Petroleum xxx (xxxx) xxx

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Asphaltene onset pressure measurement and calculation techniques:

A review
Sherif Fakher*, Amr Yousef, Aseel Al-Sakkaf, Shams Eldakar
Petroleum and Energy Engineering, The American University in Cairo, Cairo, Egypt

a r t i c l e i n f o a b s t r a c t

Article history: Asphaltene precipitation can result in several production, operational, and transportation problems
Received 8 October 2022 during oil recovery. If asphaltene precipitates and deposits, it can reduce reservoir permeability, damage
Received in revised form wellbore equipment, and plug the pipelines. It is therefore extremely important to evaluate the condi-
31 January 2023
tions at which asphaltene precipitation occurs; this is referred to as the asphaltene onset pressure.
Accepted 3 April 2023
Asphaltene onset pressure has been measured using many different experimental techniques. There have
also been many attempts along the years to predict asphaltene onset pressure using mathematical
Keywords:
correlations and models. This research provides an up-to-date comprehensive review of the methods by
Asphaltene onset measurement
which asphaltene onset pressure can be measured using laboratory experiments and mathematical
models. The research explains the main mechanisms of all the laboratory experiments to measure
asphaltene onset pressure under static conditions and how to conduct them and highlights the advan-
tages and limitations of each method. The research also provides a summary of the commonly used
mathematical models to quantify asphaltene onset pressure directly and indirectly.
© 2023 Southwest Petroleum University. Publishing services by Elsevier B.V. on behalf of KeAi
Communications Co. Ltd. This is an open access article under the CC BY-NC-ND license (http://
creativecommons.org/licenses/by-nc-nd/4.0/).

1. Introduction in the crude oil. In precipitation, asphaltene remains suspended in

Asphaltene is a solid component in the crude oil that can cause
many operational and production problems. If present in the crude
oil, asphaltene can have different chemical compositions, elemental
compositions, characteristics, and behaviors [1e5]. This makes
asphaltene one of the most complex components of crude oil.
Initially, asphaltene is stable in the crude oil as nano-colloids. If any
disturbance to this stability occurs, such as production drawdown
or enhanced oil recovery, asphaltene may begin to precipitate
[5e8]. If precipitation is not treated, asphaltene flocculation and
deposition can occur [9]. Asphaltene precipitation is when
asphaltene comes out of solution. The asphaltene becomes visible
* Corresponding author.
E-mail addresses: Sherif.fakher@aucegypt.edu (S. Fakher), amrmyousef@
aucegypt.edu (A. Yousef), AseelShawqi@aucegypt.edu (A. Al-Sakkaf), shamsalaa@
aucegypt.edu (S. Eldakar).
Peer review under responsibility of Southwest Petroleum University.
Production and Hosting by Elsevier on behalf of KeAi
the oil however, and does not deposit. Asphaltene concentration
depends on the origin of the oil and the conditions at which it was
formed. It is usually ties to the concentration of heavy components
although it can be present in light oil as well. Asphaltene instability
in the reservoir and the well column occurs when there is disrup-
tion to its thermodynamic equilibrium. This usually occurs due to
excessive drawdown during production along with the introduc-
tion of other chemicals that disrupt the molecular equilibrium of
the components of the crude oil [5,8]. Asphaltene precipitation will
occur when the asphaltene onset pressure is reached [10,11]. This
pressure varies based on the asphaltene properties, the oil prop-
erties, and the thermodynamic properties of the medium. It is vital
for this pressure to be known in order to understand the pressure
and temperature conditions at which asphaltene precipitation is
likely to occur.
Many researchers have investigated asphaltene precipitation
experimentally [12]. studied the factors impacting emulsion crea-
tion during production using artificial lift. One of the problems
identified was asphaltene and wax presence in the crude oil. The
research did not discuss how to detect asphaltene onset pressure
but rather asphaltene mitigation mechanisms which are lacking
since asphaltene onset pressure measurement could avoid severe

https://doi.org/10.1016/j.petlm.2023.04.001
2405-6561/© 2023 Southwest Petroleum University. Publishing services by Elsevier B.V. on behalf of KeAi Communications Co. Ltd. This is an open access article under the CC
BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).

