Fuel 118 (2014) 426–431

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Fuel
journal homepage: www.elsevier.com/locate/fuel

Organic and elemental elucidation of asphaltene fraction of Nigerian

crude oils
F.M. Adebiyi a,b,⇑, V. Thoss a
a
School of Chemistry, Bangor University, Bangor, United Kingdom
b
Department of Chemistry, Obafemi Awolowo University, Ile-Ife, Nigeria

h i g h l i g h t s

 We provide data on the organic and elemental composition of the asphaltene component of Nigerian crude oils.
 We provide information on the quality of Nigerian crude oils.
 The study provides information on the properties of asphaltene component.
 The information provided will assist in the refining and processing paths of the natural resource.

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

Article history: This paper provides data on the chemical composition of the asphaltene component of Nigerian crude oils
Received 8 July 2013 in order to ascertain its properties which can assist in the refining and processing paths of the natural
Received in revised form 17 October 2013 resource. Crude oil samples were collected from three major oil fields in Nigeria and were deasphalted
Accepted 17 October 2013
using n-pentane. The organic characteristics of the precipitated asphaltenes were determined using Fou-
Available online 8 November 2013
rier Transform Infrared (FT-IR) Spectrometry, while the elemental contents were measured by Induc-
tively Coupled Plasma Atomic Emission spectroscopy (ICP-OES) and Carbon and Nitrogen Analyzer.
Keywords:
Comparison of the average content of the Nigerian crude oils asphaltene with that of other nations shows
Asphaltene
Crude oil
that the Nigerian crude oil asphaltene content (3.65%, w/w) is less than that of other nations, except for
Element Russian crude oil, but slightly higher than that of Brazilian crude oil, indicating that asphaltene deposition
Organic group may pose less problems during Nigerian crude oil development than most of the crude oils from other
Spectroscopic analyses nations. The IR spectra of the asphaltenes indicate the presence of alkanes, aromatic rings, phenyl rings,
alcohols, ethers, carboxylic acids, esters, aldehydes, ketones, anhydrides, organic sulphoxides, sulphate
salts and thiobenzophenones, confirming the fact that asphaltenes are composed of high molecular
weight polycyclic constituents comprising of nitrogen, sulphur and oxygen heteroatoms. Ten elements
(Cr, Cu, Fe, Mn, Ni, S, V, Zn, C and N) are examined and their concentrations determined. The results show
that the values of all the elements are comparatively higher in the asphaltenes than the crude oils due to
the presence of comparatively high concentrations of porphyrins in the asphaltenes than the crude oils.
This is confirmed by their T-test values. Cross plot analysis result between the asphaltenes and crude oils
using their elemental mean concentrations as variables indicates that moderate and positive correlation
(R2 = 0.53) exists between them, indicating inter-element and geochemical relationships between them.
Elemental clustering analysis results present two groups which are also fairly correlated. As expected, the
elements show very close clustering because all the elements are known to associate with petroleum
hydrocarbon formation. Also, apart from N, S and C; other elements are transition metals with similar
chemical affinity.
Ó 2013 Elsevier Ltd. All rights reserved.

1. Introduction at a dilution ratio of 40 volumes of solvent per volume of the petro-

Asphaltenes are usually defined as that fraction of petroleum,
which is soluble in toluene and insoluble in n-pentane or n-heptane
⇑ Corresponding author at: Department of Chemistry, Obafemi Awolowo Univer-
sity, Ile-Ife, Nigeria. Tel.: +234 8034237426.
E-mail addresses: fmbiy@oauife.edu.ng, biyi20042000@yahoo.com
(F.M. Adebiyi).
leum sample. Asphaltenes are present in crude oils as colloidally
suspended solid particles. Precipitation of asphaltene occurs when
the oil loses its capacity to keep those particles dispersed [12,13,6].
Alterations in pressure, temperature, composition and shear
rate may cause asphaltene precipitation and deposition. The alter-
ations may occur due different processes used; primary depletion,
injection of natural gas or carbon dioxide, acidizing treatments and

