Determination and evaluation of minimum miscibility

pressure using various methods: experimental, visual

observation, and simulation
Muslim Abdurrahman, Wisup Bae, Asep Kurnia Permadi

To cite this version:

Muslim Abdurrahman, Wisup Bae, Asep Kurnia Permadi. Determination and evaluation of minimum
miscibility pressure using various methods: experimental, visual observation, and simulation. Oil &
Gas Science and Technology - Revue d’IFP Energies nouvelles, Institut Français du Pétrole, 2019, 74,
pp.55. �10.2516/ogst/2019028�. �hal-02157027�

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REGULAR ARTICLE

Determination and evaluation of minimum miscibility pressure using

various methods: experimental, visual observation, and simulation
Muslim Abdurrahman1,*, Wisup Bae2, and Asep Kurnia Permadi3
1
Department of Petroleum Engineering, Universitas Islam Riau, Indonesia
2
Department of Energy and Mineral Resources Engineering, Sejong University, Republic of Korea
3
Department of Petroleum Engineering, Institut Teknologi Bandung, Indonesia

Received: 8 October 2018 / Accepted: 18 April 2019

Abstract. This research proposes a simultaneous technique using various methods to yield the most reliable
Minimum Miscibility Pressure (MMP) value. Several methods have been utilized in this study including slim
tube test, swelling test, vanishing interfacial tension test, visual observation during swelling test and vanishing
interfacial tension test, and simulation. The proposed method may reduce the uncertainty and avoid doubtful
MMP. The method can also demonstrate discrepancies among the results. There were two samples used in this
study namely Crude Oil AB-5 and Crude Oil AB-4. It showed that for Crude Oil AB-5 the discrepancies among
the results from that of the slim tube test were between 3.9% and 10.4% and 0% and 5.9% for the temperature
of 60 °C and 66 °C, respectively. The highest discrepancy was shown by the results from the visual observation
during vanishing interfacial tension test and the lowest discrepancy was shown by the results from the swelling
test. The vanishing interfacial tension test was found to be the fastest method for predicting the MMP. The
method also consumed a smaller amount of oil and gas samples for the experiment. The simultaneous method
proposed in this study is considered as more proper and exhibits a valuable method for predicting the MMP.
This technique has never been found to be performed by previous researchers and accordingly it becomes
the strong point of this study to contribute to the global research in the area of MMP determination.

1 Introduction and Abdurrahman et al. (2015). In their study, they com-

pared the results using two or three methods to yield the
The Minimum Miscibility Pressure (MMP) is essential for more reliable MMP. Nevertheless, none of the mentioned
CO2 injection. The MMP can be determined either by lab- researchers have compared the results of using more than
oratory experiments or numerical studies. Several research- three methods.
ers have introduced experiments methods for predicting the In this study, we propose a new approach to produce the
MMP such as Yellig and Metcalfe (1980), Christiansen and MMP with high confidence level and less doubtful results.
Haines (1987), Wang (1986), Hagen and Kossack (1986), We use various methods including slim tube test, vanishing
Rao (1997), Tsau et al. (2010), Abdurrahman et al. interfacial tension test, swelling test, visual observation
(2015), Alomair et al. (2015), and Rahimi et al. (2017). through swelling and vanishing interfacial tests, and simu-
Some other methods have also been introduced by lations in order to obtain the MMP. Our approach is to
Cronquist (1978), Johnson and Pollin (1981), Sebastian simultaneously plot results of slim tube test vs. swelling
et al. (1985), Glaso (1985), Ahmed (2000), and Stalkup test, VIT test vs. swelling test, and slim tube test vs. VIT
and Yuan (2005). However, each individual method has dis- test in the same graph. In the analysis, we include results
tinctive disadvantages in yielding the accurate value as dis- of visual observation and simulations to obtain more rea-
cussed by Danesh (1998), Johns and Orr (1996), Ayirala sonable MMP value.
and Rao (2006), and Tsau et al. (2010). Several researchers
have tried simultaneous methods in order to reduce the
uncertainties including Thomas et al. (1994), Elsharkawy 2 Preparation and procedures
et al. (1992), Ayirala and Rao (2006), Tsau et al. (2010),
Various stages are intentionally prepared to yield appropri-
* Corresponding author: [email protected] ate results of either slim tube test, swelling test, vanishing

This is an Open Access article distributed under the terms of the Creative Commons Attribution License (http://creativecommons.org/licenses/by/4.0),
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2 M. Abdurrahman et al.: Oil & Gas Science and Technology - Rev. IFP Energies nouvelles 74, 55 (2019)

Fig. 1. The procedure of study.

