Characterization of crude oil

Physical properties
Thermal properties
Electrical properties
Optical properties
Chromatographic techniques
Spectroscopic methods (Principles and
Applications of UV-Visible, IR, and NMR
Spectroscopy)
Petroleum exhibits a wide range of physical properties and several
relationships can be made between various physical properties.
Whereas properties such as viscosity, density, boiling point, and
color of petroleum may vary widely, the ultimate or elemental
analysis varies, as already noted, over a narrow range for a large
number of petroleum samples. The carbon content is relatively
constant, while the hydrogen and heteroatom contents are
responsible for the major differences between petroleum samples.
Coupled with the changes brought about to the feedstock
constituents by refinery operations, it is not surprising that
petroleum characterization is a monumental task.
Petroleum assay is an investigative (analytic) procedure
in laboratory for qualitatively assessing or quantitatively measuring
the presence or amount or the functional activity of a target entity
(the analyte).
Thus, analyses are performed to determine whether each batch of
crude oil received at the refinery is suitable for refining purposes.
The tests are also applied to determine if there has been any
contamination during wellhead recovery, storage, or transportation
that may increase the processing difficulty (cost). The information
required is generally crude oil dependent or specific to a particular
refinery and is also a function of refinery operations and desired
product slate. To obtain the necessary information, two different
analytical schemes are commonly used and these are: (1) an
inspection assay and (2) a comprehensive assay
Inspection assays usually involve determination of several key
bulk properties of petroleum (e.g., API gravity, sulfur content, pour
point, and distillation range) as a means of determining if major
changes in characteristics have occurred since the last
comprehensive assay was performed.
On the other hand, the comprehensive (or full) assay is more
complex (as well as time consuming and costly) and is usually
performed only when a new field comes on stream, or when the
inspection assay indicates that significant changes in the composition
of the crude oil have occurred. Except for these circumstances, a
comprehensive assay of a particular crude oil stream may not be
updated for several years. A full petroleum assay may involve at least
determinations of (1) carbon residue yield, (2) density (specific
gravity), (3) sulfur content, (4) distillation profile (volatility), (5)
metallic constituents, (6) viscosity, and (7) pour point, as well as any
tests designated necessary to understand the properties and behavior
of the crude oil under examination.
Recommended Inspection Data Required for Petroleum and Heavy Feedstocks (Including Residua)
Petroleum Heavy Feedstocks
Density, specific gravity Density, specific gravity
API gravity API gravity
Carbon, wt.% Carbon, wt.%
Hydrogen, wt.% Hydrogen, wt.%
Nitrogen, wt.% Nitrogen, wt.%
Sulfur, wt.% Sulfur, wt.%
-Nickel, ppm
-Vanadium, ppm
-Iron, ppm
Pour point Pour point
Wax content
-Wax appearance temperature
Viscosity (various temperatures) Viscosity (various temperatures)
Carbon residue of residuum Carbon residue
-Ash, wt.%
Distillation profile: Fractional composition:
-All fractions plus vacuum residue -Asphaltenes, wt.%
-Resins, wt.%
-Aromatics, wt.%
-Saturates, wt.%
Characterization of medium and heavy crude oils using thermal
analysis techniques :

This study focused on the characterization of heavy and medium

grade crude oils in limestone matrix using differential scanning
calorimeter (DSC) and thermogravimetry (TG-DTG). DSC and TG-
DTG curves produced for two different crude oils+limestone
mixtures indicate that the crude oil undergoes two major
transitions when subjected to an oxidizing and constant rate
environment known as low- and high-temperature oxidation.
Kinetic analysis in the low- and high-temperature oxidation
regions were performed using two different kinetic methods.
Throughout the study, it was observed that the activation energy
values of the samples are varied between 2.40–10.62 and 42.3–
181.9 kJ/mol in low- and high-temperature oxidation regions
respectively.
 Refinery Coke
Hydrogen/Carbon Atomic Ratio

Vacuum Resid

Atmospheric Resid

Crude Oil

Gas Oil

Jet Fuel/Diesel

Gasoline

LPG
Average Carbon Number (Atoms per Molecule)
 Petroleum Hydrocarbon
Boiling Range (°C) Boiling Range (°F)
Fractions Range

