierent Test
changed with time due to the dissolution of CO2 into the Temperatures and Initial GasOil Ratios (GORs) in
pendant oil drop and the light-HCs extraction by CO2. After Volumea
approximately 0.5 h, the small pendant oil drop and
test gas/mole GOR MMP/
surrounding CO2 phase reached an equilibrium state, at no. T/K oil fraction (Vgas:Voil) MPa Pmax/MPa
which the measured dynamic IFT was unchanged and an
1 294.15 dead CO2 (0.99998) 4000:1 6.9 10.7
equilibrium IFT was achieved. In this study, the dynamic IFT
2 313.15 dead CO2 (0.99998) 4000:1 9.1 16.5
measurement was repeated for at least three dierent pendant
3 326.15 dead CO2 (0.99998) 4000:1 10.6 23.2
oil drops. Only the average value of the equilibrium IFTs of
4 294.15 dead 0.7487 CO2 + 4000:1 14.3 20.8
three repeated IFT measurements at the same test conditions 0.2513 CH4
was noted and is presented in this paper. The measurement 5 326.15 dead 0.8406 CO2 + 4000:1 16.3 26.7
error for such an average equilibrium IFT (eq) was found to be 0.1594 CH4
0.05 mJm2 at a prespecied equilibrium pressure (Peq) and a 6 326.15 dead 0.7487 CO2 + 4000:1 21.4 29.8
prespecied constant temperature (T), whose measurement 0.2513 CH4
errors were equal to 0.01 MPa and 0.1 K. After each 7 294.15 live CO2 (0.99998) 4000:1 7.0 9.9
8 313.15 live CO2 (0.99998) 4000:1 9.3 15.1
equilibrium IFT at a lower prespecied equilibrium pressure
9 326.15 live CO2 (0.99998) 4000:1 12.5 23.6
was measured, more pure/impure CO2 was injected to further
10 294.15 live 0.7487 CO2 + 4000:1 15.3 22.3
pressurize the high-pressure IFT cell. The equilibrium IFT 0.2513 CH4
measurement was repeated at a higher prespecied equilibrium 11 313.15 live 0.7487 CO2 + 4000:1 17.6 25.6
pressure by following the same IFT experimental procedure, 0.2513 CH4
while the test temperature was kept to be constant in each IFT 12 326.15 live 0.7487 CO2 + 4000:1 21.7 30.4
test. The IFT test was continued in a progressively increasing 0.2513 CH4
equilibrium pressure manner until either the measured 13 326.15 dead CO2 (0.99998) 200:1 10.4 23.5
equilibrium IFT (eq) reached (1.00 to 2.00) mJm2 or the 14 326.15 dead CO2 (0.99998) 10:1 10.3 22.6
tested equilibrium pressure (Peq) was as high as 26.00 MPa. For 15 326.15 dead CO2 (0.99998) 3:1 9.7 22.7
a new dynamic/equilibrium IFT test at a dierent constant a
Notes: The uncertainty of T = 0.1 K; the uncertainty of impure
temperature or initial GOR, the above-described experimental CO2 composition = 0.0001 in mole fraction; the uncertainty of
steps were repeated and the progressively increasing equili- MMP = 0.1 MPa; and the uncertainty of Pmax = 0.1 MPa.
brium pressure manner was followed from the beginning.
In this study, a total of 15 IFT tests for ve dead/live crude
oilpure/impure CO2 systems were conducted under dierent
test conditions (T and GOR), which are summarized in Table sensitive to the test temperature at GOR = 4000:1, irrespective
5. More specically, in each IFT test, the equilibrium pressure of the crude oilCO2 system tested. It is also found from
was tested and increased progressively in a large range of Peq = Figures 3(a to d) that in general, the measured equilibrium IFT
(0.10 to 26.00) MPa. The constant test temperature was reduces more slowly with the equilibrium pressure at a higher
chosen to be T = 294.15, 313.15, and 326.15 K and the initial test temperature, which results in a higher MMP or Pmax. This is
GOR (Vgas:Voil) was set to be 4000:1, 200:1, 10:1, and 3:1 in because CO2 solubility in the crude oil is lower at a higher test
volume, respectively. Table 5 also lists the measured minimum temperature if the equilibrium pressure is kept the same.