interfacial test, visual observation, and simulation. After- 2.2.2 Swelling test
wards, the entire results are compared to each other as a
means to examine any discrepancy among the results. The main apparatus used for the swelling test in the present
Figure 1 exhibits the flowchart of our research methodol- study consists of a high-pressure cell made of sapphire glass.
ogy, while the following explanations describe each experi- To fill-up the cell by CO2 we use precision pump namely
ment stage conducted in the current study. ISCO Pump 250DM. A heater is used to control the tem-
perature of the air bath system. To help control the CO2
liquid state before it is injected into the cell we use a cooler.
2.1 Light oil composition and CO2 quality To obtain images and to record the course of the experi-
ment we use a simple camera located outside of the air bath
Two types of crude oil are used in this study. The crude oil system. A stirring bar located inside the cell is used to mix
samples are taken from Layer AB-4 and AB-5 within Air the CO2 and oil until it reaches its equilibrium condition.
Benakat Formation of South Sumatra Basin located in A rare magnet located within a slot outside the cell is used
Jambi Province, Indonesia. The composition and other to control the movement of the bar. Other standard auxil-
properties of the oil samples are shown in Tables 1, iary equipment for measuring pressure and temperature are
S1a, and S1b. The CO2 gas used in this study has 99.99% also included in the experimental system. Our swelling test
of purity. experimental diagram is shown in Figure 2.

2.2 Experimental apparatus and procedures

2.2.3 Vanishing interfacial test
2.2.1 Slim tube test
The experimental diagram of the vanishing interfacial test
The procedure for the experiments generally consists of is shown in Figure S2. Two syringe pumps from ISCO
three major stages including preparation, experiment, and Company is used for water and CO2 injections and a
cleaning stages. The stages applied for the slim tube test goniometer apparatus from Rame-Hart Instrument Co.
as well as the other tests. The preparation stage for the slim combined with a visual cell is used for this experiment.
tube test includes leak testing, slim tube saturation using A high-pressure and high-temperature visual cell is
the sample of up to 2.0 PV, Back-Pressure Regulator equipped to measure the Interfacial Tension (IFT) in reser-
(BPR) setting at the desired pressure, and air bath temper- voir condition. The cell diameter is 30 mm, its height is
ature system setting at the reservoir condition. The experi- 60 mm, and its thickness is 16 mm. The maximum operat-
mental stage involves CO2 injection at the rate of ing pressure and temperature of the visual cell are 3000 psi
0.2 cc/min until it reaches 1.2 PV, effluent collection in and 300 °C, respectively. The needle, which has Outside
the measuring cylinder and oil volume measurement. At Diameter (OD) of 0.91 mm and length of 50 mm and made
the same time, the change in oil color is observed in the from stainless steel is used. A pair of face-to-face sapphire-
visual cell for estimating the condition of miscibility then glass window is equipped within the visual cell. The glass
the oil recovery is calculated for each pressure and the windows with the thickness of 10 mm and the diameter of
results are plotted. The cleaning stage involves oil sample 30 mm is attached to the visual cell. A certain volume of
cleaning in the slim tube using toluene and then nitrogen. dead-oil is mounted on the stainless-steel piston-chamber
The miscibility is estimated at the break-over point in the with 0–4000 psi maximum operating pressure. A metering
plot of recovery factor vs. pressure as suggested by Yellig valve and a check valve are applied to ensure the constant
and Metcalfe (1980). The experimental diagram of the slim oil flow rate and to prevent the flow-back within the cell.
tube test is shown in Figure S1. The description and speci- The temperature is measured with a calibrated thermocou-
fication of the slim tube is shown in Table S2. ple located inside the cell. Afterwards, the pressure of the
 M. Abdurrahman et al.: Oil & Gas Science and Technology - Rev. IFP Energies nouvelles 74, 55 (2019) 3