Light gases C2-C4 -90 ~ 1 -130 ~ 30

Gasoline (light and

C4-C10 -1 ~ 200 30 ~ 390
heavy)

Naphtha (light and

C4-C11 -1 ~ 205 30 ~ 400
heavy)

Jet fuels C9-C14 150 ~ 225 300 ~ 490

Kerosene C11-C14 205 ~ 225 400 ~ 490
Diesel fuel C11-C16 205 ~ 290 400 ~ 550
Light gas oil C14-C18 255 ~ 315 490 ~ 600
Heavy gas oil C18-C28 315 ~ 425 600 ~ 800
Wax C18-C26 315 ~ 500 600 ~ 930
Lubricating oil >C25 >400 >750
Vacuum gas oil C28-C55 425 ~ 600 800 ~ 1100
Residuum >C55 >600 >1100
ELEMENTAL (ULTIMATE ) ANALYSIS :
The analysis of petroleum for the percentages of carbon, hydrogen, nitrogen,
oxygen, and sulfur is perhaps the first method used to examine the general
nature, and perform an evaluation, of a feedstock.

Of the data that are available, the proportions of the elements in petroleum
vary only slightly over narrow limits:
• Carbon 83.0 to 87.0%
• Hydrogen 10.0 to 14.0%
• Nitrogen 0.1 to 2.0%
• Oxygen 0.05 to 1.5%
• Sulfur 0.05 to 6.0%
• Metals (Ni and V) <1000 ppm
DENSITY AND SPECIFIC GRAVITY :

The density and specific gravity of crude oil are two properties that have
found wide use in the industry for preliminary assessment of the character and
quality of crude oil.

Density, specific gravity, or API gravity may be measured by means of a

hydrometer, a pycnometer, by the displacement method, or by means of a
digital density meter and a digital density analyzer.

The specific gravity of petroleum usually ranges from about 0.8 (45.30 API) for
the lighter crude oils to over 1.0 (less than 100 API) for heavy crude oil and
bitumen.

One percent by weight solids in the sample can raise the density by 0.007
g/cm3.
VISCOSITY :
Viscosity is the force in dynes required to move a plane of 1 cm2 area at a
distance of 1 cm from another plane of 1 cm2 area through a distance of 1 cm
in 1 sec.

Viscosity is derived from the equation:

µ=πrrP/8nl,
where r is the tube radius, l the tube length, P the pressure difference
between the ends of a capillary, n the coefficient of viscosity, and m the
quantity discharged in unit time.

In the early days of the petroleum industry, viscosity was regarded as the body
of petroleum, a significant number for lubricants or for any liquid pumped or
handled in quantity.
SURFACE AND INTERFACIAL TENSION :

Surface tension is a measure of the force acting at a boundary between

two phases. If the boundary is between a liquid and a solid or between
a liquid and a gas (air) the attractive forces are referred to as surface
tension, but the attractive forces between two immiscible liquids are
referred to as interfacial tension.

The values of surface tension vary over a narrow range of

approximately 24–38 dyne/cm for such widely diverse materials as
gasoline (26 dyne/cm), kerosene (30 dyne/cm), and the lubricating
fractions (34 dyne/cm)
VOLATILITY :

The volatility of a liquid or liquefied gas may be defined as its

tendency to vaporize, that is, to change from the liquid to the vapor
or gaseous state.
For some purposes, its necessary to have further more information
regarding vaporization.
The flash point of petroleum or a petroleum product is the
temperature to which the product must be heated under specified
conditions to give off sufficient vapor to form a mixture with air that
can be ignited momentarily by a specified flame. The fire point is the
temperature to which the product must be heated under the
prescribed conditions of the method to burn continuously when the
mixture of vapor and air is ignited by a specified flame.
ANILINE POINT :

The aniline point of a liquid was originally defined as the consolute or

critical solution temperature of the two liquids, that is, the minimum
temperature at which they are miscible in all proportions. The term is
now most generally applied to the temperature at which exactly
equal parts of the two are miscible.

For oils of a given type, it increases slightly with molecular weight;

for those of given molecular weight it increases rapidly with
increasing paraffinic character.
SPECIFIC HEAT :

Specific heat is defined as the quantity of heat required to raise a

unit mass of material through one degree of temperature.

