Charactersation and Analytical Techniques in Crude Oil

7/31/2019 Charactersation and Analytical Techniques in Crude Oil

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By:Deep Chaudhari


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Characterization of crude oilPhysical propertiesThermal propertiesElectrical propertiesOptical properties

Chromatographic techniques

Spectroscopic methods (Principles andApplications of UV-Visible, IR, and NMRSpectroscopy)


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Petroleum exhibits a wide range of physical properties and severalrelationships can be made between various physical properties.Whereas properties such as viscosity, density, boiling point, andcolor of petroleum may vary widely, the ultimate or elementalanalysis varies, as already noted, over a narrow range for a largenumber of petroleum samples. The carbon content is relativelyconstant, while the hydrogen and heteroatom contents areresponsible for the major differences between petroleum samples.Coupled with the changes brought about to the feedstockconstituents by refinery operations, it is not surprising thatpetroleum characterization is a monumental task.


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Petroleum assay is an investigative (analytic) procedure

in laboratory for qualitatively assessing or quantitatively measuringthe presence or amount or the functional activity of a target entity(the analyte).

Thus, analyses are performed to determine whether each batch ofcrude oil received at the refinery is suitable for refining purposes.The tests are also applied to determine if there has been anycontamination during wellhead recovery, storage, or transportationthat may increase the processing difficulty (cost). The informationrequired is generally crude oil dependent or specific to a particularrefinery and is also a function of refinery operations and desired

product slate. To obtain the necessary information, two differentanalytical schemes are commonly used and these are: (1) aninspection assay and (2) a comprehensive assay


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Inspection assays usually involve determination of several key

bulk properties of petroleum (e.g., API gravity, sulfur content, pourpoint, and distillation range) as a means of determining if majorchanges in characteristics have occurred since the lastcomprehensive assay was performed.

On the other hand, the comprehensive (or full) assay is more

complex (as well as time consuming and costly) and is usuallyperformed only when a new field comes on stream, or when theinspection assay indicates that significant changes in the compositionof the crude oil have occurred. Except for these circumstances, acomprehensive assay of a particular crude oil stream may not beupdated for several years. A full petroleum assay may involve at least

determinations of (1) carbon residue yield, (2) density (specificgravity), (3) sulfur content, (4) distillation profile (volatility), (5)metallic constituents, (6) viscosity, and (7) pour point, as well as anytests designated necessary to understand the properties and behaviorof the crude oil under examination.


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Characterization of medium and heavy crude oils using thermalanalysis techniques :

This study focused on the characterization of heavy and mediumgrade crude oils in limestone matrix using differential scanningcalorimeter (DSC) and thermogravimetry (TG-DTG). DSC and TG-

DTG curves produced for two different crude oils+limestonemixtures indicate that the crude oil undergoes two majortransitions when subjected to an oxidizing and constant rateenvironment known as low- and high-temperature oxidation.Kinetic analysis in the low- and high-temperature oxidationregions were performed using two different kinetic methods.Throughout the study, it was observed that the activation energyvalues of the samples are varied between 2.4010.62 and 42.3181.9 kJ/mol in low- and high-temperature oxidation regionsrespectively.


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Refinery Coke

Vacuum Resid

Atmospheric Resid

Crude Oil

Gas Oil

Jet Fuel/Diesel

Gasoline

LPGAverage Carbon Number (Atoms per Molecule)

H

ydrogen/Carbon

AtomicRatio


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PetroleumFractions

HydrocarbonRange

Boiling Range (C) Boiling Range (F)

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

Gasoline (light and

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

Naphtha (light and

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

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


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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 generalnature, and perform an evaluation, of a feedstock.

Of the data that are available, the proportions of the elements in petroleumvary 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)


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VISCOSITY :

Viscosity is the force in dynes required to move a plane of 1 cm2 area at adistance 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:

=rrP/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.


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SURFACE AND INTERFACIAL TENSION :

Surface tension is a measure of the force acting at a boundary betweentwo phases. If the boundary is between a liquid and a solid or betweena liquid and a gas (air) the attractive forces are referred to as surface

tension, but the attractive forces between two immiscible liquids arereferred to as interfacial tension.