Please cite this article as: S. Fakher, A. Yousef, A. Al-Sakkaf et al., Asphaltene onset pressure measurement and calculation techniques: A review,
Petroleum, https://doi.org/10.1016/j.petlm.2023.04.001
S. Fakher, A. Yousef, A. Al-Sakkaf et al.
issues which in turn would reduce or eliminate the cost of miti-
gation [13e15]. evaluated asphaltene precipitation in an Iranian oil
reservoir using experimental and modeling and simulation ap-
proaches. Based on their results, the experimental method were
much more accurate and preferable compared to the mathematical
models that could not be applied except under limited cases
[16e18]. performed an extensive study to investigate factors
impacting enhanced oil recovery in unconventional reservoir and
showed that asphaltene is a major issue in nano pores. Their results
showed that asphaltene damage in nano pores is extremely severe
which highlights the importance of asphaltene onset pressure
determination especially in extremely small pores sizes such as in
unconventional reservoirs [19]. researched asphaltene pore plug-
ging in the formation using different experimental setups including
a long slim tube sand pack. Results showed that asphaltene pore
plugging became severe especially when the long porous media
was used. This is an indication that static asphaltene onset pressure
measurement should be translated to a dynamic measurement to
determine the effect of the porous media length and fluid move-
ment [20]. showed that the interfacial behavior of live crude oil can
be used as an indication of asphaltene onset pressure. This was one
the significant methods by which asphaltene onset pressure could
be measured, however the research did not discuss the limitations
of this method compared to other methods for measuring asphal-
tene onset pressure [21]. studied the effect of asphaltene on
reducing recovery during vapor extraction oil recovery process but
did not compare it to other methods [22]. performed an experi-
mental study of asphaltene stability in crude oil using different
analysis techniques including SARA, acid number, base number, and
asphaltene onset pressure [23]. showed that asphaltene onset
pressure can be measured using a modified mercury-free PVT
apparatus with an optical observation cell however they did not
discuss the limitations of this method [24]. quantified oil solvent
quality for a mixture of crude oil with asphaltene using refractive
index [25]. developed a novel method of determining asphaltene
onset flocculation using kinematic viscosity measurements. Based
on the above, asphaltene onset pressure has been measured using
many different experimental techniques, however the difference
between each of these techniques and the optimum technique to
use under different conditions have not been significantly high-
lighted in any of the studies mentioned above, which raises an issue
of the importance of comparing all the methods used to determine
asphaltene onset pressure in crude oil.
Asphaltene precipitation has also been studied using mathe-
matical equations and modeling [26]. presented a new method to
quickly predict asphaltene onset pressure using rate dependent
calculations with a nominal uncertainty of 500 psi [27]. studied
asphaltene stability in crude oil with compositional change [28].
developed a model that relies on titration lab data to study
asphaltene flocculation behavior under different conditions [29].
provided a method for asphaltene instability prediction based on
experimental analysis of asphaltene behavior [30]. developed a
compositional model using experimental results to model asphal-
tene onset pressure during carbon dioxide injection [31]. provided
an overview on the properties of asphaltene including two of the
most famous mathematical models used to model asphaltene
behavior [32]. used downhole fluid analysis adnd the Flory-
Huggins-Zuo equation of state to analyze two case studies
involving asphaltene instability [33]. Combined Arrhenius and
Vogel-Tammann-Fulcher Equations to provide an improved equa-
tion to model asphaltene onset [34]. used the Cubic Plus Associa-
tion Equation of State to assess the impact of temperature and
initial pressure on asphaltene onset [35]. developed a scaling
equation to determine asphaltene onset pressure [36]. incorpo-
rated effect of deposition rate, entrainment, and pore plugging on
2
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asphaltene precipitation in an equation. It can be observed that
different mathematical models have been developed for asphaltene
onset pressure determination all of which have multiple limita-
tions. This highlights the importance of undergoing experimental
tests to determine asphaltene onset pressure.
Asphaltene onset pressure can be measured using a plethora of
methods all of which have their advantages and limitations. It can
also be predicted using different mathematical techniques that
have different restrictions based on how they were developed, and
the data used in their development. Based on this, it is important to
provide an updated guide to the different methods present to
predict asphaltene onset pressure and under what conditions each
of these methods can be used effectively and accurately. This
research provides a detailed review of all the different experi-
mental methods for measuring asphaltene onset pressure under
static conditions. The review will focus on the experimental pro-
cedures, setups, advantages and limitation. Following this, the
research will elaborate on how each experimental method can be
improved. The research will also focus on the mathematical models
that have been introduced as a direct and indirect method for
asphaltene onset measurement. Overall, this research aims to
provide a roadmap to the different methods by which asphaltene
onset pressure can be measured or calculated.
2. Asphaltene thermodynamic properties
Asphaltene passes through multiple phases in the crude oil
depending on the crude oil properties, reservoir properties,
asphaltene properties and concentration, and operational param-
eters during production. Based on these parameters, the four main
asphaltene behaviors. These behaviors have unique characteristics
that are explained as follows [37]:

Asphaltene stable: Initially before production, the asphaltene is
stable in the crude oil. Following the Yen-Mullins model of
nanocolloidal structures of asphaltenes, asphaltenes exist in the
crude oil as nanocolloids. Although asphaltenes can be stable in
the reservoir initially, many oil reservoirs are at or near their
asphaltene onset pressure. This is due to the presence of
incompatible oil and gas charges. When a gas charge occurs in
an oil reservoir, the gas can diffuse in the oil thus increasing the
solution gas. This results in asphaltene expulsion from the oil in
an equilibrium distribution of clusters. This has been reported in
many oil reservoirs worldwide [38].

Asphaltene precipitation: Once a disturbance occurs in the
reservoir, usually manifested in production or injection, the
asphaltene stability conditions become compromised. This re-
sults in asphaltene precipitation. This is the most important
asphaltene behavior since it the main component measured
using the asphaltene onset pressure measurements. Precipita-
tion is defined chemically as coming out of solution. During this
behavior, the asphaltene becomes visual in the crude oil, how-
ever it remains suspended in solution. Asphaltene precipitation
is reversible if it occurs for a short duration, and can be treated
effectively if detected early [39]. The fact that asphaltene be-
comes detectable is one of the main methods by which
asphaltene onset pressure can be measured.