It can be given by this general equation:

C = 1/d (0:388 + 0:00045t)
C is the specific heat at t0F of an oil whose specific gravity 60/600F
is d; thus, specific heat increases with temperature and decreases
with specific gravity.
HEAT OF COMBUSTION :

The gross heats of combustion of crude oil and its products are given
with fair accuracy by the equation:
Q = 12,400 - 2100d2

where d is the 60/608F specific gravity. Deviation is generally less

than 1%, although many highly aromatic crude oils show considerably
higher values; the ranges for crude oil is 10,000 to 11,600 cal/g and
the heat of combustion of heavy oil and tar sand bitumen is
considerably higher.

Heats of combustion of petroleum gases may be calculated from the

analysis and data of the pure compounds.
CONDUCTIVITY :

From the fragmentary evidence available, the electrical conductivity of

hydrocarbons is quite small. For example, the normal hydrocarbons (from
hexane up) have an electrical conductivity smaller than 1016 V/cm;
benzene itself has an electrical conductivity of 4.4 1017 V/cm, and
cyclohexane has an electrical conductivity of 7 1018 V/cm. It is
generally recognized that hydrocarbons do not usually have an electrical
conductivity larger than 1018 V/cm. Thus, it is not surprising that the
electrical conductivity of hydrocarbon oils is also exceedingly small, of
the order of 1019 to 1012 V/cm.
Available data indicate that the observed conductivity is frequently more
dependent on the method of measurement and the presence of trace
impurities than on the chemical type of the oil. Conduction through oils
is not ohmic; that is, the current is not proportional to field strength: in
some regions it is observed to increase exponentially with the latter.
Time effects are also observed, the current being at first relatively large
and decreasing to a smaller steady value. This is partly because of
electrode polarization and partly because of ions removed from the
solution. Most oils increase in conductivity with rising temperatures.
DIELECTRIC CONSTANT :

The dielectric constant, ε, of a substance may be defined as the ratio

of the capacity of a condenser with the material between the
condenser plates C to that with the condenser empty and under
vacuum C0:
ε = C/C0
The dielectric constant of petroleum and petroleum products may be
used to indicate the presence of various constituents, such as
asphaltenes, resins, or oxidized materials. Further, the dielectric
constant of petroleum products that are used in equipment, such as
condensers, may actually affect the electrical properties and
performance of that equipment. The dielectric constant of
hydrocarbons, and hence most crude oils and their products, is usually
low and decreases with an increase in temperature. It is also
noteworthy that for hydrocarbons, hydrocarbons fractions, and
products, the dielectric constant is approximately equal to the square
of the refractive index. Polar materials have dielectric constants
greater than the square of the refractive index.
STATIC ELECTRIFICATION :

Dielectric liquids, particularly light naphtha, may acquire high static

charges on flowing through or being sprayed from metal pipes. The
effect seems to be associated with colloidally dispersed
contaminants, such as oxidation products, which can be removed by
drastic filtration or adsorption. Since a considerable fire hazard is
involved, a variety of methods have been studied for minimizing the
danger.
For large-scale storage, avoidance of surface agitation and the use
of floating metal roofs on tanks are beneficial. High humidity in the
surrounding atmosphere is helpful in lowering the static charge, and
radioactive materials have been used to try to induce discharge to
ground. A variety of additives have been found that increase the
conductivity of petroleum liquids, thus lowering the degree of
electrification; chromium salts of alkylated salicylic acids and other
salts of alkylated sulfo-succinic acids are employed in low
concentrations, say 0.005%.
REFRACTIVE INDEX :