Table 1. Sample properties (Abdurrahman et al., 2015). the oil and the CO2 become one phase or the oil drop disap-
pears from the needle tip at some higher pressure. This phe-
Properties AB-4 AB-5 nomenon can be easily observed by visual means. Again,
API Gravity 20 41.38 regardless this method is effective in recognizing when the
miscibility occurs; it is obviously not accurate and should
Reservoir temperature (Tr) [°C] 60 65
be regarded only as approximation.
Reservoir pressure (pr) [psi] 786 1134
Bubble point pressure (pb) [psi] 740 1116 2.2.5 Simulation
Viscosity [cp] 4.6 0.21
Zick (1986) discovered a combination between condensing
and vaporizing gas drive mechanisms during miscibility
process of CO2 and crude oil. However, this phenomenon
system is measured through a pressure indicator. All appa- cannot be observed using ternary diagram. Therefore,
ratus is connected by using stainless steel tubing lines. according to Zick, various methods using numerical simula-
Before initiating the measurement, all lines and the tions have been proposed by Jaubert et al. (1998a, 1998b),
apparatus are cleaned by using toluene, dried by using and Jaubert et al. (2002). Jaubert et al. (1998a) pointed out
nitrogen, and vacuumed. The pressure inside the cell is their study on predicting the MMP using a slim tube simu-
conditioned by injecting some CO2 into the cell. Then, lator. The result showed excellent accuracies compared to
the temperature condition is maintained constant by instal- 1D simulator. In addition, the compositional slim tube sim-
ling the heater. A sequential experiment is run with a serial ulator was about 18–80 times faster compared to 1D simu-
condition of pressure that ranges from 700 to 2500 psi and lator. Jaubert et al. (1998a) devoted their study on using
temperature that ranges from 60 °C to 66 °C. After that, real petroleum fluid model. They mentioned that one cell
the pressure and temperature inside the cell are constantly simulator has some limitations for estimating the MMP.
maintained according to the desired condition which usu- Due to the time consuming and very expensive experiments
ally takes about 20–30 min. The water with a specific rate for determining the MMP, Jaubert et al. (2002) conducted
of 0.1 cc/min is pumped into the chamber and the piston swelling and multiple contact tests in their study. They con-
pushes up the dead oil inside the chamber. The dead oil is cluded that the two tests are faster and cheaper for predict-
flown from the chamber through the tubing line until it ing the MMP.
reaches the needle’s tip. When the oil drop reaches the nee- In these days, numerical simulators offer several options
dle’s tip, the drop hang and this condition is maintained at for predicting the MMP. This paper uses CMG simulator of
stable condition for a certain time by adjusting the meter- which it provides options in WinProp that can be utilized
ing valve. In this experiment, the stable condition of the to calculate the MMP. The Multiple-Contact Miscibility
drop should be maintained between 40 and 60 s. This time (MCM) option or the First-Contact Miscibility (FCM)
range has been suggested by previous researchers including pressure for a given oil and solvent at a particular temper-
Yang and Gu (2005) and Yang et al. (2015). ature or the Minimum Miscibility Enrichment (MME) level
that is required for the multiple- or single-contact miscibil-
2.2.4 Visual observation ity at given temperature, pressure, oil composition, primary
and make up gas composition are available in the program.
Visual observation during swelling test The C7+ characterization has to be made since the splitting
Visual observation is performed through images captured as of the oil compositional data of the samples is not possible
videos or pictures similar to the method conducted previ- while the simulator requires components to be defined until
ously by Wang (1986). This method has also been per- C35. The MMP can then be determined for a given solvent
formed by Abdurrahman et al. (2015). This method is composition by entering a range of pressure to be tested.
aimed to observe visually the change in color of the oil as The program reports the MMP if it is found and the mech-
the pressure increases. The observation is done during the anism by which the miscibility occurs is achieved. It could
extraction-condensation stage when the swelling factor be vaporizing or condensing drive mechanisms.
begins to decrease. The MMP should be obtained when For the MMP calculation in the present study, the pres-
the interface of the CO2-rich phase and the CO2 vapor dis- sure increment is divided into 10 steps. The calculation
appears. According to Abdurrahman et al. (2015), this begins with the lowest pressure of 500 psi and terminates
method is obviously not accurate and should be regarded at the maximum pressure of 2500 psi. The results including
only as an approximate method to estimate the MMP. the ternary diagrams are collected for each pressure step of
which is used to specify the pressure range and values cor-
Visual observation during VIT test responding to the MMP. The required data for the simula-
Visual observation through videos or pictures during the tion includes temperatures of 60 °C and 66 °C, pressures
vanishing interfacial test is used in determining the MMP ranging from 500 psi to 2500 psi, oil composition, and the
in this study. This is aimed to observe the change in drop primary gas composition, i.e. the CO2 with the purity of
shape of the oil as the pressure increases. When the pressure 99.99%. The equation of state used in this work is
in the view cell is increased, the CO2 dissolves in the crude Peng–Robinson EOS. The viscosity model is that of
oil and the oil drop shape at the tip of the needle gradually Jossi–Stiel–Thodos with the aqueous phase salinity (or
changes. This phenomenon occurs until the oil drop disap- NaCl) concentration equals to zero. The simulator version
pears at the tip of the needle. The MMP is obtained when is CMG Sofware (2014).
4 M. Abdurrahman et al.: Oil & Gas Science and Technology - Rev. IFP Energies nouvelles 74, 55 (2019)

moderate components are rapidly extracted from the oil

drop causing the CO2 to be oil-rich. This phenomenon leads
to the decrease of the Interfacial Tension (IFT) between the
oil and the CO2. However, when the pressure increases and
reaches the near-miscibility condition the heavy component
remains in the crude oil. At this condition, the oil drop
begins to shrink and the IFT reduces quite slowly. Based
on this explanation, in the present study two regions are
recognized during the vanishing interfacial test. The first
is referred to as Region A representing the diffusion stage
and the second is referred to as Region B representing the
shrinkage stage. In this regard, the MMP is determined
by linear extrapolation of the diffusion line versus pressure
data to zero value of IFT. A linear regression analysis for
estimating the MMP of Crude Oil AB-5 at temperatures
of 60 °C and 66 °C results in the equations below:

IFT ¼ 0:0262  P þ 42:22; ð1Þ

Fig. 2. The diagram of swelling test experiment (Abdurrahman IFT ¼ 0:0226  P þ 40:17: ð2Þ
et al., 2015).
The first equation is for estimating the MMP at 60 °C
with the correlation coefficient is found to be
3 Results R2 = 99.99%. The second equation is for estimating the
MMP at 66 °C with the correlation coefficient is found to
3.1 Estimating MMP by slim tube test be R2 = 99.99%. According to the value of R2 for these
The slim tube test experiment uses Crude Oil AB-5 for two equations, it is believed that the estimated MMP is consid-
reservoir temperature conditions of 60 °C and 66 °C. The erably acceptable. Nevertheless, these equations can only be
slim tube experiment results for both temperatures are applied to a pressure range between 700 psi and 1500 psi for
shown in Figure S3. The MMP is determined by using the temperature of 60 °C and between 700 psi to 1550 psi
the break-over point technique as suggested by Yellig and for the temperature of 66 °C. Above these two-pressure
Metcalfe (1980). The results from this slim tube experiment ranges the equation many not be applicable due to the
show that the miscibility occurs at 1540 psi and 1700 psi for occurrence of different phenomena.
the two temperature conditions of 60 °C and 66 °C, Similarly, a linear regression analysis for estimating the
respectively. MMP of Crude Oil AB-4 at temperatures of 60 °C and
66 °C results in the equations below:
3.2 Estimating MMP by plots of swelling factor
IFT ¼ 0:0255  P þ 48:92; ð3Þ
vs. pressure
The swelling test experiment offers a new technique for esti-
mating the MMP graphically by plotting the resulted swel- IFT ¼ 0:0258  P þ 53:44: ð4Þ
ling factor as a function of pressure. Tsau et al. (2010)
suggested in their experiment on how to predict the The first equation is for estimating the MMP at 60 °C
MMP based on data resulted from a swelling test. The with the correlation coefficient is found to be R2 = 98.7%.
approach involves the determination of the MMP by recog- The second equation is for estimating the MMP at 66 °C
nizing the intersection between the extraction-condensation with the correlation coefficient is found to be R2 = 99.1%.
line and the condensation line. According to the value of R2 for these equations, it is also
Figure S4 shows that the intersection between the con- believed that the estimated MMP is considerably accept-
densation-extraction line and the extraction line that occurs able. Again, because of the occurrence of different phenom-
at the pressure of 1600 psi and 1700 psi. As a result, for the ena at other pressure values, these equations can only be
temperature of 60 °C, the MMP can be estimated as 1600 applied to a pressure range between 700 psi and 1800 psi
psi and for the temperature 66 °C, the MMP is obtained for the temperature of 60 °C and 700 and 1900 psi for the
as 1700 psi. Due to some technical limitations, this method temperature of 66 °C.
can only be applied to Crude Oil AB-5. The MMP estimates under elevated pressure and tem-
perature for Crude Oil AB-5 are shown in Figure S5 while
3.3 Estimating MMP by plots of IFT vs. pressure the MMP estimates for Crude Oil AB-4 are shown in
Figure S6. Using Equations (1) and (2) at the IFT value
An experimental study performed by Yang and Gu (2005) equals to zero the interfacial tension shows that the misci-
explained that during the diffusion process the light and bility in Crude Oil AB-5 occurs at 1611 psi and 1777 psi
 M. Abdurrahman et al.: Oil & Gas Science and Technology - Rev. IFP Energies nouvelles 74, 55 (2019) 5