Asphaltene flocculation: Following asphaltene precipitation,
the asphaltene molecules begin cohering to each other, a pro-
cess referred to as flocculation. This coherence results in the
formation of larger asphaltene particles known as flocculation.
Asphaltene flocculation begin increasing in density to a point
where they are no longer able to be suspended in the crude oil.
The detected asphaltene flocculation during asphaltene testing
can be as small as 10 nm.
S. Fakher, A. Yousef, A. Al-Sakkaf et al.

Asphaltene Deposition: Once the density of the asphaltene
flocculation exceeds that of the crude oil, the flocculation begins to
deposit into the pores of the formation; this is referred to as
asphaltene deposition. This is the most severe form of asphaltene
damage that can result in pore plugging and permeability reduc-
tion. Asphaltene deposition does not occur in a downward direc-
tion. Instead, asphaltene deposition behaves in a form relative to
heterogeneous nucleation [38]. The asphaltene tends to stick to
the pore surface and grows on it. This coating mechanism is one of
the main reasons why asphaltene can alter the formation wetta-
bility to strongly oil wet. The sticking mechanism is mainly due to
conformal free energies of the asphaltene flocculation.
Asphaltene onset pressure can be defined as the pressure at which
asphaltene precipitation occurs at a given temperature. This pressure
is vital since it can detect asphaltene instability at an early stage
where mitigation is still relatively simple. Asphaltene stability is a
function of pressure and temperature, as is shown in Fig. 1. At
reservoir conditions the asphaltene is not visible. Once the upper
asphaltene boundary is reached, the asphaltene begins precipitating.
This is the line for asphaltene onset at different temperatures. It is
important to note that the phase diagram does not show any liquid
asphaltene phase. This is because asphaltene cannot be liquified. If
asphaltene is heated excessively it will disintegrate, therefore it
cannot be converted to a liquid state, which is the main reason behind
asphaltene being a severely damaging component [40e44].
3. Asphaltene onset pressure
3.1. Asphaltene onset pressure measurement
There are various methods by which asphaltene onset pressure
can be measured experimentally. The main methods are explained
in this section. For each method, there may exist slight variations.
These variations will also be mentioned and explained, if available.
Also, it is important to note that many of the methods discussed can
be applied to the reservoir and the well column. This research in-
cludes all the AOP methods in general in order for the research to be
a guideline for asphaltene measurement techniques.
3.1.1. Near infrared light scattering method (NIR-LSM)
This is one of the most commonly used methods to measure
asphaltene onset pressure [45,46,47,13,26,48,49,50,51,52,19].
Fig. 1. Asphaltene Phase Behavior [43].
3
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Although there are more than ten different variations to the setup,
the fundamental operational method remains the same. An illus-
tration of the most fundamental setup to measure asphaltene onset
using NIR-LSM method is presented in Fig. 2. The setup is composed
of a pump to provide pressure to a high-pressure glass cell. The cell
houses the crude oil with asphaltene in it. A laser source emits near
infrared light to the sample as the pressure changes. A detector
receives the signal, and the transmitter relays the signal to a
computer.
The exact experimental procedure to measure asphaltene onset
pressure using the NIR-LSM method is as follows:
1. The high-pressure glass cell is filled with a predetermined vol-
ume of crude oil at a specific pressure and temperature condi-
tion using the pump and a heating jacket.
2. The near infrared laser source begins emitting rays through the
cell. The pressure in the cell is then gradually decreased via a
piston.
3. The detector detects the emitted rays and transmits the reading
to the transmitter. This reading is then received by the computer
and a plot is drawn with the laser strength versus the pressure.
4. The pressure keeps decreasing until asphaltene begins precipi-
tating from the oil. This results in an abrupt change in the laser
strength on the computer screen. This can then be used to
measure asphaltene onset pressure.
5. The process can be repeated by increasing the pressure and then
decreasing it again to ensure repeatability of the experiment.
The experiment should be conducted at a constant temperature
since a variation in temperature will result in a change in the
asphaltene onset pressure.
The NIR-LSM method is one of the most commonly used
methods due to many advantages. These include that it can be
performed at a wide range of pressures and temperatures and re-
quires a small sample of oil to conduct. Also, since it relies on near
infrared source, it can also be used in dark samples. One of the
limitations of this method is that small pressure increments should
be done to ensure that the exact asphaltene onset pressure is
recorded, which can be slightly difficult if a low accuracy pump is
used. Since asphaltenes are stable in the crude oil as nanocolloids,
there is a large range of undetected asphaltene particles when
using optics. This is mainly due to the optics method being
diffraction limited. This is the main limitation of the optics method
for asphaltene onset pressure detection [53].
Dumont, H. et al. [54] also introduced a method to measure
asphaltene onset pressure in oil wells real time at reservoir depth.
This was done using optical light scattering methods. The downhole
fluid analyzed managed to obtain accurate measurements for mul-
tiple parameters including saturation pressure and asphaltene onset
pressure. This introduced multiple advantages including measure-
ment at reservoir pressure, minimum sample handling thus reducing
costs, real time asphaltene onset pressure measurement, and
asphaltene onset pressure measurement before sample cooling
which could lead to irreversible asphaltene flocculation.
3.1.2. Organic deposition cell (ODC)
The ODC can be seen as a combination of two different tech-
niques including NIR-LSM method and the visual method [55]. An
illustration of the ODC apparatus is presented in Fig. 3. The setup is
composed of a high-pressure cell that houses the crude oil. A
luminescent spectrophotometer is connected to the setup via fiber
optics. The cell is equipped with a heat jacket to provide a wide
range of temperatures if needed.
The ODC is almost identical to the near infrared light scattering
technique, explained previously. The only main difference is that
S. Fakher, A. Yousef, A. Al-Sakkaf et al.
Fig. 2. Near infrared light scattering method experimental setup.
Fig. 3. Odc experimental setup.
instead of using a near infrared light, or laser, source, this method
