pubs.acs.

org/EF Article

Evaluation of Asphaltene Stability of a Wide Range of Mexican

Crude Oils
Roque Guzmań , Silvano Rodríguez, Pablo Torres-Mancera, and Jorge Ancheyta*

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ABSTRACT: Appropriate prediction of asphaltene stability can anticipate operational problems such as plugging of lines and
process equipment (pumps, heat exchangers, separation tanks, among others), thus assuring the production, processing,
transportation, and storage of petroleum. In the present study, the physical and chemical properties of a series of Mexican crude oils
with American Petroleum Institute (API) gravity ranging from 10 to 52 were determined. Based on saturate, aromatic, resin and
asphaltene (SARA) analysis, the following indexes were calculated: colloidal instability index, colloidal stability index, Stankiewicz
stability criterion, stability cross plot, and oil compatibility model. The stability of crude oils was also evaluated by means of
experimental techniques such as spot test, S-value, and static stability test column. No uniform results were obtained when
determining the stability of crude oils with different methodologies. Due to the discrepancies disclosed, it is recommended to
evaluate stability by various methodologies to adequately predict the stability of asphaltenes in crude oils. Hence, the stability of
asphaltenes in a given crude oil may be ascribed based on the average result. However, from a practical point of view, pertinent
cautions on the handling of samples must be observed if at least one of the methods classifies the sample as unstable or metastable.

1. INTRODUCTION aromaticity and polycondensation of aromatics, as well as the

Asphaltenes are the heaviest and most polar fractions of crude solubility of asphaltenes in resins.12−16
oils. They are compounds insoluble in linear low-molecular- Complications related to the stability of asphaltenes may
weight alkanes, such as n-pentane (n-C5), n-hexane (n-C6), or appear throughout the production chain. In the upstream
n-heptane (n-C7) but soluble in aromatic solvents such as sector, it starts at the well where oil recovery can be reduced
toluene, benzene, xylene, or pyridine.1−3 Some crude oils due to changes in reservoir wettability, clogging of rock pores
contain high concentrations of asphaltenes depending on their by deposition of asphaltenes, and the formation and
nature and origin, which may exhibit stability problems under strengthening of oil−water emulsions. In midstream oper-
certain conditions of pressure, temperature, or flow regime that ations, during storage, blending, and transportation of crude
in turn cause difficulties during transportation and storage.4−7 oils that may result in damage of pipelines and pumping
Typically, asphaltene content increases as the crude oil equipment. Finally, in downstream where crude oil is refined,
becomes heavier, i.e., the lower the American Petroleum since instability of asphaltenes may lead to coking, fouling, and
Institute (API) gravity, the higher the asphaltenes content. deactivation of the catalysts used in the different refining
Paradoxically, the precipitation of asphaltenes is often observed processes.8,16
in light crude oils that have a low content of them, which is due Despite the fact that crude oils own a complex composition,
to the presence of high amounts of linear alkanes of low compounds in crude oils can be grouped into four main
molecular weight in which asphaltenes show limited solubility. fractions designated as SARA: saturated, aromatic, resin, and
In contrast, heavy crude oils contain large amounts of asphaltenes. Regarding their capacity to keep asphaltene in a
intermediate-molecular-weight components that keep asphal- solubilized state, saturated compounds are considered non-
tenes in a peptized state,8,9 yielding less stability issues in heavy solvent, while resins and aromatics are solvents. According to
crude oils despite being generally rich in asphaltenes. the micellar theory, in stable crude oils, asphaltenes are
Asphaltenes show a natural tendency toward aggregation, associated with resins within a stable equilibrium of solubility.
which potentially may produce its separation from crude oil The imbalance of the colloidal structure favors the separation
and their buildup as a solid phase. The phenomenon consists of the phases, causing instability in the medium that in many
of flocculation/precipitation followed by sedimentation; for
this reason, asphaltenes are considered the main precursors of
sediment formation.10,11 Asphaltene stability of crude oils also Received: September 30, 2020
represents complications during refining. An important Revised: December 3, 2020
concern when processing heavy crude oils by catalytic Published: December 24, 2020
hydrotreating/hydrocracking is sediment formation. It has
been reported that during hydrotreating, the most important
factors responsible for the generation of sediments are

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Table 1. Properties of Crude Oils

property C52 C37 C34 C32 C29 C24 C16 C10
API gravity 51.62 37.19 33.65 32.88 29.41 24.69 16.05 9.60
kinematic viscosity, cSt @ 25.0 °C 1.47 5.06 16.28 12.651 24.17 116.52 3293 104 027
sulfur, wt % 0.140 0.931 1.099 2.299 2.252 2.469 4.666 4.540
characterization factor, KUOP 12.23 12.02 12.11 11.96 11.94 11.93 11.63 11.40
acidity, mg KOH/g 0.09 0.47 0.39 0.20 0.27 0.16 0.25 3.61
n-C7 insoluble, wt % 0.95 0.95 1.94 2.96 3.05 3.21 4.05 6.51
nickel, ppm 0.30 3.54 17.03 16.99 24.60 46.62 85.43 89.61
vanadium, ppm 0.25 16.75 23.60 66.02 85.78 131.65 369.11 442.63