The refractive index is the ratio of the velocity of light in a vacuum to the
velocity of light in the substance. The measurement of the refractive index is
very simple, requires small quantities of material, and, consequently, has found
wide use in the characterization of hydrocarbons and petroleum samples.
The refractive and specific dispersion, as well as the molecular and specific
refraction, have all been advocated for use in the characterization of petroleum
and petroleum products. The refractive dispersion of a substance is defined as
the difference between its refractive indices at two specified wavelengths of
light. Two lines, commonly used to calculate dispersions are, the C (6563 Å, red)
and F (4861 Å, blue) lines of the hydrogen spectrum. The specific dispersion is
the refractive dispersion divided by the density at the same temperature:
Specific dispersion = nF – nC/d
This equation is of particular significance in petroleum chemistry because all the
saturated hydrocarbons, naphthene and paraffin, have nearly the same value
irrespective of molecular weight, whereas aromatics are much higher and
unsaturated aliphatic hydrocarbons are intermediate.
OPTICAL ACTIVITY :
The occurrence of optical activity in petroleum is universal and is a general
phenomenon not restricted to a particular type of crude oil, such as the paraffinic or
naphthenic crude oils. Petroleum is usually dextrorotatory, that is, the plane of
polarized light is rotated to the right, but there are known leavo-rotatory crude oils,
that is, the plane of polarized light is rotated to the left, and some crude oils have
been reported to be optically inactive. Examination of the individual fractions of
optically active crude oils shows that the rotatory power increases with molecular
weight (or boiling point) to pronounced maxima and then decreases again. The
rotatory power appears to be concentrated in certain fractions, the maximum lying at
a molecular weight of about 350 to 400; this maximum is about the same for all crude
oils. The occurrence of optically active compounds in unaltered natural petroleum has
been a strong argument in favor of a rather low temperature origin of petroleum from
organic raw materials.
A magnetic field causes all liquids to exhibit optical rotation, usually in the same
direction as that of the magnetizing current; this phenomenon is known as the
Faraday effect, θ and it may be expressed by the relation:
θ = pth
θ is the total angle of rotation, t is the thickness of substance through which the light
passes, and h is the magnetic field; the constant p is an intrinsic property of the
substance, usually termed the Verdet constant (minutes of arc/cm per G); there have
been some attempts to use the Verdet constant in studying the constitution of
hydrocarbons by physical property correlation.
GAS CHROMATOGRAPHY :

Gas–liquid chromatography (GLC) is

a method for separating the volatile
components of various mixtures. It
is, in fact, a highly efficient
fractionating technique, and it is
ideally suited to the quantitative
analysis of mixtures when the
possible components are known and
the interest lies only in determining
the amounts of each present.

A gas chromatograph with a

headspace sampler
Thin layer chromatography
(TLC) :

It is a chromatography technique used to

monitor the progress of a reaction, identify
compounds present in a given substance,
determine the purity of a substance and
separate mixtures of compounds.
Thin layer chromatography is performed on
a sheet of glass, plastic, or aluminum foil,
which is coated with a thin layer of
adsorbent material, usually silica gel,
aluminum oxide, or cellulose. This layer of
adsorbent is known as the stationary phase.
TLC plate can be made by dissolving silica
gel in chloroform or methanol and glass
plate should be dip into that.
After that sample has been applied on the
plate, a solvent or solvent mixture (known
as the mobile phase) is drawn up the plate
via capillary action because different
compounds run on the TLC plate at
different rates due to different polarity of
each compound so that separation is Separation of black ink on a TLC
achieved.
plate
ION-EXCHANGE CHROMATOGRAPHY :

Ion-exchange chromatography is widely used in the analyses of

petroleum fractions for the isolation and preliminary separation of
acid and basic components.
This technique has the advantage of greatly improving the quality of
a complex operation, but it can be a very time consuming
separation.
Cation-exchange chromatography is now used primarily to isolate the
nitrogen constituents in a petroleum fraction
Anion-exchange chromatography is used to isolate the acid
components (such as carboxylic acids and phenols) from petroleum
fractions.
High-Performance Liquid
Chromatography(HPLC) :

HPLC, particularly in the normal

phase mode, has found great utility
in separating different hydrocarbon
group types and identifying specific
constituent types.
The general advantages of high-
performance liquid chromatography
method are: (1) each sample is
analyzed as received; (2) the boiling
range of the sample is generally
immaterial; (3) the total time per
analysis is usually of the order of
minutes; and (4) the method can be
adapted for on-stream analysis.
A modern self contained HPLC.
Column Chromatography :

Proteins are often fractionated by

column chromatography. A mixture
of proteins in solution is applied to
the top of a cylindrical column filled
with a permeable solid matrix
immersed in solvent. A large amount
of solvent is then pumped through
the column. Because different
proteins are retarded to different
extents by their interaction with the
matrix, they can be collected
separately as they flow out from the
bottom. According to the choice of
the matrix, proteins can be
separated according to their charge,
hydrophobicity, size or ability to
bind to particular chemical groups.
INFRARED SPECTROSCOPY :