The values of surface tension vary over a narrow range ofapproximately 2438 dyne/cm for such widely diverse materials asgasoline (26 dyne/cm), kerosene (30 dyne/cm), and the lubricatingfractions (34 dyne/cm)


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VOLATILITY :

The volatility of a liquid or liquefied gas may be defined as itstendency to vaporize, that is, to change from the liquid to the vaporor gaseous state.

For some purposes, its necessary to have further more informationregarding vaporization.

The flash point of petroleum or a petroleum product is thetemperature to which the product must be heated under specifiedconditions to give off sufficient vapor to form a mixture with air that

can be ignited momentarily by a specified flame. The fire point is thetemperature to which the product must be heated under theprescribed conditions of the method to burn continuously when themixture of vapor and air is ignited by a specified flame.


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ANILINE POINT :

The aniline point of a liquid was originally defined as the consolute orcritical solution temperature of the two liquids, that is, the minimumtemperature at which they are miscible in all proportions. The term isnow most generally applied to the temperature at which exactlyequal 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.


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SPECIFIC HEAT :

Specific heat is defined as the quantity of heat required to raise aunit 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 60/600Fis d; thus, specific heat increases with temperature and decreases

with specific gravity.


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HEAT OF COMBUSTION :

The gross heats of combustion of crude oil and its products are givenwith fair accuracy by the equation:

Q= 12,400 -2100d2

where d is the 60/608F specific gravity. Deviation is generally lessthan 1%, although many highly aromatic crude oils show considerablyhigher values; the ranges for crude oil is 10,000 to 11,600 cal/g andthe heat of combustion of heavy oil and tar sand bitumen is

considerably higher.

Heats of combustion of petroleum gases may be calculated from theanalysis and data of the pure compounds.


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CONDUCTIVITY :

From the fragmentary evidence available, the electrical conductivity ofhydrocarbons is quite small. For example, the normal hydrocarbons (fromhexane up) have an electrical conductivity smaller than 1016 V/cm;benzene itself has an electrical conductivity of 4.4 1017 V/cm, andcyclohexane has an electrical conductivity of 7 1018 V/cm. It isgenerally recognized that hydrocarbons do not usually have an electrical

conductivity larger than 1018 V/cm. Thus, it is not surprising that theelectrical conductivity of hydrocarbon oils is also exceedingly small, ofthe order of 1019 to 1012 V/cm.Available data indicate that the observed conductivity is frequently moredependent on the method of measurement and the presence of traceimpurities than on the chemical type of the oil. Conduction through oils

is not ohmic; that is, the current is not proportional to field strength: insome regions it is observed to increase exponentially with the latter.Time effects are also observed, the current being at first relatively largeand decreasing to a smaller steady value. This is partly because ofelectrode polarization and partly because of ions removed from thesolution. Most oils increase in conductivity with rising temperatures.


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DIELECTRIC CONSTANT :

The dielectric constant, , of a substance may be defined as the ratioof the capacity of a condenser with the material between thecondenser plates C to that with the condenser empty and undervacuum C0:

=C/C0

The dielectric constant of petroleum and petroleum products may beused to indicate the presence of various constituents, such asasphaltenes, resins, or oxidized materials. Further, the dielectricconstant of petroleum products that are used in equipment, such ascondensers, may actually affect the electrical properties andperformance of that equipment. The dielectric constant of

hydrocarbons, and hence most crude oils and their products, is usuallylow and decreases with an increase in temperature. It is alsonoteworthy that for hydrocarbons, hydrocarbons fractions, andproducts, the dielectric constant is approximately equal to the squareof the refractive index. Polar materials have dielectric constantsgreater than the square of the refractive index.


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STATIC ELECTRIFICATION :

Dielectric liquids, particularly light naphtha, may acquire high staticcharges on flowing through or being sprayed from metal pipes. Theeffect seems to be associated with colloidally dispersedcontaminants, such as oxidation products, which can be removed bydrastic filtration or adsorption. Since a considerable fire hazard is

involved, a variety of methods have been studied for minimizing thedanger.For large-scale storage, avoidance of surface agitation and the useof floating metal roofs on tanks are beneficial. High humidity in thesurrounding atmosphere is helpful in lowering the static charge, andradioactive materials have been used to try to induce discharge to

ground. A variety of additives have been found that increase theconductivity of petroleum liquids, thus lowering the degree ofelectrification; chromium salts of alkylated salicylic acids and othersalts of alkylated sulfo-succinic acids are employed in lowconcentrations, say 0.005%.