for the temperatures of 60 °C and 66 °C, respectively. It can that the CO2 can extract only the oil components of C5 to
also be seen that the MMP increases as the temperature C30 (Stalkup, 1984). Photographic sketches illustrating the
increases. Increasing the temperature from 60 °C to 66 °C process of miscibility development were demonstrated by
causes the increase in the MMP of about 166 psi or Wang (1986) when the oil shrinks to its minimum volume.
27.7 psi/°C. Similarly, using Equations (3) and (4) at the
IFT value equals to zero the interfacial tension shows that
the miscibility in Crude Oil AB-4 occurs at 1918 psi and 3.4.2 Visual observation during VIT test
2072 psi for the temperatures of 60 °C and 66 °C, respec- Wang (1986) suggested that the MMP can be estimated
tively. The MMP also increases as the temperature visually during a swelling test experiment. The method
increases. The increase in temperature from 60 °C to 66 ° has also been done by Abdurrahman et al. (2015) to predict
C causes the increase in the MMP of about 154 psi or the MMP in their experiments. In the present work, the
25.7 psi/°C. These results are reasonably consistent with MMP is also proposed to be predicted by visual observation.
those of Hemmati-Sarapardeh et al. (2013). In their study, Figure S10 depicts the phenomena in Crude Oil AB-5 during
the increase of the MMP is about 22.6 psi/°C. At higher vanishing interfacial test at the temperature of 60 °C.
temperature, the CO2 solubility in the crude oil is lower, Clearly, at 1700 psi, the oil drop shape cannot be recognized
which results in a higher MMP. as can be seen in the figure. Figure S11 depicts the same
phenomena during the vanishing interfacial test for Crude
3.4 Estimating MMP by visual observations during Oil AB-5 at the temperature of 66 °C. The oil drop shape
swelling test and vanishing interfacial test slightly changes as the pressure increases. In this experi-
ment, the oil drop shape starts to change its shape to an
3.4.1 Visual observation during swelling test irregular form when the pressure is higher than 1650 psi.
The MMP may be estimated by visual observation during At the pressure of 1800 psi, the oil drop shape cannot be
the swelling tests as suggested by Wang (1986). In the pre- recognized clearly as can be seen in the figure.
sent study, the observation is focused on the occurrence Figure S12 depicts the phenomena during the vanishing
when the swelling factor begins to decrease which happens interfacial test at the temperature of 60 °C for Crude Oil
in the extraction-condensation stage. It should be noted AB-4. The oil drop slightly changes as the pressure
here that the MMP estimate through visual observation is increases. It is clearly seen during the experiment that the
certainly subjective and may not reflect the correct MMP. oil drop shape does not change to irregular form until the
The timing when the extraction-condensation and the pressure reaches 2600 psi. The IFT between oil and CO2
extraction stages occur in the cell should also be determined at this pressure is 0.91 dyne/cm. This value can be
carefully. Relating to the means the MMP is defined, the categorized as ultra-low IFT. Figure S13 depicts similar
MMP is estimated when the interface of the CO2-rich phase phenomena for Crude Oil AB-4 during the vanishing inter-
and the CO2 vapor disappears. Figure S7 and Figure S8 facial test at the temperature of 66 °C. It is also clearly seen
depict the phenomenon during the swelling test for Crude from the figure that the oil drop shape does not change to
Oil AB-5. The oil color changes slightly as the pressure any irregular form until the pressure is increased to
increases. The more notable oil color change occurs when 2600 psi. This is the highest pressure possible during the
the swelling factor starts to decrease suggesting that the experiment. Any changes above this pressure is not possible
miscibility of the CO2 and the oil has been achieved. As due to some technical reasons. At the pressure of 2600 psi,
mentioned by Huang et al. (1989) and Wang (1986), the the drop shape is still recognized as regular and the interfa-
phenomenon when the oil color starts to change from its cial tension between the oil and CO2 at this pressure is
original color as the pressure increases is known as the tran- found to be 2.41 dyne/cm.
sition zone. While the pressure keeps increasing at this
stage, the CO2 and the oil dissolve each other and eventu- 3.5 Determining MMP by simulations
ally become one phase. Then, the color of the oil looks
brighter. In this experiment, the oil color starts to change Our simulation results using Peng–Robinson EOS calcu-
at the pressure of 1600 psi and 1700 psi for the temperature lated the MMP for Crude Oil AB-5 as 1670 psi and
of 60 °C and 66 °C, respectively. 1790 psi at 60 °C and 66 °C, respectively. Similarly, for
In the extraction process, the pressure is higher than the Crude Oil AB-4, the MMP was found to be 2030 psi and
MMP and the oil color changes to even much brighter as 2240 psi at 60 °C and 66 °C, respectively. The cell-to-cell
can be seen in Figure S9. This phenomenon results from a method is used in estimating the miscibility by detecting
large number of moderate components of the oil that has the pressure at which the tie line reaches the critical point.
been extracted leaving only the heavier components to The simulation method is much faster than the experiment.
remain at the bottom of the cell. The heaviest component It also does not require much input data. In this work, the
subsequently precipitates in the form of black asphaltic MMP calculation is done without any tuning in predicting
flakes as it was also observed by Wang (1986). Assuming the phase behavior as suggested by Danesh (1998). The
the yellow color observed within the cell represents the critical properties of the hydrocarbon and non-hydrocarbon
moderate components, this finding reveals clear evidences components are defined in the simulator as shown in
that the CO2 extracts only the intermediate components Table S3. The binary interaction coefficients between the
of the oil. Similar observation results were also obtained hydrocarbon and non-hydrocarbon components are shown
by previous investigators. In their reports, it was mentioned in Table S4 and Table S5.
6 M. Abdurrahman et al.: Oil & Gas Science and Technology - Rev. IFP Energies nouvelles 74, 55 (2019)

