SPE 164184

Asphaltene Precipitation From Crude Oils : How To Predict It And To

Anticipate Treatment?
Nicolas Passade-Boupat, Honggang Zhou, Marianna Rondon-Gonzalez, Total Exploration & Production

Copyright 2013, Society of Petroleum Engineers

This paper was prepared for presentation at the SPE Middle East Oil and Gas Show and Conference held in Manama, Bahrain, 10–13 March 2013.

This paper was selected for presentation by an SPE program committee following review of information contained in an abstract submitted by the author(s). Contents of the paper have not been
reviewed by the Society of Petroleum Engineers and are subject to correction by the author(s). The material does not necessarily reflect any position of the Society of Petroleum Engineers, its
officers, or members. Electronic reproduction, distribution, or storage of any part of this paper without the written consent of the Society of Petroleum Engineers is prohibited. Permission to
reproduce in print is restricted to an abstract of not more than 300 words; illustrations may not be copied. The abstract must contain conspicuous acknowledgment of SPE copyright.

Abstract
The prediction of asphaltene precipitation is an important topic in petroleum industry. Reliable evaluation of the asphaltene
stability requires representative samples and measurement using special high pressure equipment. Moreover, development
project may involve many reservoirs with many different fluids. Even inside of a connected reservoir, the quality of the oil
and the asphaltene can vary through a large scale and the investigation of each fluid in the representative conditions become
very expensive and often impossible.
Many fast screening methods have been proposed so far. The De Boer’s diagram is one of the most useful methods.
However, it takes into account only the properties of the hydrocarbon phase without any investigation on the asphaltene
fraction : this method gives always pessimistic prediction of the risk of asphaltene precipitation. Other methods, colloidal
instability index for example, are not consistent enough to be used for flow assurance issue.
Based on some relevant solubility properties of the asphaltene fractions, a new and easy way for screening asphaltene
instability is proposed. Using PVT properties of the live oil and an easy asphaltene characterization procedure, this method
allow limiting advanced investigation only to fluids which present a real risk of precipitation. The asphaltene characterization
can be performed on dead oil samples.
If a precipitation risk is stated, additional tests, performed on pressurized representative samples or taking into account
reorganization of asphaltenes from different fluids, will help to define the severity of the risk. For mitigation, a test set-up has
been developed: it allows evaluating the efficiency of chemical additives to prevent plugging under flow conditions of fluids
above the asphaltene precipitation threshold. Depending on the crude oil, the severity of the precipitation conditions, and the
nature of the additive, the blocking of the capillary tube can be delayed or prevented.

Introduction
The understanding and the prediction of asphaltene precipitation are an important topic in petroleum industry. Reliable
evaluation of the asphaltene stability requires representative samples and measurement using special high pressure
equipments. Moreover, important development projects may involve many reservoirs with many different fluids. Even inside
of a connected reservoir, the quality of the oil and the asphaltene can vary through a large scale, and the investigation of each
fluid in their representative conditions become very expensive and often impossible. Fast screening methods are then
required to discard the low risk cases in order to concentrate the investigations on the high risk cases.
Many fast screening methods have been proposed so far. The De Boer’s diagram is one of the most useful [1], [2]. However,
it only takes into account the properties of the hydrocarbon phase without any investigation on the asphaltene fraction. Thus,
this method gives mostly pessimistic prediction of the risk of asphaltene precipitation. If many other screening methods have
been proposed, most of them have the same drawback, as they only take into account the composition of the hydrocarbon
phase and the concentration of asphaltenes without any investigation on the actual solubility class of asphaltenes in the crude.
Knowing the solubility class of the asphaltenes is one of the two most important properties in order to accurately predict the
risk linked with deposition of asphaltenes. The composition of the hydrocarbon phase gives insight on the solubilization
power of the oil, the other important property of the system. Only taking into account the percentage of asphaltenes, without
considering their solubility class, consider the asphaltene fraction in an irrelevant way, and it may lead to erroneous
predictions.
2 SPE 164184