0016-2361/$ - see front matter Ó 2013 Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.fuel.2013.10.044
 F.M. Adebiyi, V. Thoss / Fuel 118 (2014) 426–431
commingled production of incompatible fluids. Asphaltenes have
practical uses, such as material for road construction, waterproof-
ing and roofing, curing agents, corrosion inhibitors, stability of oil–
water emulsions and in formation wettability, however they are
usually ascribed to be a threat in the oil field. Asphaltene deposi-
tion may occur at many points along the production system, such
as inside the formation pumps, tubing, wellheads, safety valves,
flow-lines and surface facilities. Sheer occurrence of asphaltenes
in crude oil does not indicate asphaltene-related production prob-
lems; minor quantity of asphaltenes when adhere to formation
grains, pumps, tubulars, safety valves and flow-lines may not dis-
rupt flow, but dense deposits can bring production to a standstill.
Optimizing production in this case calls for the knowledge of the
oil composition and the conditions under which its asphaltenes
will remain in solution. Asphaltene-deposition problems may also
be pronounced in lighter oil containing little content of asphalt-
enes in reservoir with pressure above bubble point [3,10,8,7].
The possibility of asphaltenes to clog systems continues down-
stream, and worrisome for refiners, because asphaltenes are signif-
icant constituents of the crude oils that are increasingly entering
refinery processing streams. Remediation of the heavy organic
deposits in the course of petroleum production has been a costly
process and it has hampered the production activities in many
parts of the world. Solid particles suspended in the crude oil may
stick to the walls of the conduits and reservoirs. The toughness
of the precipitate may be related to the occurrence of asphaltene
in the crude oil even at small levels. Asphaltene is a highly polar
compound and usually act as glue and mortar in hardening the
deposits and, as a result, preventing oil flow [12,4,5].
Nigeria is endowed with huge deposits of crude oil. She is the
13th major world oil producer, and there are investigations
[1,11] which are still on-going on the deposits, but there are few
references to the asphaltene fraction of the crude oils. This article
therefore characterizes the asphaltene fraction of crude oils ob-
tained from three major Nigerian crude oil deposits using Fourier
Transform Infrared (FT-IR) Spectrometry for compound types,
while Inductively Coupled Plasma Atomic Emission spectroscopy
(ICP-OES) and carbon/nitrogen (C/N) analyzer were used for ele-
mental composition elucidation. This will give insight to the con-
tents and nature of the asphaltene fraction as well as assisting
the refining and processing paths of Nigerian crude oils.
2. Experimental
2.1. Precipitation of asphaltene from crude oil
Samples of crude oil were collected from Belema, Imo and Eket
oil fields in the Niger Delta area, Nigeria. Asphaltenes for this work
were precipitated with n-pentane using a solvent to the crude oil
ratio of 40:1. The precipitated asphaltenes were separated from
maltenes (n-pentane solubles) by filtration and then washed with
an equal volume of n-pentane. The solvent (n-pentane) was then
removed using stream of N2 gas followed by drying of the asphal-
tene at 70 °C in oven. The total yield (%/weight) was then calcu-
lated and reported.
2.2. Spectroscopic analyses
2.2.1. Infrared (IR) spectroscopy identification of functional groups in
the asphaltene fraction
Infrared (IR) spectra were recorded on a Perkin Elmer Model spec-
trum 100 Fourier Transform Infrared Spectrometer coupled with
Samsung ML-3051N printer. Solutions for obtaining the IR spectra
were prepared by dissolving 30–50 mg of sample in 1.00 ml of Nujol
(spectroscopic grade). All IR spectra were obtained using a 0.1-mm
427
path length sample KCl cell. Spectra were recorded using the follow-
ing settings; number of scans 4; gain 1; apodization weak; and reso-
lution 4. Salt plates and windows of sealed cells were of KCl.
2.2.2. Elemental characterization
2.2.2.1. Inductively Coupled Plasma Optical Emission Spectrometry
(ICP-OES) analysis. Measured weight (0.50 g) each of the asphal-
tene samples was put in a covered crucible and placed in a Gallen-
hamp muffle furnace which was maintained at 550 °C for 5 h. After
ashing and cooling, 1 ml of 2 M HCl was added to the sample and
allowed to boil to near dryness. This was followed by another batch
of 1 ml of 2 M HCl but left to boil only for a few minutes before
being transferred into a 50 ml volumetric flask. The crucible was
rinsed several times with deionized water into the flask and then
made up to the graduating mark. The above procedure was strictly
followed in the preparation of the blank sample. All the digested
samples were stored in thoroughly cleaned plastic bottles for ele-
mental analysis using Inductively Coupled Plasma-Optical Emis-
sion Spectrometer ICP-OES (model Varian 71 O-ES ICP Optical
Emission Spectrometer).
2.2.2.2. Carbon–nitrogen analysis. 0.150 g samples were weighed in
a tin crucible and placed in the auto sampler and introduced into
the high temperature combustion furnace. At 1100 °C the carbon
was completely oxidized to CO2 and nitrogen converted into NOy
in the presence of oxygen. After the catalyst furnace where the oxi-
dation reaction usually takes place, the sample passed through a
Peltier cooler to remove moisture formed by condensation. Then
the sample gas splitted and transferred, by the carrier gas helium
to the reduction oven. In the reduction oven of 600 °C NOy was re-
duced, in the presence of a copper reductor, to N2. Then first the
CO2 was measured by Non Dispersive Infra-red Detection (NDIR)
for total carbon and subsequently the by-products, water and car-
bon dioxide were removed by an absorber. Secondly the N2 gas was
measured by Thermal Conductivity Detection (TCD).
2.3. Quality assurance and quality control
An Analar grade ethylenediaminetetraacetic acid (EDTA) with N
(41.03%) and C (9.57%) was used as standard reference material for
C and N analysis. The analyzed EDTA was prepared following the
same protocols as the asphaltene samples, and the results N
(40.93%) and C (9.60%) obtained were in good agreement with
the stated certified values. The C/N Analyzer, IR spectrometer and
ICP-OES used were calibrated using in-house calibration standards.
2.4. Data analysis
The overall data obtained on the elemental investigation of the
asphaltenes were statistically analyzed and interpreted using
descriptive and inferential technique viz; variation diagrams, T-
test, cluster and cross plot analyses. Cross plot analysis using gross
elemental concentrations as variables was carried out in this study
to establish inter-elemental relationship the Nigerian crude oil and
its asphaltene fraction. The cross plot analysis was carried out
using Microsoft Excel. The cluster analysis was carried out using
the furthest neighbor (complete linkage) grouping of the hierarchi-
cal cluster analysis in the Statistical Package for Social Scientist
(SPSS) package. This was done to group the analyzed elements into
families. The concentrations of the analyzed elements in the Nige-
rian crude oil and its asphaltene were also subjected to statistical
analysis using T-test. The T-test was calculated using Microsoft ex-
cel. The data were analyzed using T-test to know whether there
was significant difference between the concentrations of each
element in the two set of samples. Level of parameter was consid-
ered significant if T-test value was less than 0.05.
428 F.M. Adebiyi, V. Thoss / Fuel 118 (2014) 426–431