4 Discussion Regardless the dominant effect of pressure, the temper-

ature in fact plays an important role in the extraction-
4.1 Comparing MMP estimations between slim tube vs. condensation stage as well as in the extraction stage that
pressure and swelling factor vs. pressure follows. Because the solubility of CO2 in oil is low at higher
temperatures, the extraction of the oil components is also
In this analysis, the MMP is determined graphically from low. Thus, during the CO2 injection process at the higher
the results of the swelling test by plotting the swelling factor temperature of 66 °C, the CO2 dissolves only slightly in
as a function of pressure. This can only be done for Crude the oil as indicated in Figure S4 causing low concentration
Oil AB-5 because of the limited data from the slim tube of the hydrocarbon that can be extracted. As a result, the
test. As suggested by Tsau et al. (2010), the MMP can be oil shrinkage is also low during the extraction-condensation
obtained when the straight-line curves of the extraction- stage and the oil volume returns to its initial condition as
condensation stage and the extraction stage intersects each indicated by the swelling factor of unity. When the injection
other. Therefore, the two curves representing the two stages is conducted at the lower temperature of 60 °C, a different
are important to estimate the occurrence of miscibility and phenomenon occurs where more CO2 dissolves into the oil
accordingly the MMP cannot be estimated with high-level and the oil shrinkage is quite high as indicated in Figure S4.
of certainty if the straight lines cannot be well developed Then, because more oil components are extracted during
from the experimental data. In the condensation-extraction the extraction-condensation stage, the swelling factor
stage that is also called near-miscibility condition, the light- decreases to a value of less than 1.0. However, when the
to-moderate components vaporize quite fast. Meanwhile, temperature increases, the MMP also increases. In the pre-
due to the already-reduced amount of the components, less sent study, the increase in temperature of 6 °C leads to the
moderate components vaporize in the extraction stage. The increase of the MMP by 100 psi or about 16.7 psi/°C. This
swelling factor decreases in both stages because CO2 has result is very much close to the result of the work by
extracted the light-to-moderate components. The intersec- Elsharkawy et al. (1992). They reported that the increase
tion between the extraction-condensation and extraction of the MMP affected by the increase of temperature fell
straight lines is therefore crucial to construct in order to within the range of 18.10 psi/°C and 27.02 psi/°C. Figure S4
ensure the correct miscibility pressure. The solubility of clearly shows this effect of temperature on the MMP. At
CO2 in oil increases as the pressure increases during the con- higher temperatures, the condensation-extraction and the
densation stage and so the swelling factor. At some point, extraction lines will be slightly flatter than the lines at lower
the oil is rich with the CO2 and at the same time the oil temperatures. The logical reasoning for this phenomenon
reaches its maximum swelling factor. It is clearly shown may be because at higher temperature the CO2 extract less
in Figure S4 that the swelling factor reaches its maximum oil components and accordingly it requires higher pressure
value of about 1.3 at 1400 psi. The miscibility, however, to achieve miscibility condition resulting in higher MMP.
has not yet occurred. After the oil is fully saturated by Figure S14 displays combined plots comparing the
CO2, the extraction-condensation stage begins and few results of the slim tube experiment and those of the swelling
moderate components of the oil move into the CO2 phase test each of which for the temperatures of 60 °C and 66 °C.
as indicated by the decrease in swelling factor. The extrac- Analyzing the plots graphically, the MMP resulted from the
tion stage occurs as the pressure increases further where the swelling test is obviously in good agreement with that from
CO2 vaporizes and more moderate components leave the oil the slim tube experiment. In other words, the MMP
phase causing the swelling factor to decrease continuously obtained from the swelling test in the present study is con-
but at different rate. As a result, for the temperature of siderably correct. This result therefore invalidates the
60 °C, the MMP is determined as 1600 psi (see Fig. S4). doubting relationship previously noted by Harmon and
Using the same procedure, the results for the other temper- Grigg (1988) between the MMP obtained from the slim
ature of 66 °C is also shown in Figure S4. The MMP for this tube experiment and that from the swelling test. The differ-
case is obtained as 1700 psi. One thing that is important to ence between the MMP obtained from the slim tube and
note here is the effect of CO2 solubility on the swelling fac- that from the swelling test is about 3.9% for the tempera-
tor. At higher pressure, the CO2 solubility is also higher ture of 60 °C and basically zero for the temperature of
making its effect on the swelling factor is more significant. 66° C (see Table S6).
Therefore, the swelling factor of 1.4 at 66 °C and 1600 psi
that is higher than that of 1.3 at 60 °C and 1400 psi in these
experiments is mainly due to the effect of pressure which is 4.2 Comparing MMP estimations between swelling
more dominant than temperature. factor vs. vanishing interfacial test
It is clearly understood from Figure S4 that the MMP
cannot be determined if the extraction stage does not occur In this analysis, the results for Crude Oil AB-5 are exam-
so that the intersection between the straight-lines of the ined. Figure S15 shows combined plots comparing the
extraction-condensation stage and the extraction stage can- results of the vanishing interfacial test and that of the swel-
not be identified. Because the extraction stage is quite faster ling test at the temperatures of 60 °C and 66 °C, respec-
than the rate of swelling after the miscibility occurs, the tively. A graphical analysis on the plots clearly shown
extraction causes the swelling factor to decrease rapidly. that the MMP resulted from the swelling test is also in good
This phenomenon was also reported by previous investiga- agreement with that of the vanishing interfacial test. As a
tors such as Tsau et al. (2010) and Harmon and Grigg result, the MMP obtained from the swelling test and that
(1988). from the vanishing interfacial test in the present study
 M. Abdurrahman et al.: Oil & Gas Science and Technology - Rev. IFP Energies nouvelles 74, 55 (2019) 7