uses a luminescent spectrophotometer is connected to the setup via
fiber optics. The procedure used to conduct the experiment for the
ODC is therefore identical to that of the near infrared light scat-
tering methods. The only difference is that instead of a detector, the
spectrophotometer is used to detect the light scattering from the
fiber optics.
This method has the same advantages and limitations of the
NIR-LSM with the only variation being the light source. The varia-
tion in the light source can create a limitation for this method since
the near infrared light source can be more penetrating that the
source used in this method.
3.1.3. Pendant drop approach (PDA)
The PDA experimental setup is primarily used to measure
interfacial tension (IFT). This method was adopted by some re-
searchers to attempt to quantify asphaltene onset pressure as a
function of change in IFT [20,56]. A simple illustration of the PDA
apparatus is presented in Fig. 4. The setup is very similar to that of
the NIR-LSM however instead of a laser source, a high-resolution
camera is used to take pictures of the oil sample. The procedure
is also very similar to the NIR-LSM method but instead of a laser
source, the images are transmitted to the computer for IFT analysis.
Above the asphaltene onset pressure, the IFT and contact angle
measurements of the crude oil follow a normal trend. Once the
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pressure falls beneath the asphaltene onset pressure, a sharp
change in the trend is observed. This is due to asphaltene wetta-
bility alteration of the sample. This sharp change can be used as an
indication of asphaltene onset pressure.
The PDA method is not widely used for asphaltene onset
pressure determination due to two main limitations. The first
limitation is that it provides an indication of asphaltene onset
pressure and does not directly measure it. The pressure is
determined indirectly as a function of IFT change. This can
reduce the accuracy of the value significantly. The second main
reason is that since the method relies on high resolution images,
it cannot be used in dark colored samples. The samples will have
to be diluted first which may impact the accuracy of the mea-
surements. It is important to note that there are modified IFT
equipment that can determine the IFT of any sample regardless
of its color, however another limitation arises, which is the
inability to conduct the experiment at high pressures and tem-
peratures. Since the IFT of the asphaltene solution continues to
change with time, the baseline also changes which could result
in erroneous readings. Also, this method is very difficult to apply
at elevated temperatures and pressures. This method can be used
if a simple indication of the asphaltene onset pressure is required
as a side result, however, for the goal of measuring asphaltene
onset pressure with high accuracy, more accurate methods
should be used.
S. Fakher, A. Yousef, A. Al-Sakkaf et al.
Fig. 4. Pda experimental setup.
3.1.4. Filtration technique
The filtration technique relies on visually determining asphal-
tene presence in the oil through a filter membrane [50,51]. An
illustration of the apparatus for the asphaltene onset pressure
determination using the filtration technique is presented in Fig. 5.
The setup is composed of a cell that houses the crude oil under a
high pressure. The cell is connected to a filter membrane which is
connected from the other side to a back pressure regulator (BPR).
The BPR is used to mimic reservoir conditions and prevent the
immediate escape of the fluids by apply and opposing pressure. The
fluids will need to overcome this opposing pressure applied by the
BPR in order to exit the setup. The BPR is usually adjusted using an
inert gas or distilled water. A separator is then attached to the outlet
of the BPR along with a flow meter.
The exact experimental procedure used to conduct the filtration
technique to determine the asphaltene onset pressure is as follows:
1. A high-pressure cell is loaded with live crude oil. Initially, the
crude oil is above saturation pressure, so the gas is completely
dissolved in the oil.
2. The pressure in the cell is reduced gradually in small pressure
steps. With each pressure step a small volume of crude oil is
allowed to flow through the outlet.
3. The extracted crude oil then flows through a filter membrane.
The membrane must have extremely small pores, ideally less
than 10 nm to detect any asphaltene particles.
4. The oil that flows through the filter membrane then passes
through a backpressure regulator to maintain its pressure. The
back pressure regulator is pressurized from the other side using
an inert gas, usually nitrogen or argon.
5. After passing through the back pressure regulator, the oil then
flows through a separator to separate the liberated gas from the
Fig. 5. Filtration technique experimental setup.
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oil. The oil is then collected for further analysis, and the gas
flows through a flow meter to determine its rate.
6. The filter membrane can then be extracted and analyzed for
asphaltene concentration. This is conducted by dissolving the
filtrate in a light normal alkane, such as n-heptane. If asphaltene
is present, it will deposit to the bottom.
7. This is repeated under different pressures until the filtrate
analysis indicates the presence of asphaltene. When this occurs,
this is considered a direct indication of asphaltene onset
pressure.
The filtration technique has a lot of major advantages including
the ability to verify the experimental results visually by seeing the
asphaltene. The setup is also very flexible with the filter membrane
size being very easy to change if needed. Also, the experiment can
be conducted at high pressure and high temperatures and can be
used with a variety of crude oils regardless of their color and
darkness. The limitation of this method is that if an improper pore
size for the filter membrane is selected, the asphaltene can pass
through and thus a false asphaltene onset pressure will be
measured. This can be detected by analyzing the fluid collected
from the separator for any asphaltene concentration that was not
detected in the filter membrane. Another major limitation with the
filter membrane is that sometimes under high pressures it can
rupture, especially if the membrane is made of paper. The solution
is to use a high strength polymeric membrane or a solid membrane.
It is also advised to include a solid screen behind the membrane to
avoid rupturing. The solid screen should have an extremely large
mesh size to avoid interfering with the experiment by creating a
back pressure on the flow. Finally, it is important to note that
filtration is less sensitive to small sized asphaltene flocculation
compared to optics.
S. Fakher, A. Yousef, A. Al-Sakkaf et al. Petroleum xxx (xxxx) xxx