Figure 1. Fractionation of the crude oil into its different components.9,10

cases leads to the precipitation of asphaltenes.12,17 Accordingly, the proportion of heavy and extra heavy crude oils. For these
stability is defined as the property of an oil to keep its reasons, the characterization of different types of crude oils and
asphaltenes in a peptized state, thus avoiding their precip- their influence on the stability of asphaltenes become an
itation and flocculation.18 important issue. Furthermore, since the blending of crude oils
Various parameters must be taken into account during the is a common practice to adjust crude oil specifications for sale
processing, transportation, and storage of petroleum. The or transportation purposes, the compatibility of crude oils also
following are the most important ones: becomes a pivotal task.
• Viscosity indicates the relative mobility of crude oils. In the present research, the stability of different crude oils
• Insoluble in n-C7 reflects the presence of heavy and polar with API gravity ranging from 10 to 52 is determined by both
hydrocarbons. theoretical and experimental methodologies. Theoretical tools
• Conradson carbon content correlates with the tendency are based on computing several indexes based on SARA
to coke formation. analysis, while experimental methods encompass spot test,
• Acidity is an indication of the corrosive properties of static column, and optical detection of the asphaltene
crude oils. precipitation onset. Additionally, the model of the compati-
• Water, salt, and sediment content cause uneven bility of oils is applied to selected blends. The aim of the
distillation behavior, causing blockage and fouling of present work is to compare various methodologies in the
heat exchangers and lead to corrosion. evaluation of crude oil stability toward the precipitation of
• Paraffin content, type of paraffin, crystallization point, asphaltenes. Based on a proper prediction of asphaltene
gel point, and pour point are important factors for the stability, operational problems such as plugging of lines and
deposition of waxes during treatment and storage. process equipment can be anticipated, thus contributing to
Temperature is also important, since it affects some production assurance, processing, transportation, and storage
properties, especially those related to mobility (density and of petroleum.
viscosity). In accordance, the most convenient crude oils to
refine are those with adequate mobility properties and the 2. EXPERIMENTAL SECTION
lowest content of impurities, which are characteristics of light Crude oils employed in the experimental study were recovered from
and super light crude oils. However, the trend in crude oil different production regions in Mexico and they encompass heavy,
production, not only in Mexico but also in other countries light, and super light crude oils. They were labeled as C52, C37, C34,
(Venezuela, Canada, Russia, etc.), corresponds to the shrinking C32, C29, C24, C16, and C10, where the numbers indicate the
of these types of crude oils with the subsequent increment in approximate API gravity of the crude oil.