miscibility pressures (MMPs) and rst-contact miscibility Moreover, a lower CO2 solubility leads to a larger density
pressures (Pmax) for these 15 IFT tests. These experimental dierence between the crude oil phase with less dissolution of
results and the detailed eects of four important factors on the CO2 and the CO2 phase. Hence, at a higher test temperature, a
measured MMP and Pmax will be presented and discussed in the higher operating pressure (MMP or Pmax) is required for the
subsequent section. crude oilCO2 system to develop the multi-contact or rst-

contact miscibility.
RESULTS AND DISCUSSION With the above-described experimental results, the temper-
ature eects on the MMP and Pmax determined by applying the
Temperature Eects. As shown in Figure 3a, the measured VIT technique are further plotted in Figure 4. On the basis of
MMP increases from 6.9, 9.1, to 10.6 MPa when the test the measured data points (symbols) in this gure, the MMP
temperature increases from 294.15, 313.15, to 326.15 K for the (MPa) and Pmax (MPa) for the four dead/live oilpure/impure
Pembina Cardium dead oilpure CO2 system. Figure 3b CO2 (0.7487 CO2 + 0.2513 CH4) systems at GOR = 4000:1
depicts that the measured MMP for the dead oilimpure CO2 are correlated to the test temperature T (K) by applying the
(0.7487 CO2 + 0.2513 CH4) system increases from 14.3 to 21.4 linear regression:
MPa when the test temperature increases from 294.15 to
326.15 K. A large increase in the MMP for the dead oilimpure MMP/MPa = 0.116(T /K) 27.1
CO2 system is attributed to the presence of CH4 in the impure
(dead oilpure CO2 system) (1a)
CO2 phase at the initial GOR of 4000:1. Figures 3c and 3d
show that the measured MMP for the live oilpure/impure
CO2 system is always higher than that for the dead oilpure/ MMP/MPa = 0.222(T /K) 51.0
impure CO2 system. It is noted from Figures 3(a to d) that the (dead oilimpure CO2 system) (1b)
measured rst-contact miscibility pressures (Pmax) increase with
the test temperature much faster than the measured MMPs for MMP/MPa = 0.168(T /K) 42.7
the four dead/live oilpure/impure CO 2 systems. In
conclusion, both the measured MMP and Pmax are rather (live oilpure CO2 system) (1c)

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Journal of Chemical & Engineering Data Article

Figure 3. Measured equilibrium IFTs at dierent equilibrium pressures and GOR = 4000:1 for (a) the Pembina Cardium dead oilpure CO2
system: , test no. 1 (T = 294.15 K, MMP = 6.9 MPa, and Pmax = 10.7 MPa); , test no. 2 (T = 313.15 K, MMP = 9.1 MPa, and Pmax = 16.5 MPa);
, test no. 3 (T = 326.15 K, MMP = 10.6 MPa, and Pmax = 23.2 MPa). (b) The Pembina Cardium dead oilimpure CO2 (0.7487 CO2 + 0.2513
CH4) system: , test no. 4 (T = 294.15 K, MMP = 14.3 MPa, and Pmax = 20.8 MPa); , test no. 6 (T = 326.15 K, MMP = 21.4 MPa, and Pmax = 29.8
MPa). (c) The Pembina Cardium live oilpure CO2 system: , test no. 7 (T = 294.15 K, MMP = 7.0 MPa, and Pmax = 9.9 MPa); , test no. 8 (T =
313.15 K, MMP = 9.3 MPa, and Pmax = 15.1 MPa); , test no. 9 (T = 326.15 K, MMP = 12.5 MPa, and Pmax = 23.6 MPa). (d) The Pembina
Cardium live oilimpure CO2 (0.7487 CO2 + 0.2513 CH4) system: , test no. 10 (T = 294.15 K, MMP = 15.3 MPa, and Pmax = 22.3 MPa); , test
no. 11 (T = 313.15 K, MMP = 17.6 MPa, and Pmax = 25.6 MPa); , test no. 12 (T = 326.15 K, MMP = 21.7 MPa, and Pmax = 30.4 MPa).