Fig. 1. Frequency distribution of the asphaltene fraction content of the Nigerian
crude oils.
3. Results and discussion
The gravimetric data for the solvent deasphaltened crude oils is
presented in Fig. 1. From the figure it is observed that crude oil ob-
tained from Belema field shows the highest value of asphaltene
(3.83%, w/w) followed by crude oil obtained from Eket field with
a value of 3.79%, w/w, while crude oil obtained from Imo field
has the lowest value (3.34%, w/w). The result indicates that trans-
portation and refining of crude oil from Imo field may encounter
less asphaltene deposition problem. Comparison of the mean con-
tent (3.65%) of Nigerian crude oil asphaltenes with that of other na-
tions – Canada, Athabasca (15.0%), Venezuela, Boscan (17.2%),
Mexico, Panucon (12.5%), Brazil, Campos (2.80%, w/w) and Russia,
Kaluga (0.5%). It is observed that the Nigerian crude oil asphaltene
content is less than that of other nations, except for Russian crude
oil and slightly higher than that of Brazilian crude oil [15]. This
suggests that Nigerian crude oils are likely to encounter less
asphaltene deposition challenges during crude oil development
than most of the crude oils from other nations.
The results of the assignment of probable functional groups in
the asphaltenes are presented in Table 1, while an IR spectrum of
one of the samples is presented in Fig. 2. The IR spectra of the
asphaltenes indicate the presence of alkanes, aromatic rings, phe-
nyl rings, alcohols, ethers, carboxylic acids, esters, aldehydes, ke-
tones, anhydrides, Organic sulphoxides, sulphate salts and
thiobenzophenones. The coexisting presence of CAO, C@O, NAH,
OH, CAOAC, C@S and S@O functional groups in the asphaltenes
confirms the fact that asphaltenes are composed of high molecular