In addition, the mechanisms of asphaltene precipitation are not always well understood. Thus, it is not uncommon to see
misdiagnosis when solid deposits are found: asphaltene deposition is diagnosed when it is simply mineral deposits or other
organic deposits containing evaporated oil residue; pressure effect is diagnosed while compatibility problem can occur;
asphaltene precipitation considered as impossible while it can occur through a tricky mechanism etc. Thus, an asphaltene
characterization method which can be used as a tool for diagnostics is very useful.
The method “ASIST” proposed by Buckley & al. [3], [4] takes into account implicitly the solubility class of the asphaltene
fraction and gives pretty good prediction of the asphaltene instability of the live oil using measurements performed on dead
oil samples. However, this method requires the use of a specific apparatus and does not measure explicitly the solubility class
of the asphaltenes fraction. Our approach is to use directly a relevant solubility property of the asphaltene fraction instead of
using complex models and chemical analyses for the understanding of the driving force of asphaltene precipitation and for
the risk evaluation. As will be explained latter in the experimental section, the method is based on the fact that the stability of
the asphaltene fraction in oil or in organic solvent depends strongly on the quality of the solvent (i.e. its composition) or of
the oil (i.e. mainly its density above the bubble pressure and its average molecular weight) and is almost independent of the
dilution. Consequently, it is difficult to describe the asphaltene stability in term of “solubility” which is expressed in weight
fraction or in mole fraction. The term of solubility class is more appropriate.
According to this solubility property, we propose an easy characterization method called ASCI rating (for Asphaltene
Solubility Class Index). The procedure for the determination of ASCI is described in the experimental section. This rating
method is applicable on an oil sample, on a residue of distillation as well as on a deposit sample. In the last case, the solid
sample needs to be re-dissolved in a small quantity of solvent prior to the ASCI rating. For asphaltene rich oils, the sample
can be diluted by toluene before measurement. Based on this rating method, a new and easy way to perform fast screening of
the asphaltene instability is proposed in this work. Using some PVT properties of the live-oil, this method leads us to limit
the investigation to the fluids which present a real risk of asphaltene precipitation. The asphaltene characterization can be
done using dead oil samples. Representative samples are required only for advanced investigation once the fluid is assessed
as risky from the point of view of asphaltene stability.
A second solubility property of the asphaltene fraction is important to be mentioned since it is important for the diagnostics
when a precipitate is discovered in a production line. In spite of the insensitivity to dilution of the asphaltene stability, when
the precipitation onset is reached, asphaltene precipitate progressively. This partial precipitation is not linked to the
“solubility” of the whole asphaltene fraction, but to the distribution of different asphaltenes with different solubility class
inside of the same oil. In addition, a strong interaction exists between the different asphaltenes species: even at low
concentration, some unstable asphaltenes can become stable because of the presence of stable asphaltenes. As a consequence,
when asphaltenes contained in a crude oil are fractionated by partial precipitation, the ASCI of the precipitated fraction
should be significantly lower than the initial ASCI of the oil. The importance of fractionation of asphaltenes with different
solubilities can be seen not only on deposition issues, but also on the behavior of oil / water interfaces [5], [11].
These intriguing properties can be used to analyze the phase behaviors of the asphaltenes in order to make differences
between the asphaltenes enrichment by phase separation such as precipitation or liquid - liquid separation, and the enrichment
by other mechanisms such as segregation or gas striping. In the case of asphaltene enrichment by gas striping, the ASCI of
the oil should not be modified since there is no asphaltene fractionation. In the case of gravity segregation, a continuous shift
of ASCI can be observed versus depth and no difference should be observed on term of ASCI rating between the core extract
and the oil sample from the same depth. In the case of asphaltene precipitation, a strong difference should be observed
between the ASCI of the dissolved precipitate and the ASCI of the oil samples.
When a risk of precipitation linked to asphaltenes is predicted, two types of action can be taken. The first type is to perfom
more complete PVT studies in order to determine if the risk that was predicted with the fast screening method will indeed
result in possible precipitation of asphaltenes. The second one is to look at possible chemicals in order to mitigate the impact
of the risk linked with asphaltenes. From the chemical additive standpoint, there are two kinds of chemicals that can be
provided. The chemicals are said to either play on the asphaltene precipitation threshold or to play on the agglomeration of
the asphaltene precipitates. By changing the agglomeration properties, it seems possible to prevent them to stick together and
the precipitates are transported without plugging either the well bore or the pipes. In order to test these additives, it would
also be very interesting to be able to test the live fluids [6], but it is very resource and time consuming. As a result, capillary
plugging tests have been developed [8], [9] in the light of what is done for mineral scales for water compatibilities studies
with blocking tests [10].
The following sections give an experimental description of how the measurement is performed, as well as examples on how it
can be practically used in order to assess either a deposition problem or to focus on the most relevant fluids for a field
development. Finally, a presentation of the asphaltene capillary test is presented.
SPE 164184 3