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2.1. Characterization of Crude Oils. The physical and chemical 2.3. Evaluation of the Stability of Selected Crude Oils by
properties of crude oils were determined by several standardized Indexes and Methods Based on SARA Analysis. 2.3.1. Colloidal
methods: API gravity by means of an ASTM D1298 method, Instability Index (CII). Asphaltenes and saturates are considered as
kinematic viscosity at 25 °C by an ASTM D445 method, sulfur compounds that promote asphaltene flocculation, while aromatics and
content by ASTM D4294, salt content by ASTM D3230, asphaltene resins work as peptizing agents, thus favoring the stability of
content measured as n-heptane insoluble by ASTM D3279, nickel and asphaltenes. Accordingly, the colloidal instability index (CII) is
vanadium content by ASTM D5863, characterization factor KUOP by a defined as the quotient between the sum of asphaltenes and saturates
UOP 375 method, and total acid number by ASTM D-664. The and the sum of aromatics and resins.20−22
results are presented in Table 1. (% asphaltenes) + (% saturates)
The spot test by ASTM D4740 was also used for qualitative CII =
determination of the stability of crude oils. A static column was (% resins) + (% aromatics) (1)
implemented to have a quantitative value of the stability of crude oils. The lower the CII value, the greater the stability of asphaltenes in the
The column was composed of two concentric tubes, in which the medium; therefore, the stability determined is relative and allows for
internal tube (110 cm length, 3.8 cm internal diameter) contained the evaluating whether one oil is more or less stable in relation to another.
oil sample, and the external tube contained the heating liquid Asomaning and Watkinson21 evaluated the stability of oils from the
(ethylene glycol) to keep to oil sample at the required temperature, SARA analysis determined by liquid chromatography and demon-
35 °C in this case. A total of 1.25 L can be loaded to the column. The strated experimentally that when CII ≥ 0.9, asphaltenes are unstable
column had three sampling points located at the bottom, middle (1/3 in the medium, when 0.7 ≤ CII ≤ 0.9, there is uncertainty about
length), and top (2/3 length). With the static column, crude oil stability, and if CII <0.7, asphaltenes are stable in oil.
properties during storage were analyzed at two moments of time; just 2.3.2. Colloidal Stability Index (CSI). This index considers that the
after being introduced in the column and after a certain time of asphaltenes of unstable crude oils are more polar than those of stable
storage (7 days). The basic idea of the static column is to detect to crude oils and takes into account both the SARA analysis and the
what extent the value of a chosen property is preserved during sample polarity of the components of crude oils based on the following
storage. In accordance, a crude oil whose chosen property is unaltered equation23
during the storage period is considered highly stable. On the contrary,
if the value of a given property changes considerably after a period of (ε asph)(% asphaltenes) + (ε sat)(% saturates)
CSI =
storage, the crude oil is unstable, since the change of such a property (ε res)(% resins) + (ε arom)(% aromatics) (2)
is likely the result of asphaltene segregation.
2.2. SARA Fractionation of Crude Oils. Separation of where the values of the dielectric constant (ε) of the SARA fractions
petroleum and residue components is based largely on their solubility are
properties in different solvents. For instance, Figure 1 shows the εasf = 18.4 and εres = 3.8 for unstable crude oils; εasp = 5.5 and εres =
fractionation of oil using first n-heptane, which generates two 4.7 for stable crude oils; and εsat = 1.921 and εarom = 2.379 for all of
fractions, the insoluble one corresponding to asphaltenes and the the crude oils.23
soluble one corresponding to maltenes.19 Subsequently, by toluene If CSI > 0.95, the crude oil is unstable (asphaltene precipitation will
addition to asphaltenes, two more fractions are obtained, one that occur).
corresponds properly to asphaltenes (soluble fraction) and the second If CSI < 0.95, the crude oil is stable and the risk of asphaltene
one that represents carbenes and carboids (insoluble fraction). The precipitation is minimal.21
insoluble fraction is finally separated using carbon disulfide to obtain 2.3.3. Stability Index (SI). The asphaltenes/resins (A/R) ratio is
carbenes (soluble) and carboids (insoluble). Both carbenes and popular and widely used because asphaltenes and resins form the
carboids are considered coke precursors due to their large number of nonvolatile part of petroleum and are therefore accurately measured.
This relationship makes sense, since resins are the natural peptizers of
condensed structures. Finally, the fraction soluble in n-heptane
petroleum and keep asphaltenes in solution. Asomaning and
(maltenes) is further separated by passing through a chromatographic
Watkinson21 reported that if the A/R ratio is lower than 0.35, the
column packed with alumina; several fractions are obtained using
crude oil will be stable.
different solvents as eluents. Thus, saturates are obtained by adding n-
heptane, aromatics are separated by adding toluene, and resins by (% asphaltenes)
adding pyridine. SI =
(% resins) (3)
In the present study, SARA fractionation was carried out by means
of preseparation of asphaltenes from the crude oil by adding an excess 2.3.4. Stankiewicz Stability Criterion. In the Stankiewicz stability
of n-heptane, using a 40:1 solvent-to-crude oil volumetric ratio, criterion (SSC), the A/R ratio is plotted against S/Ar. This type of
according to ASTM D-4124. The saturated, aromatic, and resin representation gives a quick identification of the risks of separation of
fractions were then extracted from the deasphalted oil using the clay− asphaltenes by locating the stable and unstable zones.24,25
gel absorption chromatographic method (ASTM D-2007). This 2.3.5. Sepúlveda Stability Criterion (Stability Cross Plot).
fractionation procedure is represented by the shaded rectangles in According to Sepúlveda et al.,24 the stability cross plot (SCP)
Figure 1. The results obtained from the SARA analysis of the different method uses four relationships
crude oils are presented in Table 2.
SCP1: [(R/A)/(S/Ar)] versus [Ar/A] (4)
Table 2. SARA Analysis of Crude Oils SCP2: [(R/A)/(S/Ar)] versus [R/A] (5)

crude saturates aromatics resins asphaltenes inorganics, SCP3: [S/Ar] versus [R/A] (6)
oil (S), wt % (Ar), wt % (R), wt % (A), wt % wt %
SCP4: [(R/A)/(S/Ar)] versus [Ar/(S/A)] (7)
C52 59.65 3.35 36.95 0.03 0.02
C37 31.85 54.08 13.14 0.91 0.02 In this method, the quotients indicated in eqs 4 and 5 are included in
C34 50.89 21.95 24.24 2.90 0.02 the four SCP, where a reference curve represents the metastable zone,
C32 19.23 42.02 36.35 2.40 0.01 and it also works as the limit between stability and instability zones.
C29 26.14 41.23 28.71 3.91 0.01 The method involves the comparison of four parameters, and it is
possible that not all of them indicate the same condition of stable,
C24 27.80 36.75 27.82 7.20 0.43
metastable, or unstable. In such a case, the sample should be classified
C16 10.48 9.00 64.08 16.17 0.27
according to the more repeated condition. For instance, in the case of
C10 9.39 31.97 35.20 23.40 0.04 a sample with the following results: SCP1 = metastable, SCP2 =