Table 1
Assignment of plausible functional groups in the crude oil asphaltene fraction.
1
Sample and Wave number, cm Plausible functional Compound type
groups
Belema crude oil (Bond)Imo crude oil Eket crude oil
Asphaltene fraction Asphaltene fraction Asphaltene fraction
Asphaltene fraction Asphaltene fraction Asphaltene fraction
2920.60(s) stretch 2921.92(s) stretch 2921.43(s) stretch CAH (CH3) Alkanes
2870.47(s) stretch 2858.81(s) stretch 2870.68(s) stretch CAH (CH2)
3086.47(m) stretch 3086.68(m) stretch 3084.13(m) stretch CH Aromatic ring
729.00; 694.43(s) bend 728.44; 694.42(s) bend 728.95(s) bend CH Phenyl ring substitution bands
1604.59(w) stretch 1604.70(w) stretch 1604.63(w) stretch C@C Aromatic ring
1178.88; 1106.55; 1030.16; 1178.72; 1106.64; 1030.23; 1178.68;1106.62; 1030.18; CAO Alcohols, ethers, carboxylic acid,
1081.38(s) stretch 1081.44(s) stretch 1081.40(s) stretch esters
1736.11(s) stretch 1735.51(s) stretch 1735.71(s) stretch C@O Aldehydes, ketones, carboxylic
acids, esters
3584.05(s) stretch 3584.30(s) stretch 3584.13(s) stretch NAH Amide
2870.47; 2920.60(b) stretch 28.581; 2921.92(s) stretch 2870.68; 2921.43(s) stretch OH Carboxylic acid
1178.68(v) 1178.72(v) 1178.68(v) CAOAC Anhydrides
1030.16(s) stretch 1030.23(s) stretch 1030.18(s) stretch S@O Organic sulfoxides
1156.44(s) stretch 1156.57(s) stretch 1157.62(s) stretch Sulfate salt
1210.13(s) stretch 1210.17(s) stretch 1210.15(s) stretch C@S Thiobenzophenones

V = variable, m = medium, s = strong, b = broad and w = weak.

Fig. 2. IR spectrum of Belema crude oil asphaltene.

 F.M. Adebiyi, V. Thoss / Fuel 118 (2014) 426–431 429

(0.97 ± 0.38)
0.54–1.23
N (%)

Ndt
(80.79 ± 6.95)
72.98–86.29
C (%)

Ndt
(19.34 ± 1.97)

(4.41 ± 2.44)
17.23–21.13
Zn (mg/kg)

2.54–7.17
Fig. 3a. Frequency distribution of elemental concentrations of the asphaltene
fraction of crude oil samples from Belema oil field (C and N are given in%, while
others are given in mg/kg).