Experimental section: Determination of the Asphaltene Solubility Class Index (ASCI)

One of the specific characteristics of stability of asphaltenes is its strong sensitivity to the quality of the solvent and its very
low sensitivity to dilution. For example, if a given quantity of an asphaltene fraction flocculates in a given ratio of a mixture
of toluene and n-heptane, these asphaltenes will still flocculate even if we dilute with 10 or 100 volumes of the same heptol
mixture. But if it is soluble in this mixture at a concentration of 0.1% wt, it will remain soluble in the same mixture at 1%wt.
On the other hand, only a very weak modification of the ratio toluene/n-heptane can modify in a spectacular way the
solubility of an asphaltene fraction. Flocculation can be induced by adding a few grams of n-heptane in one litre of toluene /
n-heptane mixture containing dissolved asphaltenes.
To describe the behaviour of such a petroleum fraction, it is not really convenient to use the word "solubility" which
generally indicates the maximum quantity of a component that can be dissolved in a solvent, and it is not really possible to
link such a behaviour to traditional "solubility equilibrium" and "solubility constant", as the solubility parameter of the
solvent is a much better parameter than the concentration in solution. So, a more appropriate description of the ability of an
asphaltene fraction to remain soluble should be its solubility class. We can characterize the behaviour of an asphaltene
fraction by a kind of "Asphaltene Solubility Class Index" (ASCI).
To measure this index of an asphaltene fraction, we add a few drops of a crude oil, or a solution of asphaltenes, in standard
solvent mixtures as described in Table 1. The quantity of the oil, or asphaltene solution, added must be insignificant
comparing to the quantity of the standard solutions (usually <1% wt).
Table 1 Solvent mixtures for ASCI measurement

Solution n° n°0 n°1 n°2 … … n°18 n°19 n°20

Toluene 100%wt 95%wt 90%wt … … 10%wt 5%wt 0%wt
n-heptane 0%wt 5%wt 10%wt … … 90%wt 95%wt 100%wt
ASCI
0 1 2 … … 18 19 20
(n-heptane %/5)