Conventional infrared spectroscopy yields information about the

functional features of various petroleum constituents. For example,
infrared spectroscopy will aid in the identification of N–H and O–H
functions, the nature of polymethylene chains, the C–H out-of-place
bending frequencies, and the nature of any polynuclear aromatic
systems.
With the recent progress of Fourier transform infrared (FTIR)
spectroscopy, quantitative estimates of the various functional groups
can also be made. This is particularly important for application to
the higher molecular weight solid constituents of petroleum (i.e.,
the asphaltene fraction). It is also possible to derive structural
parameters from infrared spectroscopic data and these are: (1)
saturated hydrogen to saturated carbon ratio; (2) paraffinic
character; (3) naphthenic character; (4) methyl group content; and
(5) paraffin chain length.
In conjunction with proton magnetic resonance, structural
parameters such as the fraction of paraffinic methyl groups to
aromatic methyl groups can be obtained.
Absorption bands in IR
Spectroscopy
Infrared Spectroscopy

Infrared Spectrum of Diethyl Ether

NUCLEAR MAGNETIC RESONANCE(NMR) SPECTROSCOPY :

Nuclear magnetic resonance has frequently been employed for

general studies and for the structural studies of petroleum
constituents. In fact, proton magnetic resonance (PMR) studies (along
with infrared spectroscopic studies) were, perhaps, the first studies
of the modern era that allowed structural inferences to be made
about the polynuclear aromatic systems that occur in the high
molecular weight constituents of petroleum.
In general, the proton (hydrogen) types in petroleum fractions can be
subdivided into five types : (1) aromatic hydrogen; (2) substituted
hydrogen next to an aromatic ring; (3) naphthenic hydrogen; (4)
methylene hydrogen; and (5) terminal methyl hydrogen remote from
an aromatic ring. Other ratios are also derived from which a series of
structural parameters can be calculated.
Example 1H NMR spectrum of ethanol plotted as signal intensity vs. chemical
shift. There are three different types of H atoms in ethanol regarding NMR. The
hydrogen (H) on the -OH group is not coupling with the other H atoms and
appears as a singlet, but the CH3- and the -CH2- hydrogens are coupling with each
other, resulting in a triplet and quartet respectively.
MASS SPECTROMETRY :

Mass spectrometry can play a key role in the identification of the

constituents of feedstocks and products.
The principal advantages of mass spectrometric methods are: (1) high
reproducibility of quantitative analyses; (2) the potential for
obtaining detailed data on the individual components and carbon
number homologues in complex mixtures; and (3) a minimal sample
size is required for analysis. The ability of mass spectrometry to
identify individual components in complex mixtures is unmatched by
any modern analytical technique. Perhaps, the exception is gas
chromatography.
However, there are disadvantages arising from the use of mass
spectrometry and these are: (1) the limitation of the method to
organic materials that are volatile and stable at temperatures up to
3000C (5700F); and (2) the difficulty of separating isomers for
absolute identification. The sample is usually destroyed, but this is
seldom a disadvantage.
Schematics of a simple mass spectrometer with sector type
mass analyzer. This one is for the measurement of carbon
dioxide isotope ratios (IRMS) as in the carbon-13 urea breath
test
Mass spectrum of a peptide showing the isotopic distribution
ULTRAVIOLET–VISIBLE SPECTROSCOPY :

Ultraviolet–visible spectroscopy (UV-Vis) refers to absorption

spectroscopy or reflectance spectroscopy in the ultraviolet-visible
spectral region. This means it uses light in the visible and adjacent
(near-UV and near-infrared (NIR)) ranges. The absorption or
reflectance in the visible range directly affects the perceived color of
the chemicals involved. In this region of the electromagnetic
spectrum, molecules undergo electronic transitions.
UV/Vis spectroscopy is routinely used in analytical chemistry for the
quantitative determination of different analytes, such as transition
metal ions, highly conjugated organic compounds, and biological
macromolecules. Spectroscopic analysis is commonly carried out in
solutions but solids and gases may also be studied.
An Example of an UV-Vis sample readout.
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