3.1.5. Precipitation method with UVevisible spectrophotometer

The precipitation method relies on the usage of a titrant to
analyze asphaltene onset pressure. Although the method can rely
on visual analysis, it becomes much more accurate with the
incorporation of an ultra-violet visible spectrophotometer
[22,48,28,29,27]. An illustration of the titration apparatus equipped
with an ultra-violet visible spectrophotometer is presented in
Fig. 6. The setup is composed of a high-pressure cell that houses a
precipitant used to dilute the crude oil. The crude oil is housed in
another vessel. A spectrophotometer is attached to the crude oil
vessel to detect change in the properties of the crude oil.
The exact procedure that is used to conduct the titration method
with UVeVisible spectrophotometer to determine asphaltene onset Fig. 7. Ect experimental setup.
pressure follows an ASTM standard procedure, D 6703, and is as
follows.
3.1.6. Electrical conductivity technique (ECT)
This technique relies on measurement of an electric current to
1. Initially, an accumulator is filled with a precipitant. This is
determine asphaltene instability [51]. An illustration of the elec-
usually a fluid that can induce asphaltene precipitation. The
trical conductivity technique for asphaltene onset determination is
most commonly used precipitant are normal alkanes including
presented in Fig. 7. The setup is composed of a high-pressure cell
n-pentane and n-heptane.
housing the crude oil attached to a multimeter. The cell is housed in
2. The precipitant filled accumulator is attached to a high pressure
an oven for temperature adjustment. A pump is used to control the
pump from one side and to a high pressure vessel to the other
pressure inside the cell.
side.
The procedure used to measure asphaltene onset pressure using
3. The high-pressure vessel is filled with crude oil that is to be
the ECT is as follows:
tested. The oil is initially pressurized above saturation pressure.
A valve is used to isolate between the crude oil and the
1. The high-pressure cell is filled with crude oil at a high pressure.
precipitant.
The pressure is provided via the high-pressure injection pump.
4. The experiment begins by injecting the titrant into the vessel
2. The cell is placed in an oven at a predetermined temperature
housing the crude oil at a pre-specified injection rate. As the
and is left to heat up for a long duration to ensure that the
precipitant begins interacting with the crude oil, asphaltene will
temperature distribution is uniform. A heating jacket can also be
begin to precipitate from solution.
used instead of an oven, although the oven will produce a more
5. An ultraviolet spectrophotometer is used to transmit a signal
uniform and constant temperature distribution.
through the sample during the experiment. If the crude oil
3. A multimeter is attached to both sides of the high-pressure cell.
contains a considerable volume of asphaltene, an inflection
The multimeter is set to measure electrical conductivity. The
point will be registered when the asphaltene precipitates. This
multimeter should begin logging the conductivity data before
inflection point can be used to determine the asphaltene onset
the experiment is commenced to provide a reference reading at
pressure.
the initial conditions.
4. The pressure in the cell is then reduced in gradual steps while
The precipitation method is one of the most commonly used
logging the electrical conductivity using the multimeter. The
methods due to its clear and well-established procedure. It is very
pressure steps should be small and consistent.
simple to use and can be applied under a wide range of pressure
5. Asphaltene precipitation results in a variance in the electrical
and temperature conditions. The two main limitations of this
conductivity of the oil and thus can be detected easily using the
method include the presence of gas and the selection of the titrant.
multimeter. This is a direct indication of the asphaltene onset
If the crude oil sample used is a live sample, the precipitant injected
pressure. The pressure can be read at the pump interface, or a
may interact with the gas and thus produce a false asphaltene onset
pressure valve or transducer can be used.
pressure reading. Also, varying the titrant can vary the mechanism
by which the asphaltene behaves, and thus different asphaltene
The ECT is one of the easiest and fastest methods to use. It has a
onset pressure values may be obtained for the same crude oil
wide range of applicability and is not limited to pressure,
sample.