proved to be considerably correct. As displayed in Table S7, interfacial test is conducted the oil surrounded by the CO2
the differences between the results of the swelling test and is too small averaging only 3–8 lL. Because of the small
that of the vanishing interfacial test are about 0.7% and oil volume, the process is not able to depict the three regions
4.3% for the temperature of 60 °C and 66 °C, respectively. such as the process occurs during swelling test. However,
It follows that the MMP obtained from the swelling test from the similarity of the curve trend and the slope changes
and that from the vanishing interfacial test at low temper- between the swelling test and the vanishing interfacial test
atures are closer to each other than the same results at during the extraction process it is believed that at the pres-
higher temperatures. In the meantime, the MMP obtained sure above the MMP the heavy component is dominating
from vanishing interfacial test is slightly higher than that the oil composition. Figure S4 as well as Figure S5 to
obtained from the swelling test. However, the difference is Figure S6 may be useful to describe such phenomenon.
still reasonable as it is considerably a small figure. It is unfortunate that due to some technical reasons the
Following the explanation provided by Yang and Gu swelling test and the slim tube test cannot be performed for
(2005), two regions namely Region A for diffusion stage Crude Oil AB-4. Therefore, the similar analysis to the
and Region B for shrinkage stage are recognized. In Region results for Crude Oil AB-5 cannot be done for Crude Oil
A the CO2 diffuses into the crude oil causing the oil to swell AB-4. However, as the composition may affect considerably
and accordingly the Interfacial Tension (IFT) to decrease. the MMP as explained above, the higher molecular weight
In this study, the IFT in Region A is found to decrease from of the heptane-plus in Crude Oil AB-4 compared to Crude
24.5 dyne/cm to 2.93 dyne/cm at 60 °C and 24.9 dyne/cm Oil AB-5 may be responsible for the higher MMP of Crude
to 3.4 dyne/cm at 66 °C. However, as the pressure contin- Oil AB-4 in the IFT experiment at both temperatures of
ues to increase the oil drop is lacking of moderate compo- 60 °C and 66 °C. To be precise, different composition
nent leaving heavy component as the main constituent of between the two oil samples results in different MMP. In
the oil drop. In that condition the oil volume decreases this case, the higher content of heavy component in Crude
owing to the shrinkage of the oil drop. On the other hand, Oil AB-4 results in the higher MMP. Line B or shrinkage
in Region B the remaining heavy component in the oil drop line of the IFT results proves the heavy component richness
only causes the IFT to slowly decrease. In this region, the of Crude Oil AB-4. Also, the IFT still exist even at high
IFT decreases from 2.6 dyne/cm to 2.5 dyne/cm at 60 °C pressures. Hence, the MMP in Crude Oil AB-4 is logically
and 3.0 dyne/cm to 2.1 dyne/cm at 66 °C. This phe- higher than that of Crude Oil AB-5. Table S8 shows the
nomenon is clearly shown in Figure S15. Regarding the comparison of the MMP for the two oil samples based on
MMP explanations according to the molecular effects, the the VIT test results.
logical reasoning may be expressed as follows. When the
CO2 injection pressure increases at Region A, more CO2 4.3 Comparing MMP estimations by slim tube
molecules will diffuse into the oil. Thus, the oil density vs. VIT test
decreases rapidly. The higher the injection pressure, the
denser the CO2 causing its density to be higher. This condi- Because of the slim tube and VIT tests results availability,
tion minimizes the density difference between the CO2 and further analysis can be done for Crude Oil AB-5. Figure S16
the oil drop. Lower density difference means the operating shows combine plots comparing the results of the slim tube
intermolecular forces between the CO2 and the oil will be and VIT tests at 60 °C and 66 °C, respectively. The MMP
close at Region B. The interface between the CO2 and resulted from the VIT test is in good agreement with that
the oil disappears when the operating intermolecular force obtained from the slim tube test. It then follows that the
between the two phases is in balanced condition. It is also MMP obtained from the VIT test is considered satisfacto-
believed that near-miscibility occurs at the intersecting rily correct. By plotting the slim tube and the VIT tests
point between Region A and B lines in the plot of the results in the same graph, the uncertain and doubtful
IFT vs. pressure. Prior to the near-miscibility region the MMP from the VIT result can be diminished. The plot also
IFT decreases more rapidly as the pressure increases. In provides enhancement to the MMP estimation. Table S9
contrast, after the near-miscibility region (or shrinkage shows the results of the MMP as well as their differences
region) the IFT continues but slowly decreases as the pres- between the two tests. As shown in the table, the discrepan-
sure increases. This is probably because of the domination cies between the two methods are 4.5% at 66 °C and 4.6%
of the heavy component. at 66 °C, respectively. In other words, the effect of temper-
It follows from the above that the existence of the inter- ature is not significant.
secting lines of the extraction-condensation and the extrac-
tion stages is crucial in estimating the MMP through 4.4 Comparing MMP estimations by experiments
swelling test. During the swelling test, three regions namely vs. simulation
condensation, condensation-extraction, and extraction
occur and can be recognized easily. These regions do not The slight disagreement between the results of experimental
exist and cannot be recognized during the vanishing interfa- and simulation methods is most likely caused by the specific
cial test. The logical reasoning may be expressed as follows. property of the oil sample used in each method. The slim
When the swelling test is conducted, the oil volume is as tube test, the vanishing interfacial test and the swelling test
much as 2.1 mL and it causes more CO2 to dissolve into use dead oil samples while the simulation uses live oil sam-
the oil. In that process, it is easy to recognize the three ples. The gas composition in the live oil sample such as
regions through the view cell. However, when a vanishing methane and nitrogen causes the MMP slightly higher
8 M. Abdurrahman et al.: Oil & Gas Science and Technology - Rev. IFP Energies nouvelles 74, 55 (2019)