MMP/MPa = 0.194(T /K) 42.2 It is found that in general, the measured MMP and Pmax
increase almost linearly with the test temperature in the range
(live oilimpure CO2 system) (1d) of T = (294.15, 313.15, to 326.15) K. In the literature, an
and almost linear correlation between the MMP and temperature
was reported up to 423.15 K.21 More specically, in this study,
Pmax /MPa = 0.384(T /K) 102.8 the MMP increases linearly with an increasing temperature at
the rates of (0.116, 0.222, 0.168, and 0.194) MPa/K and Pmax
(dead oilpure CO2 system) (2a) increases linearly with an increasing temperature at the rates of
(0.384, 0.281. 0.417, and 0.247) MPa/K for the above-
Pmax /MPa = 0.281(T /K) 61.9 mentioned four dead/live oilpure/impure CO2 (0.7487 CO2
(dead oilimpure CO2 system) (2b)
+ 0.2513 CH4) systems, respectively. Hence, the reservoir
temperature has strong eects on the multicontact minimum
miscibility pressure (MMP) and rst-contact miscibility
Pmax /MPa = 0.417(T /K) 113.5
pressure (Pmax) of a given crude oilCO2 system. Precisely
(live oilpure CO2 system) (2c) speaking, the MMP for the dead/live oilimpure CO2 system is
more sensitive to the test temperature than that for the dead/
Pmax /MPa = 0.247(T /K) 50.8 live oilpure CO2 system. As expected, Pmax increases with
temperature more quickly than the MMP. Moreover, the
(live oilimpure CO2 system) (2d) addition of 0.2513 CH4 (mole fraction) into pure CO2
1366 dx.doi.org/10.1021/je4001137 | J. Chem. Eng. Data 2013, 58, 13611370
Journal of Chemical & Engineering Data Article

Figure 4. Measured MMPs and Pmax values of the Pembina Cardium

dead/live oilpure/impure CO2 (0.7487 CO2 + 0.2513 CH4) systems
at dierent temperatures [T = (294.15, 313.15, and 326.15) K] and
GOR = 4000:1: , live oilimpure CO2 system; , dead oilimpure
CO2 system; , live oilpure CO2 system; , dead oilpure CO2
system.

dramatically increases the measured MMP and Pmax. On the

other hand, the live oilpure/impure CO2 system has
apparently but marginally higher MMP and Pmax than those
for the dead oilpure/impure CO2 system at GOR = 4000:1.
Oil Composition Eects. As shown in Figure 5a, the
measured MMP for the live oilpure CO2 system is moderately
higher than that for the dead oilpure CO2 system because the
live oil sample was saturated with the synthetic produced HC
gas (0.7020 CH4 + 0.1002 C2H6 + 0.1026 C3H8 + 0.0906
normal-C4H10 + 0.0046 N2). Figure 5b shows that the
measured MMP for the live oilimpure CO2 (0.7487 CO2 +
0.2513 CH4) system is only slightly higher than that for the
dead oilimpure CO2 system, both of which are far higher than
those for the dead/live oilpure CO2 systems. It is seen from Figure 5. Measured equilibrium IFTs at dierent equilibrium
these two gures that Pmax is strongly dependent on the gas pressures, T = 326.15 K, and GOR = 4000:1 for (a) the Pembina
phase composition (pure/impure CO2) but insensitive to the Cardium dead/live oilpure CO2 system: , test no. 3 (dead oil,
crude oil composition (dead/live oil). MMP = 10.6 MPa, and Pmax = 23.2 MPa); , test no. 9 (live oil, MMP
The oil composition eects on the measured MMP and Pmax = 12.5 MPa, and Pmax = 23.6 MPa). (b) The Pembina Cardium dead/
are further summarized in Figure 6, and three conclusions can live oilimpure CO2 (0.7487 CO2 + 0.2513 CH4) system: , test no.