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unstable, SCP3 = stable, and SCP4 = metastable, the final

classification of the sample corresponds to metastable.
2.4. Evaluation of the Stability of Crude Oils with
Experimental Techniques. Some standardized analytical techni-
ques to detect the onset of asphaltene precipitation by means of
optical devices are commercially available. Three recognized methods
are next listed: a Turbiscan based on the ASTM D7061 method
renders a separability number of asphaltenes; a Porla crude oil
stability and compatibility analyzer based on the ASTM D 7112
method yields solvent equivalence, P-value, and FR5/1; and an ROFA
France automated stability analyzer based on the ASTM D7157
method whose results are indicated as the intrinsic stability of the oil
(S-value), the peptizing power of the oil (So), and the peptizability of
asphaltenes (Sa). In the present research, the ROFA France method
was employed.26
Additional nonoptical-based methodologies can also be used to
estimate the stability of crude oils. In this research, two methods were
executed: the static column test, based on the degree of modification
of a particular crude oil property after a certain time on storage, and
the spot test based on the ASTM D4770 method,27 which
encompasses visual inspection of the pattern of a drop on the surface
of a filter paper.
2.4.1. Determination of Intrinsic Stability (S-Value, ROFA).
Intrinsic stability was measured by the ASTM D7157 method,
which is based on measuring the asphaltene flocculation point in
crude oil samples. The method encompasses previous peptization of
asphaltenes by adding an aromatic solvent (toluene), and then a
constant flow of a paraffinic solvent (n-heptane) is successively added
until the asphaltene flocculation point is detected by an optical sensor
in an automated integrated analytical measurement system.
For the analysis of the stability of a sample, three different dilutions
in toluene are prepared. All three dilutions are automatically titrated
with n-heptane to detect asphaltene precipitation. The optical sensor
monitors the formation of flocculated asphaltenes during the titration.
In the first stage, the optical signal is gradually increased due to the
clearest sample by consistent addition of n-heptane. In the second
stage, aggregation of asphaltenes produces a large and sustained Figure 2. Equipment for the static column test.
decrease in light intensity. Hence, the maximum in the signal is
ascribed as the flocculation point of asphaltenes.
Based on the amount of n-heptane added at the flocculation point,
the sample mass, and the volume of toluene used in the three highly stable. On the contrary, if the value of a given property changes
dilutions, the computation routine calculates the intrinsic stability of considerably after a period of storage, the crude oil is unstable, since
the oil (S-value), the peptizing power of the oil (So), and the the change of such property is likely the result of asphaltene
peptizability of asphaltenes (Sa). The calculation of these parameters segregation.
includes plotting the oil-to-solution ratio (1/X) and the flocculation By the static column test, stability can be evaluated based on
ratio (FR) and fit the three dilutions data into a straight line to obtain several properties, such as the content of sulfur, metals, and
the reciprocal critical n-heptane dilution and the maximum asphaltenes; density; or viscosity. In the present study, stability is
flocculation ratio according to the following equations related to the content of asphaltenes. For such evaluation, an aliquot
of the crude oil is transferred and stored in the static column. The
1 mass of oil content of asphaltenes is analyzed and then the sample is left to rest
=
X volume of toluene + volume of n−heptane (8) for 7 days at a temperature of 35 °C and atmospheric pressure
(typical operating conditions of storage tanks). Afterward, the crude
volume of toluene oil samples taken from the upper, middle, and lower parts of the
FR = column are recovered and characterized. The crude oil samples were
volume of toluene + volume of n−heptane (9)
subjected to the stability test in the static column, and the results
S = 1 + X min (10) obtained are presented in Table 9.
stability =
Sa = 1 − FR max (11)
asphaltene content t = 0 − asphaltene content after the storage period
1.0 − [ ]
S0 = S × FR max (12) asphaltene content t = 0
2.4.2. Stability Evaluation of Crude Oils in a Static Column. A (13)
simple way to measure the stability in crude oil samples or mixtures is The storage stability of a product is revealed when its properties after
with the “static column stability” test. This method is based on the the storage period in the static column are equal to its original
analysis of a selected crude oil property in a sample stored in a properties (zero resting time). Hence, the ideal stability value = 1.0,
stainless steel vessel, as depicted in Figure 2. The sample is analyzed at since it corresponds to the case when the same value of the property
two moments in time: just after being introduced in the vessel and measured at the beginning and at the end of the storage is observed.
after a certain time of storage as defined by the researcher. The basic Depending on the property chosen to assess the stability after storage,
idea is to detect to what extent the value of a chosen property is the value of the property may result in a higher or lower value with
preserved during sample storage. In accordance, the crude oil whose respect to the value at zero resting time. For this reason, the stability
chosen property is unaltered during the storage period is considered of the samples by the static column test may take values lower or