(Dong et al., 2000). Table S10 shows the differences 7. Despite the closeness of the results, each method has
between the results of the swelling test and the simulation shown results that are in fact different to each other.
for Crude Oil AB-5 are about 4.2% and 5.0% at the temper- However, in general, all the methods can be properly
ature of 60 °C and 66 °C, respectively. Meanwhile, the dif- used for predicting the MMP.
ferences between the results of the vanishing interfacial test
and that of the simulation are about 3.5% and 0.7% at the
temperature of 60 °C and 66 °C, respectively. Then, the dif- Acknowledgments. This work is financially supported by the
ferences between the results of the slim tube test and that of Energy Resources R&D Program of the Korea Institute of
simulation are about 7.8% and 5.0% at the temperature of Energy Technology Evaluation and Planning (KETEP) and
60 °C and 66 °C, respectively. It then follows that all the by the Korean Government Ministry of Trade, Industry and
experimental methods including the swelling test, the Energy through Sejong University, Korea. The Authors also
vanishing interfacial test, and the slim tube test provide wish to thank Universitas Islam Riau and CMG for the encour-
satisfactory estimates of the MMP. It can also be seen in agement of writing this paper.
the table that the MMP estimated by the VIT method
has the closest value to the MMP from the EOS method.
In contrast, the highest difference from EOS method is Supplementary Material
the result of the slim tube test. Furthermore, the difference
of the MMP values obtained from swelling test to that of Supplementary material is available at https://ogst.ifpen-
the EOS is consistent at both temperatures. As a conclu- ergiesnouvelles.fr/10.2516/ogst/2019028/olm.
sion, the MMP at a specific temperature resulted from Figures S1 to S17 and Tables S1 to S12.
the methods used in the present study does not show a sin-
gle or exactly the same value. There is always a discrepancy
among the results no matter how small it is.
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