Fig. 6. Titration method with UVevisible spectrophotometer experimental setup.

6
S. Fakher, A. Yousef, A. Al-Sakkaf et al.
temperature, or crude oil properties. The method is considerably
rapid and can provide an immediate value for the asphaltene onset
pressure without the need for any mathematical equations or al-
terations. The two limitations of this method are the accuracy of the
multimeter and the location of the two poles attached to the
multimeter to record the electrical conductivity, which is why a
reference reading before the experiment begins is vital. Another
limitation is that the high-pressure cell must be able to transmit
electricity and thus some material cannot be used such as plastic
and glass.
3.1.7. Modified mercury free PVT apparatus
The modified mercury free PVT apparatus relies on a high-
resolution microscope and a diluent to determine asphaltene pre-
cipitation [57,23]. An illustration of the experimental setup for this
method is presented in Fig. 8. The setup is composed of an aging
cell that contains the crude oil. A diluent housed an accumulator
that is attached to the aging cell. A high-resolution microscope is
attached to the aging cell to observe the oil sample at a high res-
olution. A sample can also be withdrawn from the aging cell for
further analysis.
This method is considered relatively new, and therefore there is
no agreed upon experimental procedure for it. However, the most
commonly used procedure to determine asphaltene onset pressure
using this experimental setup is as follows:
1. A diluent is placed in a high-pressure accumulator. The diluent is
usually a chemical that can dilute the crude oil sample. This
includes a wide range of aromatics such as xylene or toluene.
2. The crude oil is placed in a high-pressure aging cell at a pre-
determined pressure. The cell could be entirely transparent or
could be made of steel with a glass window. The high-pressure
cell is connected to the diluent accumulator.
3. When the experiment begins, the diluent is injected into the
crude oil sample with a predetermined concentration. The
sample is left to age for a specified time. A microscope with a
high magnification is attached to the cell. It is used to visually
detect asphaltene precipitation. The cell is sometimes equipped
with a fiber optic light bundle to provide some illumination if
the crude oil sample is too opaque.
4. If asphaltene precipitation is detected, the pressure is recorded,
and a sample of crude oil is extracted from the aging cell for
further analysis under the microscope.
The main advantage of this method is the ability to visualize
asphaltene precipitation using a microscope. This method has
several limitations however, including that if the sample is too dark
Fig. 8. Modified mercury free PVT apparatus experimental setup.
7
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to method will fail to detect asphaltene accurately. Also, the vari-
ation of the diluent can impact the asphaltene stability in the crude
oil. Finally, the microscope may not have a large enough accuracy to
detect very small asphaltene particles and thus can result in a
misidentification of the asphaltene onset pressure.
3.1.8. Kinematic viscosity measurement (KVM)
This method relies on the concept of viscosity variation due to
change in composition of the crude oil. The method has different
variation, all of which function based on viscosity reading. The
variations can be in the measurement itself with some setups
designed to measure kinematic viscosity, while others detect ab-
solute or dynamic viscosity. The variation can also be in the setup
with some setups using a diluent to reduce the viscosity of the
crude oil gradually and others do not. Also, the viscometer used to
measure the viscosity value can also differ from one setup to the
other [58,25].
An illustration of a setup used to determine the asphaltene
onset pressure using the KVM method is shown in Fig. 9. The setup
is composed of diluent housed in a high-pressure accumulator. The
crude oil is housed in an aging cell. The cell can be heated by
attaching a heating jacket to it. The outlet of the aging cell is
attached to a high-pressure viscometer. The type of viscometer can
vary from one setup to the other, however, it must be a high-
pressure viscometer to be able to measure the viscosity of the
crude oil leaving the aging cell at high pressure.
The procedure used to measure the asphaltene onset pressure
using the viscosity, kinematic or dynamic, variation method is as
follows:
1. A diluent is placed in a high-pressure accumulator that is
attached to the aging cell housing the crude oil. If the diluent is
not needed, then this step can be neglected. Usually, the diluent
will only be needed if the viscosity of the crude oil is too high to
be detected by the viscometer, therefore the viscosity of the oil
will need to be reduced.
2. The aging cell houses the crude oil that is pressurized to a
predetermined pressure. If heating is required, a heating jacket
is attached to the aging cell. Heating should be conducted before
beginning the experiment.
3. The pressure of the crude oil is reduced gradually in equal
pressure steps. With each pressure step, a volume of the crude
oil is allowed to move through the valve and enter the high-
pressure viscometer.
4. The high-pressure viscometer is then used to measure the crude
oil viscosity. If the experiment is run at a high temperature, the
viscometer should be equipped with a heating element to avoid
abrupt change in temperature.
S. Fakher, A. Yousef, A. Al-Sakkaf et al. Petroleum xxx (xxxx) xxx

Fig. 9. Kvm experimental setup.