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higher than 1.0, and the criterion employed is that when the stability solution. Based on SI, all the samples are ascribed as stable and
value is closer to 1.0, the stability degree is higher. only the C10 sample is characterized as unstable.
By considering the possible stratification of heavy components in The CII can also be represented graphically by plotting the
the crude oil sample, the design of the static column shown in Figure sum of saturates and asphaltenes (S + A) as a function of the
2 includes valves for sampling at three different heights in the column:
at the top, in the middle, and at the bottom of the column.
sum of resins and aromatics (R + Ar), as shown in Figure 3. In
2.4.3. Spot Test. This method is used to quickly identify possible
risks of operation during the transportation and storage of oils (sludge
settlement in storage tanks, plugging in process lines, etc.), caused by
the incompatibility between the different streams, which by presenting
notable differences between their chemical nature lead to the
separation and precipitation of heavy species (asphaltenes).
The test consists basically of placing a drop of the sample under
evaluation on a filter paper, drying it to defined conditions, and at the
end, visually observing the spot left by the drop and classifying it
according to reference numbers.
By direct observation of the spot pattern left by each oil on the
filter paper, crude oils can be qualitatively classified within five groups
of samples as a function of the asphaltene flocculation degree. From 1
to 5, the asphaltene state may be ascribed as high peptized asphaltenes
(level 1) to precipitated asphaltenes (level 5). According to the
method, if a sample leaves spots that are classified as 3 or more, the
said sample presents instability, and evidently, it grows as approaching Figure 3. Graphical representation of CII with data from the SARA
the maximum value of 5. analysis of crude oils.

3. RESULTS AND DISCUSSION

3.1. Stability of Crude Oils by Methods Based on such a representation, CII falls into the reference dotted line
SARA Analysis. From the results shown in Table 2, it can be and three zones are readily identified: (1) a zone of instability
seen that the highest asphaltene content corresponds to C10 at the left-hand side of the curve, delimited by (S + A) ≥ 47.4
and C16. The asphaltene fraction is the only one that shows a wt % corresponding to (R + Ar) ≤ 52.6 wt % (CII ≥ 0.9), (2)
correspondence with respect to API gravity of crude oils, the a zone of metastability at the middle, where 47.4 wt % > (S +
heavier the crude oil (lower API), the higher its asphaltene A) > 41.1 wt % and 52.6 wt % < (A + R) < 58.9 wt % (0.9 >
content. In the case of saturated compounds, it is normal to CII >0.7), and (3) a zone of stability at the right-hand side of
find them more concentrated in light crude oils. Regarding the the curve, delimited by (S + A) ≤ 41.1 wt % corresponding to
content of resins and aromatics, a clear trend with API gravity (R + Ar) ≥ 58.9 wt % (CII ≤ 0.7). Figure 3 allows for a better
is not observed, maybe because of the different oil fields from visualization of the nature of the studied crude oils. It is
which the crude oils were recovered. observed that most of the samples are located within the
Based only on crude oil characterization by SARA analysis, stability zone, which includes C24, C10, C37, C29, C16, and
the behavior in terms of the stability or instability of their C32. Samples C52 and C34 are located in the zone of unstable
asphaltenes cannot be established. For this reason, the SARA- crude oils.
based stability/instability parameters were calculated. CII also allows to ascertain the degree of stability, since, for
Table 3 presents the values obtained for stability index (SI), the stable samples, they exhibit the following stability order:
colloidal instability index (CII), and colloidal stability index C32 > C16 > C29 > C37 = C10 > C24. Such an affirmation is
based on the statement that the higher the CII value, the worse
Table 3. Results of SI, CII, and CSI the colloidal stability. The Stankiewicz criterion (SSC), where
the A/R ratio is plotted against S/Ar, is shown in Figure 4. It is
crude observed that C52, C32, C37, and C39 are stable, with C32
oil SI designation CII designation CSI designation
being the most stable crude oil, as it corresponds to the
C52 0.001 stable 1.48 unstable 0.78 stable furthest point from the curve limiting the stable zone curve.
C37 0.069 stable 0.49 stable 0.35 stable Accordingly, C16 and C34 are unstable, with C34 being the
C34 0.120 stable 1.16 unstable 1.05 unstable
C32 0.066 stable 0.28 stable 0.19 stable
C29 0.136 stable 0.43 stable 0.31 stable
C24 0.259 stable 0.54 stable 0.43 stable
C16 0.252 stable 0.36 stable 0.34 stable
C10 0.665 unstable 0.49 stable 0.61 stable

(CSI), which were calculated with the SARA analysis of the

crude oils. The stability index accounts for the asphaltene/
resins (A/R) ratio, and it has been stated that crude oils with
SI values lower than 0.35 can be considered as stable.23 The SI
index is simple and is broadly used because both asphaltenes
and resins are heavy, nonvolatile, and can be precisely
quantified. It is based on the consideration that resins act as
natural peptizers of asphaltenes, maintaining them in the oil Figure 4. Criteria of stability of Stankiewicz for crude oils.

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Figure 5. Stability cross plot for different relationships based on SARA analysis.24

Table 4. Behavior of Crude Oils in SCP charts

crude oil SCP1 SCP2 SCP3 SCP4 average
C52 stable stable stable stable stable
C37 stable stable stable stable stable
C34 stable stable stable stable stable
C32 stable stable stable stable stable
C29 stable stable stable stable stable
C24 stable stable stable stable stable
C16 unstable metastable metastable metastable metastable
C10 metastable unstable stable metastable metastable