6 (dead oil, MMP = 21.4 MPa, and Pmax = 29.8 MPa); , test no. 12
be made accordingly. First, it is found that the oil composition
(live oil, MMP = 21.7 MPa, and Pmax = 30.4 MPa).
eects on the measured MMP and Pmax are measurable but
minimal. It is worthwhile to note that at an extremely high
initial GOR of 4000:1, no dead/live oil sample was preinjected
into the high-pressure IFT cell and saturated with the existing
CO2 phase to reach an equilibrium state before a pendant
dead/live oil drop was formed. In this special case, the dead/
live oil composition was solely represented by an extremely
small ( 0.010 cm3) pendant dead/live oil drop used in the
IFT tests. This fact indicates that the ADSA technique for the
pendant drop case used in the IFT measurements is accurate
and the VIT technique applied in the MMP and Pmax
determination is reliable. Second, the oil composition eects
on the MMP and Pmax obtained in this study at GOR = 4000:1
are minimized and thus cannot represent those for a CO2-EOR
project in an oil reservoir. In the eld application case, the
residual live oil under the actual reservoir conditions is fully
Figure 6. Measured MMPs and Pmax values of the Pembina Cardium
saturated with the solution gas of primarily CH4, which can dead/live oilpure/impure CO2 (0.7487 CO2 + 0.2513 CH4) systems
signicantly increase the MMP and Pmax especially when the at T = 326.15 K and GOR = 4000:1: , impure CO2; , pure CO2.
GOR is rather low at the beginning of CO2 ooding. Finally,
Figure 6 also shows that impure CO2 with 0.2513 CH4 (mole
fraction) causes the MMP and Pmax to drastically increase. The
1367 dx.doi.org/10.1021/je4001137 | J. Chem. Eng. Data 2013, 58, 13611370
Journal of Chemical & Engineering Data
specic gas composition eects on the measured MMP and
Pmax will be analyzed in the following section.
Gas Composition Eects. It is well-known that both the
multicontact MMP and the rst-contact miscibility (Pmax)
strongly depend on the gas composition or the impurities of
CO2. In an actual eld application of a CO2-EOR project, the
injected pure CO2 will be likely coproduced with some solution
gas of HCs, the primary component of which is methane.22 In
this work, the eects of CH4 in an impure CO2 stream on the
MMP and Pmax are purposely studied by adding approximately
0.16 and 0.25 CH4 in mole fraction into pure CO2 to prepare
two dierent impure CO2 samples, respectively. Figure 7a
shows that the MMP for the Pembina Cardium dead oil at T =
326.15 K and GOR = 4000:1 increases quickly from (10.6, 16.3,
to 21.4) MPa if CH4 content increases from zero (i.e., pure
CO2), 0.1594, to 0.2513. Meanwhile, Pmax moderately increases
Figure 7. Measured equilibrium IFTs at dierent equilibrium
pressures, T = 326.15 K, and GOR = 4000:1 for (a) the Pembina
Cardium dead oilpure/impure CO2 system: , test no. 3 (pure CO2,
MMP = 10.6 MPa, and Pmax = 23.2 MPa); , test no. 5 (0.8406 CO2 +
0.1594 CH4, MMP = 16.3 MPa, and Pmax = 26.7 MPa); , test no. 6
(0.7487 CO2 + 0.2513 CH4, MMP = 21.4 MPa, and Pmax = 29.8 MPa).
(b) The Pembina Cardium live oilpure/impure CO2 system: , test
no. 9 (pure CO2, MMP = 12.5 MPa, and Pmax = 23.6 MPa); , test no.
12 (0.7487 CO2 + 0.2513 CH4, MMP = 21.7 MPa, and Pmax = 30.4
MPa).
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with CH4 content. It is worthwhile to note that at such an
extremely high GOR, the gas composition eects on the MMP
and Pmax are maximized. Figure 7b indicates that the MMP and
Pmax for the Pembina Cardium live oil at T = 326.15 K and
GOR = 4000:1 increase respectively from 12.5 MPa to 21.7
MPa and from 23.6 MPa to 30.4 MPa when 0.2513 CH4 is
added into pure CO2. Obviously, as the lightest HC gas, CH4
can signicantly increase the MMP and Pmax. This is because
CH4 has a much lower solubility in the crude oil and a much
weaker ability to extract light to intermediate HCs from the
crude oil than CO2. It is well-known that CO2 is an excellent
extracting solvent for reducing the crude oil viscosity and crude
oilsolvent IFT under the actual reservoir conditions. Thus
CH4 in an impure CO2 stream can severely prevent the
multicontact or rst-contact miscibility development.