These solutions are then stirred and stored at 50°C for about 48 hours before observation. If the asphaltene precipitation starts
in the pure toluene, the "asphaltene" fraction obtains an index equal to 0 (0% heptane). In case of the “asphaltene” fraction
precipitates only in pure n-heptane, it gets an index equal to 20 (100% heptane). If the solution k shows a precipitate but the
asphaltene fraction is soluble in the solution k-1, it gets an index equal to k.
Contrary to other methods used to qualify solubilities of asphaltenes, the ASCI procedure, with long enough times and high
dilution ratio, tries to define a thermodynamic solubility, and to avoid kinetic effects.
From our experience, the concentration of asphaltenes in the oil has little incidence on the solubility class index measured
using this method as long as the minimal by-pass ratio (one oil mass for more than 20 masses of standard mixture) is
respected. For crude oils having a high level of sediment, a good way to detect the precipitation point, without being tricked
by the presence of these sediments, is to remember that the fraction of asphaltenes precipitated should increase when the level
of heptane, i.e. the ASCI note of the solvent, increases.
Fig. 1 illustrate the insensitivity of the ASCI note, hence the asphaltene precipitation threshold, to dilution. An oil containing
about 3%wt of asphaltene as measured by standard ASTM method is diluted in toluene at three concentrations going from 2.5
%wt to 0.1%wt. It represents between about 750 ppm and 30 ppm of asphaltenes. The ASCI note of these model systems is
determined, as previously explained, by adding a few drops of the solutions to the heptol mixtures. Whatever the
concentration of asphaltene, precipitation is never seen for ASCI=12 (60% heptane), and is always seen for ASCI=13 (65%
heptane). It is also possible to see in Fig. 1 that the amount of precipitated asphaltene increases with the heptane/toluene ratio
going from ASCI=13 (65% Heptane) to ASCI=15 (75% heptane).
This Total in-house method allows comparison between asphaltene fractions, independently of their solvent media. The
higher the ASCI, the more stable the asphaltene fraction, as it requires more precipitating solvent to induce phase separation.
For a given hydrocarbon solvent, the solubilization of an asphaltene fraction implies that this solvent allows the solubilization
of all the fractions having a higher solubility class index. The precipitation of a fraction in a given solvent implies the
inability of this solvent to dissolve all the asphaltene fractions having a lower solubility class index.
The solubility class of an asphaltene is little affected by its concentration in the oil. However, it can be strongly affected if
another asphaltene fraction is added or if it is fractionated by a partial precipitation. After a partial precipitation, the
precipitated fraction, once redissolved and noted, will get a lower index. That is why if asphaltene deposits is found in the
production equipments, these deposits will show an ASCI much lower than the ASCI found for the asphaltene fraction in the
oil. As it is implicitly said in the examples of asphaltenes having an ASCI note of 0 (0% heptane) or 20 (100% heptane), it is
possible to find asphaltenes being soluble in heptane, and asphaltenes being insoluble in toluene, in contradiction to the strict
"handbook" definition.
4 SPE 164184

Fig. 1 : ASCI note for 3 solutions of the same asphaltene at 3 different concentrations going for 750 ppm to 30 ppm
12 (60% Heptane) 13 (65% Heptane) 14 (70% Heptane) 15 (75% Heptane)

2.5% Oil in Toluene

(~750 ppm asphaltenes)

0.5% Oil in Toluene

(~150 ppm asphaltenes)

0.1% Oil in Toluene

(~30 ppm asphaltenes)