Table 5. Comparison of Stability Results Based on SARA Fractions

crude oil CII CSI SI SSC SCP average
C52 unstable stable stable stable stable stable
C37 stable stable stable stable stable stable
C34 unstable unstable stable unstable stable unstable
C32 stable stable stable stable stable stable
C29 stable stable stable stable stable stable
C24 stable stable stable metastable stable stable
C16 stable stable stable unstable metastable metastable
C10 stable stable unstable metastable metastable metastable

most unstable crude oil, while C10 and C24 crude oils have a that on average, the most stable crude oils are C37 and C32
metastable character. (which are the lightest crude oils), since the five compared
Figure 5 shows the graphical representation of these four methods agreed on the stable characteristic. The crude oils
relationships. It is necessary to examine the behavior of each with less stability are C16 and C10, since the average of the
sample in the four graphs to obtain a single result that four compared methods characterizes them as metastable.
characterizes the state of the asphaltenes contained in the In general, the results do not show a correlation between the
sample. It was observed that most of the crude oils are stable, type of crude oil according to its API gravity and its
and only C16 and C10 oils are metastable. The behavior of classification as stable or unstable. In spite of the high content
each of the samples in the four graphs is presented in Table 4. of asphaltenes, heavy crude oils were found as stable given
The results obtained with the different methods were their high content of resins that preserves the colloidal system
compared to verify the effectiveness of the different criteria, steady. On the other hand, instability was observed in the case
which are summarized in Table 5. In general, it can be seen of some light crude oils. In general, as the crude oils become
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lighter, the relative amount of saturates grows and the content samples can be qualitatively classified within five groups as a
of asphaltenes diminishes. Light crude oils with a minimal function of the asphaltene flocculation degree, with spot
amount of asphaltenes may be classified as unstable by some reference 1 being the case when the asphaltene state may be
indexes, but the precipitation of asphaltenes is not quantifiable. ascribed as high peptized asphaltenes, while spot reference 5
This is the case of the C52 sample. However, light crude oils corresponds to precipitated asphaltenes. The characteristics of
with a significant amount of asphaltenes, as in the C34 sample, the spot pattern according to the scale referred in the method
usually are prone to deactivation as a result of the high amount are included in Table 6. By such an approach, it was
of saturates.
Some variations in the prediction of crude oil stability Table 6. Spot Test Scale
measured by the different indexes based on SARA analysis
spot
were observed. In this sense, it is important to highlight that reference spot characteristics
SARA analysis groups hydrocarbons according to their 1 homogeneous spot (no presence of inner ring)
solubility/insolubility behavior (Figure 1). In a broad sense, 2 very thinly defined inner ring
the stability condition of crude oils depends on the equilibrium 3 well-defined inner ring, faint and only slightly darker than the
among the SARA fractions where the polar asphaltenes are background or rest of the spot
stabilized by resins within the less polar aromatic and saturate 4 well-defined inner ring, slightly denser than reference spot 3 and
components in the crude oils; in such a case, molecular somewhat darker than the background or rest of the spot
interactions reach a balanced colloidal system. Unbalance of 5 solid or almost solid area, very dark in the center; the central area
is much darker than the background or rest of the spot
such a system may result in aggregation of asphaltenes and
eventually in solid precipitation. Accordingly, disturbance of determined that C52, C32, C29, C24, C16, and C10 crude
the crude oil colloidal system is usually produced by changes in oils are stable. C37 presents a stain corresponding to level 2
composition, temperature, or pressure. (very dimly defined inner ring), but it is also stable. C34 crude
The assessment of stability using SARA-based method- oil has a stain pattern of level 3 that corresponds to the crude
ologies is based on the solubility behavior of the components oil with flocculated asphaltenes and therefore is unstable.
of the crude oil. However, chemical and structural parameters The values of S, Sa, and So obtained with an ROFA
of the molecules and molecular interactions are not considered equipment for all crude oils are presented in Table 7. The
within SARA-based indexes, and it may explain the lack of
uniformity by several indexes for predicting stability in some Table 7. Intrinsic Stability Parameters
crude oil samples. In this sense, it is important to consider the
properties of asphaltenes such as the type of molecular crude S Sa So condition
structure, elemental composition, aromaticity, and self- C52 2.62 0.02 2.56 stable
aggregation phenomena in the stability character of crude C37 2.70 0.84 0.44 stable
oils.30 For instance, the unstable character of crude oil samples C34 3.61 0.75 0.89 stable
was related to low hydrogen-to-carbon ratios and high C32 3.90 0.79 0.81 stable
aromaticity of asphaltenes.31,32 Accordingly, further research C29 2.70 0.72 0.76 stable
efforts are necessary to include the properties of asphaltenes C24 3.65 0.76 0.88 stable
within indexes or methodologies to count on reliable and C16 2.89 0.65 1.00 stable
universal tools to predict the stability of crude oils. C10 3.22 0.69 1.00 stable
3.2. Stability of Crude Oils Obtained with Exper-
imental Techniques. The results obtained by means of the
standard test method for cleanliness and compatibility of minimum value of S is 1, which indicates that the sample is
residual fuels are shown in Figure 6. By direct observation of unstable and its asphaltenes are already precipitated without
the spot pattern left by each crude oil on the filter paper, the the addition of paraffin. As the value of S increases, the crude