With the above-described experimental results, the gas
composition eects on the MMP and Pmax are compared in
Figure 8. On the basis of the measured data points (symbols) in
Figure 8. Measured MMPs and Pmax values of the Pembina Cardium
dead/live oilpure/impure CO2 systems with dierent CH4 contents
(yCH4 = 0, 0.1594, and 0.2513), T = 326.15 K, and GOR = 4000:1: ,
live oil; , dead oil.
this gure, the MMP (MPa) and Pmax (MPa) measured at T =
326.15 K and GOR = 4000:1 are linearly correlated to CH4
content in an impure CO2 phase in mole fraction, yCH4, for the
dead/live oil:
MMP/MPa = 42.2yCH + 10.3 (dead oil) (3a)
4
MMP/MPa = 36.6yCH + 12.5 (live oil) (3b)
4
and
Pmax /MPa = 25.8yCH + 23.0 (dead oil) (4a)
4
Pmax /MPa = 27.1yCH + 23.6 (live oil) (4b)
4
The above four correlations show that both the MMP and
Pmax are rather sensitive to the gas composition, that is, CH4
content in CO2. They increase almost linearly with CH4
content up to 0.2513 mol fraction. More specically, the
MMP and Pmax increase linearly with an increasing CH4 content
at the rates of 0.422/0.366 MPa per 0.01 CH4 and 0.258/0.271
MPa per 0.01 CH4 for the dead/live oil, respectively. These
rates indicate that for a CO2 ooding project, the contents of
dx.doi.org/10.1021/je4001137 | J. Chem. Eng. Data 2013, 58, 13611370
Journal of Chemical & Engineering Data
the produced HCs (especially CH4) in the produced CO2
should be monitored and controlled during the entire CO2-
EOR project. In this way, the reinjected CO2 with some
produced HCs is miscible or near-miscible with the reservoir oil
at any time.23 In case the total HC content (especially yCH4) is
higher than a threshold value, some makeup pure CO2 should
be added into the produced gas (CO2 + HCs) to increase its
CO2 content prior to its reinjection. On the other hand, the
detrimental eect of CH4 on the miscibility development can
sometimes be oset by the benecial eects of the intermediate
HCs (C3 to C6) if they are present in the produced gas (CO2 +
HCs) to some extent. In this case, even though the produced
gas (CO2 + HCs) from a CO2 ood may contain a relatively
large amount of HCs (including CH4), it can still be miscible or
at least near-miscible with the residual crude oil under the
actual reservoir conditions.23,24
Initial GasOil Ratio (GOR) Eects. Figure 9a shows
lower equilibrium IFTs, relatively lower MMP and Pmax of the
dead oilpure CO2 system measured at GOR of 3:1 or 10:1.
For the dead oilpure CO2 system, its equilibrium IFT
Figure 9. Measured equilibrium IFTs of the Pembina Cardium dead
oilpure CO2 system at dierent equilibrium pressures, T = 326.15 K,
and (a) at GOR = 3:1 or 10:1: , test no. 15 (GOR = 3:1, MMP = 9.7
MPa, and Pmax = 22.7 MPa); , test no. 14 (GOR = 10:1, MMP = 10.3
MPa, and Pmax = 22.6 MPa). (b) At GOR = 200:1 or 4000:1: , test
no. 13 (GOR = 200:1, MMP = 10.4 MPa, and Pmax = 23.5 MPa); ,
test no. 3 (GOR = 4000:1, MMP = 10.6 MPa, and Pmax = 23.2 MPa).