Application of the method

Predictive studies during field development phase : A fast screening method for the evaluation of the risk of
asphaltene precipitation due to pressure drawdown
As said in the introduction, measuring the ACSI only gives us the solubility characteristic of the asphaltene fraction. To
evaluate the stability limit of asphaltenes in given oils, this characteristic must be compared with the solubilization power of
the oil in the considered conditions.
The stability of an asphaltene fraction with a given solubility class in an oil or in a solvent mixture will depends mainly on
the molecular volume and on the density of the oil or of the solvent, and it is rather independent on the concentration of the
asphaltenes. For oils with similar molecular volume, the higher the density of the oil, the higher its capability to dissolve
asphaltenes. When the density is similar for two oils, the oil with smaller average molecular volume will have higher
capability to dissolve asphaltenes. The asphaltene stability depends also slightly on the temperature. Generally, most of
authors found that at constant density of the oil, an increase of the temperature will increase slightly the asphaltene stability.
In Fig. 2, the average molecular weight of reservoir fluids from our fluid database is plotted against the density of the oil at
reservoir conditions. For confidentiality purpose, values of the densities are not provided. We can see that the two parameters
are roughly correlated for the reservoir fluids found in our fluid data base, Thus, we can consider the stability of the
asphaltene fraction with a given solubility class as mainly density dependent. The ASCI of the asphaltenes is measured for
each of these fluids. In Fig. 3, the ASCI value is plotted against the density of the oil at reservoir pressure. In this figure, the
higher the density of the fluid and the ASCI, the more stable the asphaltene fraction in the oil. If an asphaltene fraction is
soluble in an oil sample, a higher ASCI asphaltene will be soluble in the same oil or in any oils with the same or higher
density. Therefore, the fluids potentially instable to be considered in the risk evaluation are all located in the left-lower border
of the graph (as indicated by the black bold line) : no fluid is found in this area, because the asphaltene fraction would not
have been soluble in the corresponding fluid. Consequently, this borderline is considered as the solubility limit – an
asphaltene fraction with given ASCI is soluble in a fluid with given density only if the couple is situated at the upper-right
side of the line.

This fast screening method allows us to focus our investigation on the high risk cases only. However, corrections need to be
done in case of high concentration of non hydrocarbon compounds.
SPE 164184 5

250 20 100

230 18 90

210 16 80

Heptane in Heptane+Tolune, %
190 14 70
Molecular weight, g/mol

170 12 60

ASCI
150 10 50

130 8 40

110 6 30

90 4 20

70 2 10

50 0 0
Density @ reservoir conditions Density @ reservoir conditions

Fig. 2 : Oil Molecular Weight vs density at reservoir conditions Fig. 3 : ASCI vs density at reservoir conditions

Flow assurance assessment on field deposits : Are asphaltenes really responsible for the deposit ?
When a field deposit is found, asphaltenes are often thought to be the cause of the problem, and mitigation strategies are
looked at while the deposit is sent for more complete analysis. Usually, what triggers such a fast operational response is that,
when performing "classical" characterizations of the deposit, people find asphaltenes, and associate them to the problem.
Sometimes, the mitigation strategies taken to fight "asphaltene deposit" can turn out to be successful even if asphaltenes are
not at all responsible for it. But, it is also very common not to solve anything, or worse to increase the issues.
As a matter of fact, if there is oil in a deposit, asphaltenes of this oil will be detected in the deposit, whether they are or not
the cause of the deposit, and it is usual to take much more attention to the amount of asphaltenes rather than to their solubility
or the solvency of the oil. People will use parameters such as the spot test or the CII, Colloidal Instability Index, which is
defined as in equation 1 to get insight on the deposit.
% %
Equation 1 CII
% %

With these indications, extra heavy oils will generally be suspected to have issues related to asphaltenes, whereas, as a
contrary which can be illustrated through the De Boer's plot or in Fig. 3, they do have a lot of asphaltenes with a low
solubility class because they can dissolve them.
We received samples of deposit from an extra heavy oil field, for which the service company had diagnosed an asphaltene
related problem, and a sample of the oil produced on the same well. As the CII of the oil was 1.5 (considered as "critical"
risk), the deposit was thought to be an asphaltene deposit (Table 2). The ASCI of the oil was measured, and the deposit was
dissolved in toluene then noted in the ASCI procedure (Table 3). For both samples, the ASCI was 11 (55% heptane in heptol
to induce precipitation). This ASCI is well above the limit ASCI of asphaltenes that such an oil can solubilize. The deposit
was not at all coming from asphaltene deposition, but was linked to the size and the amount of solids produced in this well.
The mitigation strategies were thus changed, and more efficient solutions were implemented to fix the productivity issue.
Table 2 Data on EHO 1 Table 3 ASCI of EHO 1 and
deposit
Sample nC5 Insoluble °API Density (kg/m3) Saturated Aromatics Resins Asphaltenes CII Sample ASCI
EHO 1 13 8.5 1010.5 47.7 24.7 12.8 9.8 1.5
EHO 1 11
Deposit from well
producing EHO 1 11