oil achieves a greater degree of stability. Hence, the method
allows for comparing the relative stability among crude oil
samples. However, the definite character of being stable or
unstable of a sample cannot be assigned. In this sense, the
order of stability of the samples measured by this technique is
C52 > C37 = C29 > C16 > C10 > C34 > C24 > C32. In all
cases, the S-value was higher than 2.5. In an arbitrary way, by
considering samples with S > 2.5 as stable, all crude oils of the
present study may be classified as stable according to this
technique.
The results shown in Table 8 include stability data for the
top, middle, and bottom of the static column. By considering
the asphaltene content, the results fall within a 5 wt % of error.
C37, C32, C29, C24, C16, and C10 samples clearly show
values of stability close to 1 along the column, thus implying
stability and that a stratification process did not occur. The
results of C34 crude oil exhibit a clear trend in the asphaltene
content and consequently in the stability values along the
column height. Hence, C34 crude oil results as an unstable
Figure 6. Spot test for crude oils. sample during storage.
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Table 8. Results Obtained in the Static Column Test 3.3. Oil Compatibility Model. The oil compatibility
model was applied to the hypothetic blends of C52 with all of
stability at the stability at the stability at the
crude top of the middle of the bottom of the the crude oil samples studied. Based on Sa and So parameters
oil column column column condition obtained from the ROFA equipment, the insolubility number
C52 1.000 0.667 1.333 stable (IN) and the solubility blending number (SBN) can be
C37 1.011 1.011 1.033 stable calculated to employ the oil compatibility model by the
C34 0.901 0.956 1.148 unstable following equations28,29
C32 1.004 1.008 1.008 stable IN = (100)So (14)
C29 1.003 1.003 1.008 stable
C24 0.986 0.992 0.969 stable SBN = 100(1 − Sa) (15)
C16 1.002 1.011 1.017 stable
C10 0.993 0.996 0.996 stable The SBN/INmax ratio is a criterion for compatibility between two
crude oils. A high value of this ratio indicates greater stability.
When this ratio is less than 1, the corresponding blend is
incompatible. A value slightly greater than 1 represents
C52 crude oil is a special case, since it has the lowest content uncertain compatibility and a value greater than 1 indicates a
of asphaltenes (0.03 wt %), and the values of the asphaltene compatible blend. The values of IN, SBN, and SBN/IN are
content at different positions range from 0.02 to 0.04 wt %. reported in Table 9.
Such values fall within the experimental error, so the stability The maximum IN value (INmax = 98) corresponds to the C52
calculated by eq 13 (1.0−1.333) must be taken into account sample. SBN/INmax values slightly higher than 1 were obtained
for this type of low-asphaltene crude oils. It should be noted for the case of blending C52 with C16 and C10, which
that small values of the asphaltene content might yield to suggests uncertain compatibility. In the case of C52 with C37,
classified samples as unstable due to errors in the experimental C34, C32, C29, and C24, values lower than 1 were obtained,
determination and not necessarily to asphaltene aggregation. which indicates a higher probability of incompatibility. Since
Hence, it is important to consider the accuracy of the property the insolubility value of C52 is higher than the SBN determined
employed to estimate stability by the static column method. In from the other crude oils, it denotes the existence of
accordance, C52 is qualified as stable crude oil. incompatible mixtures. This agrees with the results of the
Methodologies for the experimental assessment of stability spot test shown in Figure 7, in which it is clearly observed that
employed in the present research include several approaches. C52 crude oil in different proportions with other crude oils is
The static column test is focused on analysis in static mode capable of causing the instability of the asphaltenes.
(storage). Nonetheless, storage implies perturbation-free Prediction of the compatibility of crude oils is still a pending
conditions resulted in the stable character of most of the issue, since a common practice in crude oil processing includes
samples. The spot test is a simple and fast test, including blending of two or more streams, sometimes of considerably
evaporation of light components of an oil drop over a filter different characteristics. There are additional methods to the
paper, which implies changes in the composition of the leftover oil compatibility model in the scientific literature.40−46
sample during the process, and the interpretation of the result Validation of such methods and/or generation of new ones
depends on the visual acuity of the observer. The S-value with application to domestic crude oils are desirable.
method encompasses modification of the sample by addition of
an aromatic solvent to assure peptization of asphaltenes and 4. CONCLUSIONS
then titration of such a modified sample with a paraffinic
solvent to provoke asphaltene flocculation. The process is According to the use of different methods to determine the
optically monitored, and the results imply extrapolation of the stability of a wide variety of crude oils, the following can be
quantities measured to those of the sample nonmodified by concluded:
aromatic solvent addition. The S-value stability results are • Based on SARA analysis, C32 crude oil shows the
useful to compare the relative stability among different greatest stability due to its relatively low content of
samples. The obtained parameters are not readily translated asphaltenes, high content of resins, which are the
to a stability/instability degree of practical significance. compounds that help asphaltenes remain in a peptized
Due to the complexity of the peptization, flocculation, and state, and also high content of aromatics. Both resins and
precipitation of asphaltene phenomena, several attempts of aromatics aid to keep the asphaltenes in solution in the
alternatives or modified methodologies for the measurement of crude oil. For these reasons, this crude oil is the most
crude oil stability have been reported.33−39 stable.