(34.18 ± 12.01)

(1.60 ± 1.70)
20.69–43.72
V (mg/kg)

0.18–3.47
(262.19 ± 21.52)
243.50–285.71

(9.04 ± 0.75)
8.18–9.54
S (mg/kg)

(40.83 ± 20.70)

(8.38 ± 5.68)
24.32–64.06

2.75–14.11
Ni (mg/kg)
Fig. 3b. Frequency distribution of elemental concentrations of the asphaltene
fraction of crude oil samples from Imo oil field (C and N are given in%, while others
are given in mg/kg).
Elemental composition and their ratios of the asphaltene fraction of Nigerian crude oil (± Standard deviation).

(1.44 ± 0.95)

(0.08 ± 0.02)
Mn (mg/kg)
0.35–2.01

0.06–0.10
(91.43 ± 4.95)

(7.78 ± 2.32)
86.29–96.16
Fe (mg/kg)

5.36–9.98
(2.65 ± 1.05)

(0.71 ± 0.32)
Cu (mg/kg)
Element (Range and mean)

1.94–3.85

0.38–1.02

Fig. 3c. Frequency distribution of elemental concentrations of the asphaltene

fraction of crude oil samples from Eket oil field (C and N are given in%, while others
are given in mg/kg).
(2.61 ± 0.91)

(0.39 ± 0.19)
Cr (mg/kg)
1.87–3.62

0.19–0.37

weight polycyclic constituents comprising of nitrogen, sulphur and

oxygen heteroatoms and are literally referred to as NSO com-
pounds [2,9,14].
The frequency distributions of the elemental concentrations of
Asphaltene component of Nigerian

the asphaltenes precipitated from the Nigerian crude oils obtained

from various oil fields are presented in Figs. 3a–3c) respectively.
Ten elements (Cr, Cu, Fe, Mn, Ni, S, V, Zn, C and N) were investi-
crude oil (this study)

gated and their concentrations determined. The range and mean

Nigerian crude oil [1]

concentrations of the elements are presented in Table 2. It is ob-

Ndt = not determined.

served from the frequency distributions and the Table 2 that C with
the range and mean values of 72.98–86.29% and 80.79 ± 6.95%
respectively has comparatively highest concentrations, followed
by N with the range value (0.54–1.23%) and mean value of
Study
Table 2