Flow assurance: Selection of additives

If a risk of asphaltene deposits has been indentified, two types of action are to be taken. The first type is to perform more in
depth PVT-studies in order to better characterize the risk. This kind of studies requires having live oil samples, or
recombined oil samples, and they are also quite lengthy. The second type of action is to use a capillary plugging test in order
to be able to assess if additives, and eventually which additives, are able to prevent flow assurance issues. In this test, the
increase of the pressure drop is measured over time in a capillary tube in which a blend of the crude oil to study, a
precipitating light alcane, and an additive are flown together. The pressure drop P is related to the flow rate Q though the
Hagen-Poisseuille law:
Equation 2 ∆P LQ
Where R and L, are, respectively, the radius and the length of the capillary and n is the fluid viscosity.
6 SPE 164184

The crude oil is put in contact with a paraffinic solvent (heptane) in order to precipitate asphaltenes in the presence or not of
additives. As a consequence of the formation of an asphaltene deposit, R decreases which produce an increase in P.
As a reference, a non precipitating solvent (toluene) is also injected with the crude oil before the paraffinic solvent to
establish the pressure drop base line without any deposition. Following the heptanes co-injection, toluene is also used to clean
and unplug the capillary by dissolving precipitates of asphaltenes. Crude oil and solvents, heptane or toluene, are injected
using three PHD Ultra 4400 syringe pumps supplied by Harvard Apparatus. A fourth pump can be used to inject a dilution of
additive in heptane in order to prevent plugging. Through this set-up, the dosage of additive can either be fixed at a constant
concentration, or varied over time, for example decreased, in order to have a first evaluation of the optimal dosage. The
experimental set-up is schematized in Fig. 4.
Fig. 4 : Asphaltene capillary precipitation test set-up

Oven
Pump with
Pressure
Crude Oil
Transducer
Pump with
Toluene
Pump with
Heptane
Capillary Tube
Pump with
Heptane & Static Mixer
Additive

In order to perform an additive study, it is first necessary to determine test conditions, in particular the crude oil / solvent
ratio and the global throughput. For that matter, the precipitation onset of the oil is determined by adding increasing volume
of heptane to a volume of crude oil, by waiting 24 hours, and by a visual determination of the ratio which has led to
asphaltene precipitation, as illustrated in Fig. 5. Fig. 5 also illustrate the complex interplay between the amount of
asphaltenes, their ASCI classification, and the solvency power of the oil : even if the three oils were identified as presenting a
risk of asphaltene precipitation, it can be seen that crude oil A, which could be initially considered as the "worse" oil with
more asphaltenes of an overall lower quality (lower ASCI), has an onset precipitation threshold above crude oil B (i.e. more
precipitant is require to initiate asphaltene precipitation), and crude oil B has the same onset as crude oil C with three times as
much asphaltenes, determined by standard procedure, and a much lower ASCI (9 vs 12).
Fig. 5 : Determination of Asphaltene precipitation onset

Crude Oil A (10% Asphaltene, ASCI=11) : Onset = 1 Crude Oil B (5% Asphaltene, ASCI=12) : Onset = 0.75
SPE 164184 7