Table 9. Results of the Oil Compatibility Model

crude S Sa So SBN = 100(So) IN = 100(1 − Sa) SBN/IN SBN/INmax

C52 2.62 0.02 2.56 256 98 2.61 2.61
C37 2.7 0.84 0.44 44 16 2.75 0.45
C34 3.61 0.75 0.89 89 25 3.56 0.91
C32 3.9 0.79 0.81 81 21 3.86 0.83
C29 2.7 0.72 0.76 76 28 2.71 0.78
C24 3.65 0.76 0.88 88 24 3.67 0.9
C16 2.89 0.65 1.00 100 35 2.86 1.02
C10 3.22 0.69 1.00 100 31 3.23 1.02

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Energy Fuels 2021, 35, 408−418
Energy & Fuels pubs.acs.org/EF Article

Figure 7. Spot test of blends of C52 with other crude oils. *RN = Reference numbers of the type of spot obtained according to ASTM D4740: 1
and 2 (dispersed asphaltenes), 3 (asphaltenes starting to flocculate), 4 (flocculated asphaltenes), and 5 (precipitated asphaltenes).26

• The colloidal instability index and the Stankiewicz plot produced by addition of solvents into crude oils.
provide uncertain results, while the stability cross plot Nonetheless, the result is displayed as a relative
method renders higher certainty for estimating the parameter. The spot test is revealed as a quick and
stability of asphaltenes in crude oils. effective technique, but it depends on the visual
• All approaches are recommended to be used to obtain a perception of the observer. The static column test has
better prediction of the stability of asphaltenes in crude several advantages: it is effective, it does not require
oils. The average result can be assumed as the solvent incorporation, and it is possible to measure the
characteristic that best defines the stability character of stability of asphaltenes at any pressure and temperature.
asphaltenes in crude oils. Nonetheless, the stability is determined indirectly by
• The intrinsic stability results obtained using the ROFA means of a chosen property, and the procedure is time-
equipment determined that all crude oils are stable and consuming.
that C32 crude oil is the most stable, while the lowest • The application of the different approaches is useful in
stability is found for C52 crude oil. the determination of the stability of asphaltenes in crude
• The spot test and the static column test classified C34 oils or blends. The stability character of asphaltenes in a
crude oil as unstable, unlike the stability predicted by the given crude oil may be established by averaging the
ROFA equipment. The other crude oils were classified results from different methodologies.
as stable by the three experimental methods. • From the practical point of view, pertinent cautions on
• The ROFA method measured stability by optical the handling of samples must be observed if at least one
detection of the flocculation of asphaltenes artificially of the methods classifies the sample as unstable or
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Energy Fuels 2021, 35, 408−418
Energy & Fuels pubs.acs.org/EF Article

metastable. It is recommendable to obtain all of the asphaltenes analysis: computational-intelligence-based models. SPE J.
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Oil−Precipitant Systems. Energy Fuels 2011, 25, 1585−1596.
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• Further research efforts are necessary to include the (14) Ancheyta, J.; Speight, J. G. Hydroprocessing of Heavy Oils and
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Press, Taylor and Francis Group, 2009.
(16) Hasanvand, M. Z.; Montazeri, M.; Salehzadeh, M.; Amiri, M.;
AUTHOR INFORMATION Fathinasab, M. A literature review of asphaltene entity, precipitation,
Corresponding Author and deposition: introducing recent models of deposition in the well
Jorge Ancheyta − Instituto Mexicano del Petróleo, Mexico City column. J. Oil Gas Petrochem. Sci. 2018, 1, 83−89.
07730, Mexico; orcid.org/0000-0001-9626-637X; (17) Matsushita, K.; Marafi, A.; Hauser, A.; Stanislaus, A. Relation
Email: [email protected] between relative solubility of asphaltenes in the product oil and coke
deposition in residue hydroprocessing. Fuel 2004, 83, 1669−1674.
Authors (18) American Society for Testing and Materials (ASTM). ASTM
Roque Guzmán − Instituto Mexicano del Petróleo, Mexico D7061, Standard Test Method for Measuring n-Heptane Induced Phase
City 07730, Mexico Separation of Asphaltene-Containing Heavy Fuel Oil as Separability
Silvano Rodríguez − Instituto Mexicano del Petróleo, Mexico Number by an Optical Scanning Device. ASTM International: West
City 07730, Mexico Conshohocken, PA, 2019.
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Pablo Torres-Mancera − Instituto Mexicano del Petróleo,
and the structure of petroleum. Oil Gas Sci. Technol. 2004, 59, 467−
Mexico City 07730, Mexico 477.
Complete contact information is available at: (20) Ashoori, S.; Sharifi, M.; Masoumi, M.; Salehi, M. M. The
https://pubs.acs.org/10.1021/acs.energyfuels.0c03301 relationship between SARA fractions and crude oil stability. Egypt. J.
Pet. 2016, 26, 209−213.
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The authors declare no competing financial interest. Heteroatom Species Effects in Fouling of Heat Exchangers by

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