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REFRACTIVE INDEX :

The refractive index is the ratio of the velocity of light in a vacuum to thevelocity of light in the substance. The measurement of the refractive index isvery simple, requires small quantities of material, and, consequently, has foundwide 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 petroleumand petroleum products. The refractive dispersion of a substance is defined asthe difference between its refractive indices at two specified wavelengths oflight. Two lines, commonly used to calculate dispersions are, the C (6563 , red)and F (4861 , blue) lines of the hydrogen spectrum. The specific dispersion isthe refractive dispersion divided by the density at the same temperature:

Specific dispersion =nFnC/dThis equation is of particular significance in petroleum chemistry because all thesaturated hydrocarbons, naphthene and paraffin, have nearly the same valueirrespective of molecular weight, whereas aromatics are much higher andunsaturated aliphatic hydrocarbons are intermediate.


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OPTICAL ACTIVITY :The occurrence of optical activity in petroleum is universal and is a generalphenomenon not restricted to a particular type of crude oil, such as the paraffinic ornaphthenic crude oils. Petroleum is usually dextrorotatory, that is, the plane ofpolarized 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 havebeen reported to be optically inactive. Examination of the individual fractions ofoptically active crude oils shows that the rotatory power increases with molecularweight (or boiling point) to pronounced maxima and then decreases again. The

rotatory power appears to be concentrated in certain fractions, the maximum lying ata molecular weight of about 350 to 400; this maximum is about the same for all crudeoils. The occurrence of optically active compounds in unaltered natural petroleum hasbeen a strong argument in favor of a rather low temperature origin of petroleum fromorganic raw materials.A magnetic field causes all liquids to exhibit optical rotation, usually in the samedirection as that of the magnetizing current; this phenomenon is known as theFaraday effect, and it may be expressed by the relation:

=pth is the total angle of rotation, t is the thickness of substance through which the lightpasses, and h is the magnetic field; the constant p is an intrinsic property of thesubstance, usually termed the Verdet constant (minutes of arc/cm per G); there havebeen some attempts to use the Verdet constant in studying the constitution ofhydrocarbons by physical property correlation.


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GAS CHROMATOGRAPHY :

Gasliquid chromatography (GLC) isa method for separating the volatilecomponents of various mixtures. Itis, in fact, a highly efficient

fractionating technique, and it isideally suited to the quantitativeanalysis of mixtures when thepossible components are known andthe interest lies only in determining

the amounts of each present.

A gas chromatograph with aheadspace sampler


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Thin layer chromatography(TLC) :

It is a chromatography technique used tomonitor the progress of a reaction, identifycompounds present in a given substance,determine the purity of a substance andseparate mixtures of compounds.

Thin layer chromatography is performed ona sheet of glass, plastic, or aluminum foil,which is coated with a thin layer ofadsorbent material, usually silica gel,aluminum oxide, or cellulose. This layer ofadsorbent is known as the stationary phase.TLC plate can be made by dissolving silicagel in chloroform or methanol and glassplate should be dip into that.

After that sample has been applied on theplate, a solvent or solvent mixture (knownas the mobile phase) is drawn up the platevia capillary action because differentcompounds run on the TLC plate atdifferent rates due to different polarity ofeach compound so that separation isachieved.

Separation of black ink on a TLCplate


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ION-EXCHANGE CHROMATOGRAPHY :

Ion-exchange chromatography is widely used in the analyses ofpetroleum fractions for the isolation and preliminary separation ofacid and basic components.

This technique has the advantage of greatly improving the quality ofa complex operation, but it can be a very time consumingseparation.

Cation-exchange chromatography is now used primarily to isolate thenitrogen constituents in a petroleum fraction

Anion-exchange chromatography is used to isolate the acidcomponents (such as carboxylic acids and phenols) from petroleumfractions.


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High-Performance LiquidChromatography(HPLC) :

HPLC, particularly in the normalphase mode, has found great utilityin separating different hydrocarbon

group types and identifying specificconstituent types.

The general advantages of high-performance liquid chromatographymethod are: (1) each sample isanalyzed as received; (2) the boilingrange of the sample is generallyimmaterial; (3) the total time peranalysis is usually of the order ofminutes; and (4) the method can beadapted for on-stream analysis.

A modern self contained HPLC.