0.97 ± 0.38% which is also followed by S with a range value of

243.50–285.71 mg/kg and a mean value of 262.19 ± 21.52 mg/kg.
430 F.M. Adebiyi, V. Thoss / Fuel 118 (2014) 426–431
Table 3
Results of the T-test for comparison of the concentra-
tions of the analyzed elements in the Nigerian crude oil
and its asphaltene fraction.
Element Values
Cr 0.0230
Cu 0.0188
5
Fe 8.6743  10
Mn 0.0653
Ni 0.0521
S 0.0012
V 0.0220
Zn 0.0007
Values which were considered significant are in bold
type.
Fig. 4. Cross plot of the asphaltene fraction and crude oil using their mean
elemental concentrations (mg/kg) as variables.
Fig. 5. Cluster analysis of the analyzed elements in the crude oils.
This may be expected, since asphaltene contains high content of
high molecular weight heteroatoms viz; N, S and O compounds
and it is also a mixture of organic and hydrocarbons of various
molecular weights [14] as also indicated by the IR spectra. The
other analyzed elements (Cr, Cu, Fe, Mn, Ni, V and Zn) are present
at various detectable levels because asphaltene consists of high
content of porphyrins which can form stable complexes with the
transition metals to form organo-metalloporphyrins [14].
With respect to the analyzed elements, it is observed that
asphaltene obtained from Eket field crude oil has comparatively
P affinity.
highest Elemental Summation { (Element)} value of 87.47%, fol-
lowed by asphaltene obtained from Belema field crude oil
(84.39%) while asphaltene obtained from Imo field crude oil has
the least value (73.56%). This substantiates the earlier statement
made that asphaltene deposition will pose less problems during
transportation and production system of crude oils obtained from
Imo oil field than the other crude oils.
Table 2 also presents the comparison of the elemental concen-
trations of the asphaltenes in this study with the Nigerian crude
oils from which they were obtained [1]. The comparison indicates
that the values of all the elements are comparatively higher in the
asphaltenes than the crude oils. This may be due to the presence of
comparatively higher concentrations of porphyrins and heteroge-
neous NSO compounds in the asphaltenes than the crude oils
[14]. Comparison of concentrations of the analyzed elements in
the asphaltenes and crude oils using T-test values are presented
in Table 3. Those which were considered significant are in bold
type, and all the values are considered significant except values
for Mn (0.0653) and Ni (0.0521). The results thus indicate consid-
erable differences in the concentrations of the elements in the
asphaltenes and crude oils.
The result of the cross plot analysis between the asphaltenes
and crude oils using their mean elemental concentrations as
variables is presented in Fig. 4. It is observed that moderate and po-
sitive correlation (R2 = 0.53) exists between them, indicating inter-
element relationship between them. This confirms the expected
geochemical relationships between the asphaltenes fraction and
the crude oils.
Fig. 5 shows clustering analysis results for the analyzed ele-
ments. On the X-axis of the dendrogram is the similarity matrix
using Euclidean distance, while on the Y-axis are listed the ana-
lyzed elements. From the clustering analysis results, the gross ele-
mental association for the asphaltenes presents two groups viz; C
as a group and other elements (Cr, Cu, Mn, V, Zn, Ni, Fe, S and N)
as a group; but the two groups are also fairly correlated. As ex-
pected, the elements show very close clustering because all the
elements are known to associate with petroleum hydrocarbon for-
mation. Also, apart from N, S and C; other elements are transition
metals with similar chemical affinity.
4. Conclusion
This paper provides data on the chemical composition of the
asphaltene component of Nigerian crude oils in order to establish
its characteristics which can help in the developmental paths of
the natural resource. Samples of crude oil were collected from
three major oil fields in Nigeria. Comparison of the average content
of the Nigerian crude oils asphaltene with that of other nations
shows that asphaltene deposition may pose less problems during
Nigerian crude oil development than most of the crude oils from
other nations. Like crude oil asphaltenes from other parts of the
world, the analyzed crude oil asphaltenes are found to be mixtures
of alkanes, aromatic rings, phenyl rings, alcohols, ethers, carboxylic
acids, esters, aldehydes, ketones, anhydrides, organic sulphoxides,
sulphate salts and thiobenzophenones with substantial levels of
some transition metals. The analyzed elements are comparatively
higher in the asphaltenes than the crude oils and were supported
by their T-test values. Cross plot analysis between the asphaltenes
and crude oils using their elemental mean concentrations as
variables indicate moderate and positive correlation indicating in-
ter-element relationship between the crude oils and their asphal-
tene fraction. This confirms the expected geochemical
relationships between the asphaltenes fraction and the crude oils.
Elemental clustering analysis results present two groups which are
also fairly correlated, indicating similar sources and/or chemical
Acknowledgements
The authors sincerely acknowledge the support of Common-
wealth Scholarship Commission in the United Kingdom for
awarding Dr. F.M. Adebiyi an Academic Fellowship tenable and
hosted at School of Chemistry, Bangor University. We also wish
to acknowledge Dr. Anna Santoro and Joanthan Roberts for
facilitating the ICP-OES and C/N analyses respectively.
 F.M. Adebiyi, V. Thoss / Fuel 118 (2014) 426–431 431

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