Crude Oil C (17% Asphaltene, ASCI=9) : Onset = 0.75

Of course, the residence time of the solution in the capillary, even at the low throughput used, is much shorter than the time
used for measuring the precipitation onset, but it is a good starting point for the capillary test.
The first step for running an additive study in the capillary test is to determine what is the pressure drop versus time for the
crude oil blended with heptane without additive : the global throughput and the heptane / oil ratio are selected in order for the
plugging of the capillary to take a few hours. In the case of crude oil A, the diameter of the capillary is 0.5 mm, the heptane /
oil ratio is set as 1.5 (see Fig. 5), and the oil throughput is 0.1 ml/min. Fig. 6 shows the pressure increase over time, as well
as the flowrates for the blank test without additives. During the first 4 hours, toluene is injected with the crude oil at a ratio of
1.5, and there is no sign of pressure increase. After 4 hours, the injection of toluene is stopped, and the injection of heptane is
started : after 2 hours, the pressure begins to increase, and reaches the "target" pressure of 8 bars after 8.5 hours. At that
point, the injection of solvent is stopped, and the pressure relaxes in the capillary.
Fig. 6 : Capillary pressure build up for Crude A

100 10

80 8
Pressure (Bar)
Volume (ml)

60 6
Crude Oil
Toluene
40 4
Heptane

20 2 Pressure

0 0
0 4 8 12 16 20
Hours (h)

The tests are then performed with anti-asphaltenes additives in order to rank their performance as illustrated is Fig. 7 : in
these tests, 2 000 ppm of anti-asphaltenes vs crude oil are used. It can clearly be seen that some additives (AA1 to AA3) do
not change the plugging kinetics, while others (AA4 to AA6) helps to prevent plugging of the capillary. The efficiency of the
additives is very much related to their dosage : for example, at 1 000 ppm of AA4, the plugging kinetics is as fast as when no
additive is introduced.
As scanning the different concentration in order to find the efficient conditions for preventing plugging, another way to use
this test set-up is to scan through several additive concentrations by decreasing them over time, as it will be illustrated with
crude oil B.
But, the first point to mention is the definition of the plugging conditions without additives with that oil. As illustrated in Fig.
5, the test initially started with an heptane / oil ratio of 0.8 and a capillary radius of 0.5 mm but no plugging occurred.
Through several steps, the heptane / oil ratio was increased whereas the capillary radius was decreased up to the point it was
finally possible to plug the capillary with an heptane / oil ratio of 3 and a capillary of 0.38 mm. Thus, plugging occurred for
much more severe conditions as far as asphaltene precipitation than for crude oil A, whereas the static asphaltene
precipitation onser was lower for crude oil B. It is also to note that through the difference of initial asphaltene ratio and
8 SPE 164184

solvent / oil ratio, there is 4 times less asphaltene passing through the capillary for crude oil B conditions than for crude oil A,
but the real parameter, albeit difficult to follow, is the amount of precipitating asphaltenes in the test conditions. With a
proper analysis of the field conditions, it is to hope that it will be possible to make a link between the PVT conditions, for
which the appearance of precipitates is observed, and a given heptane / oil ratio for running the capillary test: this would
allow to determine if the precipitating conditions would cause plugging or only the transport of precipitates in the pipe.
Fig. 7 : Capillary pressure build up for Crude A – Fig. 8 : Capillary pressure build up for Crude B –
constant additive concentration variable additive concentration

Ratio Heptane/Crude Oil A (10% Asp ASCI=10) = 1.5

8

2000 ppm
No additive
6
AA1
Pressure (bar)

AA2
AA3
4
AA4
AA5
AA6
2

0
0 2 4 6 8 10
Time from heptane injection (h)