5. When asphaltene onset pressure is reached, a sudden variation 1. A predetermined volume of crude oil is placed in a high-
in the viscosity of the crude oil will be detected. This is due to pressure vessel at the design pressure. The oil is pressurized
the asphaltene being a very heavy component, and thus a small via a high-pressure pump attached to the cell.
variation in the asphaltene concentration will result in a varia- 2. An acoustic source is used to emit an acoustic wave at a specific
tion of the crude oil viscosity. If the kinematic viscosity is being frequency. The acoustic source should be placed at a known
measured, then the density of the crude oil must also be known. distance from the cell. If the distance varies, the new distance
In this case, a densitometer should be used to measure the must be known and adjusted on the computer software to avoid
variation in the density of the crude oil as well. errors in the calculation of the asphaltene onset pressure.
3. The acoustic wave is maintained constant for the duration of the
This method is one of the most widely used method to measure experiment. The pressure in the cell is reduced gradually. The
asphaltene onset pressure due to its multiple advantages. These reduction in pressure will impact the acoustic waves propa-
include ability to run under different pressures and temperatures. gating through the cell. This change will be detected by the
Also, the setup is highly modifiable based on the properties of the detector and then recorded as a graphical plot on the computer.
asphaltene and the crude oil. The limitations of this method include 4. Once asphaltene onset pressure is reached, the behavior of the
the use of a diluent, if needed, which may impact the oil behavior, acoustic wave will change significantly. This significant change
live oil is usually not since the gas can impact the viscosity readings, will appear at the detector. This abrupt change is a direct indi-
and the type of viscometer used may impact the value of the cation of asphaltene onset pressure.
asphaltene onset pressure as well.
The acoustic resonance method has many advantages including
the ability to be run at high pressures and temperatures and is not
3.1.9. Acoustic resonance technique (ART)
limited to the color, origin, or source of the crude oil. Its main
The acoustic resonance technique relies on acoustic waves to
limitations include the need for a relatively large volume of oil to
determine the asphaltene onset pressure [47,51]. An illustration of
run the experiment compared to other methods. Also, the acoustic
the experimental setup used to measure asphaltene onset pressure
source distance from the cell, frequency and amplitude must be
using the acoustic resonance technique is presented in Fig. 10. The
known initially in order to be able to accurately determine the
setup is composed of a high-pressure cell housing the crude oil. An
asphaltene onset pressure. The distance of the receiver from the
acoustic source is used to generate a sound wave. A receiver detects
aging cell must also remain constant to avoid change in the read-
the sound wave after it passes through the cell. The receiver then
ings. The distance must be predetermined in the experimental
transmits the reading to a computer which logs the data.
design, and should be input to the computer software before
The exact procedure used to quantify asphaltene onset pressure
running the experiment.
using the acoustic resonance techniques is as follows:

Fig. 10. Acoustic resonance technique experimental setup.

8
S. Fakher, A. Yousef, A. Al-Sakkaf et al. Petroleum xxx (xxxx) xxx

asphaltene onset pressure. There are many variations to the setup

which include complex equipment [47,59,10]. An illustration of the
main setup used to measure asphaltene onset pressure using the
gravimetric analysis technique is presented in Fig. 11. The setup is
composed of a high-pressure aging cell that houses the crude oil.
The cell is attached to a densitometer which measures the density
of the fluid passing through it. The densitometer transmits the
density reading to a computer which logs the data.
The main procedure followed to conduct the asphaltene onset
pressure measurement using the gravimetric method illustrated in
Fig. 11 is as follows:

1. The crude oil is placed in a high-pressure aging cell at a pre-

determined pressure. The pressure is provided by the pump
attached to the aging cell.
2. The pressure is then reduced gradually in the cell. After each
Fig. 11. Gravimetric analysis technique experimental setup. pressure reduction step, a small sample of the crude oil flows
through the valve into the densitometer.
3. The density of the fluid sample is measured and recorded on the
3.1.10. Gravimetric analysis technique (GAT) computer screen. Once the asphaltene onset pressure is
The gravimetric method relies on a weight change measure- reached, an abrupt change in density is observed on the com-
ment. It is one of the oldest and most established methods to detect puter screen. This is due to the asphaltene precipitating from the

Table 1
Asphaltene onset pressure mathematical models.