1369
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reduction with the equilibrium pressure is mainly caused by
CO2 dissolution into the crude oil and the light-HCs extraction
from the crude oil to CO2. These two physical processes occur
simultaneously and at the end jointly cause the equilibrium IFT
reduction as the test pressure increases, especially at a low
initial GOR. In this case, both dead oil and CO2 phases are
substantially modied so that they are much similar and thus
can easily reach their multicontact or even rst-contact
miscibility. At a high initial GOR of 200:1 or 4000:1, on the
other hand, Figure 9b gives slightly higher MMP and Pmax. At a
high initial GOR, the light-HCs extraction by CO2 can make
the crude oil heavier but pure CO2 phase remains almost
unchanged because there was a small amount of dead oil inside
the IFT cell, both of which lead to marginally higher MMP and
Pmax. The experimental data in Figures 9(a and b) are combined
together and plotted in Figure 10 to manifest the initial GOR
Figure 10. Measured MMPs and Pmax values of the Pembina Cardium
dead oilpure CO2 system at T = 326.15 K and dierent initial GORs
in volume (GOR = 3:1, 10:1, 200:1, and 4000:1).
eects on the MMPs and Pmax values of the dead oilpure CO2
system at T = 326.15 K and GOR = 3:1, 10:1, 200:1, and
4000:1. It is seen from this gure that the initial GOR used in
the IFT tests has little eect on either the MMP or Pmax.
However, it is expected that the initial GOR eects on the
MMP and Pmax of the live oilimpure CO2 system will be much
stronger due to the presence of CH4 in both the live oil and
impure CO2. In fact, an initial GOR determines to what extents
the oil composition (e.g., dead/live oil) and the gas
composition (e.g., CH4 content) will aect the measured
MMP and Pmax.
CONCLUSIONS
The advanced axisymmetric drop shape analysis (ADSA)
technique for the pendant drop case is used to measure the
equilibrium interfacial tensions (IFTs) of the light crude oil
CO2 system at dierent equilibrium pressures. With the
measured equilibrium IFT versus pressure data, the vanishing
interfacial tension (VIT) technique is applied to determine the
minimum miscibility pressures (MMPs) and the rst-contact
miscibility pressures (Pmax) of ve dead/live oilpure/impure
CO2 systems under various experimental conditions. In
particular, the test temperature, crude oil composition, and
gas composition, and initial gasoil ratio (GOR) in volume are
studied to determine their specic eects on the measured
MMP and Pmax. It is found that both the MMP and Pmax
dx.doi.org/10.1021/je4001137 | J. Chem. Eng. Data 2013, 58, 13611370
Journal of Chemical & Engineering Data
increase almost linearly with an increasing test temperature in
the range of T = (294.15, 313.15, and 326.15) K. Thus the
reservoir temperature has a strong eect on the crude oilCO2
miscibility development. Moreover, both the oil composition
(from dead to live oil) at GOR = 4000:1 and the initial GOR
(from 3:1 to 4000:1) for the dead oilpure CO2 system have
measurable but weak eects on the MMP and Pmax. In the eld
applications, nevertheless, the residual live oil saturated with the
solution gas of CH4 under the actual reservoir conditions can
substantially increase the MMP and Pmax, especially at the
beginning of CO2 ooding. Also it is expected that the initial
GOR will strongly aect the MMP and Pmax of the live oil
impure CO2 system due to the presence of CH4 in both the live
oil and impure CO2. Finally, the addition of CH4 into pure CO2
drastically increases the MMP and Pmax. Therefore, CH4
content in the CO2 injection stream has to be closely
monitored and well controlled during an oileld CO2-EOR
project. If CH4 content is higher than a threshold value, the
makeup pure CO2 should be added into the produced gas
(CO2 + HCs) so that the reinjected produced gas is miscible or
at least near-miscible with the reservoir oil under the actual
reservoir conditions at any production time.
AUTHOR INFORMATION
Corresponding Author
*Tel.: 1 (306) 585-4630. Fax: 1 (306) 585-4855. E-mail: Peter.
Gu@Uregina.Ca.
Funding
The authors acknowledge the discovery grant and the
collaborative research and development (CRD) grant from
the Natural Sciences and Engineering Research Council of
Canada and the industrial R&D fund from the PennWest
Exploration to Dr. Yongan Gu.
Notes
The authors declare no competing nancial interest.
ACKNOWLEDGMENTS
The authors thank Ms. Meng Cao at the University of Regina
for editing some tables and gures.
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