With the defined conditions, the capillary test is run with additive concentrations decreasing from 10 000 ppm to 300 ppm
every 3.5 hours, or about the time needed for plugging of the capillary without additive (Remark : the label of the additives
are different between Fig. 7 and Fig. 8 because not all the same additives have been used in both studies). Fig. 8 shows that :
 2 additives have the same plugging speed than without additive
 For 3 additives, plugging occurs when the additive concentration is decreased from 10 000 ppm to 3 000 ppm
 For 1 addive, plugging occurs when only 1 000 ppm of additive is used
 For the last one, there are signs of partial plugging beginning at 3 000 ppm, and 1 000 ppm, but complete plugging
only occurs with 300 ppm
Even if complete plugging only occurs at 300 ppm with additive A7, additive A6 seemed like a better choice for showing
absolutely no sign of pressure increase for a longer time period.
As explained in the introduction, some additives are said to have an impact on the agglomeration of the asphaltene
precipitated particles whereas others should play on the precipitation onset. The test protocols that are shown above are
performed above the asphaltene precipitation threshold of the crude oil : it may explain why some additives do not seem to
show any improvement over the reference system. A third way to run the capillary precipitation test could be to increase the
heptane / oil ratio over time for a fixed additive concentration, either introduced in the oil or the crude oil, in order to
demonstrate differences in precipitation thresholds.
Conclusions
A universal, phased approach to the prediction, verification, and treatment of asphaltene deposits has been described.
By defining a simple characterization procedure of the solubility class of asphaltenes at very high dilution, it is possible to
efficiently determine whether asphaltenes are or will be responsible for production offsets.
If initial characterization indicates a high likelihood of asphaltene deposition, a high-pressure test setup can facilitate
confirmation, as well as evaluate remediation options for the treatment of these deposits under flow conditions. Using a
dynamic capillary asphaltene deposition test can help to select additives in order to remediate the issues.

Acknowledgement
The authors would like to Total for allowing publishing this research. They would also like to thank their colleagues
Christian Hurtevent, and Benjamin Brocart for their contributions to these studies.

References
[1] : S. Verdier, Experimental study and modelling of asphaltene precipitation caused by gas injection, PhD thesis, Technical University of
Denmark, 2006.
[2] : Boer, R.B.d., K. Leerlooyer, M.R.P. Eigner, A.R.D. van Bergen, SPE 24987 : "Screening of Crude Oils for Asphalt Precipitation:
Theory, Practice, and the Selection of Inhibitors", 1995
SPE 164184 9

[3] : J. X. Wang, J. S. Buckley, SPE 64994, An Experimental Approach to Prediction of Asphaltene Flocculation, 2001
[4] : Jill S. Buckley, Jianxin Wang, Jefferson L. Creek, Solubility of the Least-Soluble Asphaltenes, 2007, pp 401-437 in "Asphaltenes,
Heavy Oils, and Petroleomics", Ed Mullins, O.C., Sheu, E.Y., Hammami, A., Marshall, A.G.
[5] : J. D. McLean, P. K. Kilpatrick, Effects of Asphaltene Solvency on Stability of Water-in-Crude-Oil Emulsions, Journal of Colloid and
Interface Science, V 189, I 2, 1997, pp 242-253
[6] : J. D. McLean, P. K. Kilpatrick, Effects of Asphaltene Solvency on Stability of Water-in-Crude-Oil Emulsions, Journal of Colloid and
Interface Science, V 189, I 2, 1997, pp 242-253
[7] : D. Abdallah, SPE162190, Impact of Asphaltenes Deposition on Completion Design for CO2 Pilot in an Onshore Abu Dhabi Field
[8] : J.X., Wang, J.S. Buckley, J.L. Creek, Asphaltene Deposition on Metallic Surfaces, J. Dispersion Science & Technology, 2004, 25,
287-298
[9] : A.S. Kurup, J. Buckley, J. Wang, H. J. Subramani, J.L. Creek, W.G. Chapman, Asphaltene Deposition Tool: Field Case Application
Protocol, SPE 23347
[10] : B. Bazin, N. Kohler, A. Zaitoun, Some Insights Into the Tube-Blocking-Test Method To Evaluate the Efficiency of Mineral Scale
Inhibitors, SPE96560
[11] : M. Rondon, J. C. Pereira, P. Bouriat, A. Graciaa, J. Lachaise, J.-L. Salager, Breaking of Water-in-Crude-Oil Emulsions. 2. Influence
of Asphaltene Concentration and Diluent Nature on Demulsifier Action, Energy & Fuels, 2008, 22 (2), pp 702–707