Model Name Mathematical Model Description Variables Reference


Flory-Huggins-Zuo va o nva gðr  ra Þðh2  h1 Þ Used to determine asphaltene R is the universal gas [32]
2 2
Equation of State ODðh2 Þ ∅a ðh2 Þ f ½da  dh1  ½da  dh2 RT instability constant
¼ ¼ e RT e
ODðh1 Þ ∅a ðh1 Þ ∅ is the volume fraction
n h 1 1
 io
va ð ð
v is the molar volume
v h3 v h1 d is the solubility
e
parameter
T is the temperature g is
the gravitational
acceleration
r is the density h is the
depth
   
Cubic Plus Association Aex
assoc 1  XA 1  XR Enables the determination of R is the universal gas [34]
¼ NA xA ln XA þ þ NR xR ln XR þ
Equation of State nRT 2 2 temperature and pressure constant
conditions for asphaltene T is the absolute
precipitation temperature n is the
total number of moles
A and R denote
asphaltene and resin
N is the number of
associated sites for
asphaltene and resin x
is mole fraction
X is the mole fraction in
lean phase (not bonded
at the association sites)
Scaling equation 0:321811  P 0:023622
Rc ¼ Xc  Mw c
Used to determine asphaltene Pc is the critical [35]
onset pressure asphaltene
precipitation pressure
Rc is a factor that
depends on crude oil
composition
Mw is the solvent
molecular weight
Viscosity Change vsp The volume of nonprecipitated W is the weight of [63]
W ¼ c
Model 5 0 asphaltene dissolved asphaltene c
q
2 is the concentration of
suspended particles
vsp is the specific
viscosity
q is a fluid dynamical
particle volume
rffiffiffiffiffiffi
Hilderbrand Solubility DE Indicates the solvency behavior DE is the heat of [31]
Parameter d ¼ of a specific solvent vaporization v is the
v
molar volume
d Hilderbrand Solubility
Parameter

9
S. Fakher, A. Yousef, A. Al-Sakkaf et al.
crude oil. Since the asphaltene is one of the heaviest compo-
nents of crude oil, precipitation of the asphaltene results in a
noticeable change in the oil sample density.
The gravimetric asphaltene onset pressure measurement
technique is one of the most applied methods due to the simplicity
of the method and rapidness of the test. Although multiple vari-
ations exist, the fundamental concept remains the same. One of
the main limitations of this method is the sensitivity and accuracy
of the densitometer especially if the asphaltene concentration is
low.
3.1.11. Combined method
Researchers have also attempted to construct experimental
setups to combine multiple methods together [59,19]. This is
mainly used as a means to overcome the limitations of each setup
individually and to compare the asphaltene onset pressure using
different readings. Although the accuracy of these setups are high,
their main limitations include high complexity, high cost, and
interference of some components of the setup with the others
which may result in incorrect readings.
3.2. Asphaltene onset pressure mathematical modeling
Many mathematical models have been developed to quantify
asphaltene onset pressure as a function of different parameters.
Although widely used, these methods have some limitations in
their application, mainly due to the wide variations in the structure
of asphaltene, and therefore the experimental methods are still
preferred [60e62]. A summary of the main mathematical models
developed to quantify asphaltene onset pressure is provided in
Table 1. The three most commonly used mathematical models are
the Flory-Huggins-Zuo Equation of State, Cubic Plus Association
Equation of State, and Hilderbrand Solubility Parameter. These
models are the most commonly used since they have an extremely
wide range of applicability. The remaining models are empirical
models that can only be applied under the conditions through
which they have been developed. All in all however, these models
should not be used unless the means by which experimental
methods can be used are not available. The models are usually used
to match the experimental results and then for predication using
other parameters after matching.
4. Conclusions
This research provides an updated guideline to the different
experimental methods and mathematical models used to mea-
sure or quantify asphaltene onset pressure. Each experimental
method was explained with an illustration of the experimental
setup and the procedure followed to conduct the experiment. The
advantages and limitations of each method are also mentioned.
The mathematical models used to quantify asphaltene onset
pressure were tabulated with all the variables explained. Also,
the three main mathematical models used to calculate asphaltene
onset pressure were highlighted. Due to the importance and
complexity of measuring asphaltene onset pressure, this research
provides a concise and up to date guide on the different methods
developed to measure this parameter regardless of the crude oil
origin and the asphaltene properties, concentrations, and
structure.
Statements of declaration
No funds, grants, or other support was received.
10
Petroleum xxx (xxxx) xxx
Declaration of competing interest
On behalf of all the co-authors, the corresponding author states
that there is no conflict of interest.
The datasets generated during and/or analyzed during the cur-
rent study are available from the corresponding author on
reasonable request.
Nomenclature
R is the universal gas constant, J mol1 K1
∅ is the volume fraction, fraction
v is the molar volume, m3/mol
T is the temperature, R or K
g is the gravitational acceleration, ft/s2
r is the density, lbm/ft3
h is the depth, ft
n is the total number of moles, mol
A and R denote asphaltene and resin, dimensionless
N is the number of associated sites for asphaltene and
resin, dimensionless
x is mole fraction, fraction
X is the mole fraction in lean phase (not bonded at the
association sites), fraction
Pc is the critical asphaltene precipitation pressure, psi or Pa
Rc is a factor that depends on crude oil composition,
dimensionless
Mw is the solvent molecular weight, g/mol
W is the weight of dissolved asphaltene, grams
c is the concentration of suspended particles, amount of
particles in millions
vsp is the specific viscosity, cp
q is a fluid dynamical particle volume, ml
DE is the heat of vaporization, J/kg
d Hilderbrand Solubility Parameter, cal1/2/cm3/2
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