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Column Chromatography :

Proteins are often fractionated bycolumn chromatography. A mixtureof proteins in solution is applied tothe top of a cylindrical column filled

with a permeable solid matriximmersed in solvent. A large amountof solvent is then pumped throughthe column. Because differentproteins are retarded to differentextents by their interaction with thematrix, they can be collectedseparately as they flow out from thebottom. According to the choice ofthe matrix, proteins can beseparated according to their charge,hydrophobicity, size or ability tobind to particular chemical groups.


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INFRARED SPECTROSCOPY :

Conventional infrared spectroscopy yields information about thefunctional features of various petroleum constituents. For example,infrared spectroscopy will aid in the identification of NH and OHfunctions, the nature of polymethylene chains, the CH out-of-placebending frequencies, and the nature of any polynuclear aromaticsystems.With the recent progress of Fourier transform infrared (FTIR)spectroscopy, quantitative estimates of the various functional groupscan also be made. This is particularly important for application tothe 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) paraffiniccharacter; (3) naphthenic character; (4) methyl group content; and(5) paraffin chain length.In conjunction with proton magnetic resonance, structuralparameters such as the fraction of paraffinic methyl groups to

aromatic methyl groups can be obtained.


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Absorption bands in IR

Spectroscopy


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Infrared Spectroscopy

Infrared Spectrum of Diethyl Ether


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NUCLEAR MAGNETIC RESONANCE(NMR) SPECTROSCOPY :

Nuclear magnetic resonance has frequently been employed forgeneral studies and for the structural studies of petroleumconstituents. In fact, proton magnetic resonance (PMR) studies (alongwith infrared spectroscopic studies) were, perhaps, the first studiesof the modern era that allowed structural inferences to be madeabout the polynuclear aromatic systems that occur in the highmolecular weight constituents of petroleum.

In general, the proton (hydrogen) types in petroleum fractions can be

subdivided into five types : (1) aromatic hydrogen; (2) substitutedhydrogen next to an aromatic ring; (3) naphthenic hydrogen; (4)methylene hydrogen; and (5) terminal methyl hydrogen remote froman aromatic ring. Other ratios are also derived from which a series ofstructural parameters can be calculated.


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Example 1H NMR spectrum of ethanol plotted as signal intensity vs. chemicalshift. There are three different types of H atoms in ethanol regarding NMR. Thehydrogen (H) on the -OH group is not coupling with the other H atoms andappears as a singlet, but the CH3- and the -CH2- hydrogens are coupling with each

other, resulting in a triplet and quartet respectively.


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MASS SPECTROMETRY :

Mass spectrometry can play a key role in the identification of theconstituents of feedstocks and products.

The principal advantages of mass spectrometric methods are: (1) highreproducibility of quantitative analyses; (2) the potential forobtaining detailed data on the individual components and carbonnumber homologues in complex mixtures; and (3) a minimal samplesize is required for analysis. The ability of mass spectrometry toidentify individual components in complex mixtures is unmatched byany modern analytical technique. Perhaps, the exception is gaschromatography.

However, there are disadvantages arising from the use of massspectrometry and these are: (1) the limitation of the method toorganic materials that are volatile and stable at temperatures up to3000C (5700F); and (2) the difficulty of separating isomers forabsolute identification. The sample is usually destroyed, but this is

seldom a disadvantage.


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Schematics of a simple mass spectrometer with sector typemass analyzer. This one is for the measurement of carbondioxide isotope ratios (IRMS) as in the carbon-13 urea breath

test


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Mass spectrum of a peptide showing the isotopic distribution


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ULTRAVIOLETVISIBLE SPECTROSCOPY :

Ultravioletvisible spectroscopy (UV-Vis) refers to absorptionspectroscopy or reflectance spectroscopy in the ultraviolet-visiblespectral region. This means it uses light in the visible and adjacent

(near-UV and near-infrared (NIR)) ranges. The absorption orreflectance in the visible range directly affects the perceived color ofthe chemicals involved. In this region of the electromagneticspectrum, molecules undergo electronic transitions.

UV/Vis spectroscopy is routinely used in analytical chemistry for the

quantitative determination of different analytes, such as transitionmetal ions, highly conjugated organic compounds, and biologicalmacromolecules. Spectroscopic analysis is commonly carried out insolutions but solids and gases may also be studied.


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An Example of an UV-Vis sample readout.


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Charactersation and Analytical Techniques in Crude Oil

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