INTRODUCTION TO

PETROLEUM REFINING &

TEST METHODS

CH 9029 –PETROLEUM REFINING AND PETROCHEMICALS

Dept of Chemical Engineering.
A.C.Tech, Anna University.
 PETROLEUM

Petroleum is a complex mixture of hydrocarbons that occur in

the sedimentary rocks in the form of gases (natural gas),
liquids (crude oil), semisolids (bitumen), or solids (wax or
asphaltite).

An underground reservoir that contains hydrocarbons is called

petroleum reservoir and its hydrocarbon contents that can be
recovered through a producing well is called reservoir fluid.

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 PETROLEUM

Generally, hydrocarbons are divided into four groups:

paraffins, olefins, naphthenes and aromatics.
Paraffins
Also called alkanes and have the general formula of CnH2n+2,
where n is the number of carbon atoms. Paraffins from C1 to
C40 usually appear in crude oil and represent up to 20% of
crude by volume. Since paraffins are fully saturated (no double
bond), they are stable and remain unchanged over long periods
of geological time.
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 GENERAL PROPERTIES OF PARAFFINS

Higher paraffins are insoluble in water. Though the lower ones

are soluble in ethers and alcohols.

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 GENERAL PROPERTIES OF PARAFFINS

Paraffins upto 3 carbon atoms have inclination to form

hydrates such as CH4. 7H2O, C2H6.7H2O and these hydrates
offer clogging and corrosion difficulties. Hence drying is
essential before usage.
Higher paraffins > C20 are prone to oxidation
Specific gravity of the series increases with molecular weight,
still paraffins have less specific gravity and boiling point than
aromatics.

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 GENERAL PROPERTIES OF PARAFFINS

Viscosity of paraffins is less , smoke point is very high with

poor illuminating characteristics.
Pour point of the paraffins is usually high (difficulty in
transportation and storage)
Isomers differes from n-paraffins by having slight low boiling
points, low pour points, high viscosity and viscosity index.
i-paraffins are more reactives than n-paraffins but burn like n-
paraffins without much illumination and smoking.

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 OLEFINS

Olefins are another series of noncyclic hydrocarbons but they

are unsaturated and have at least one double bond between
carbon-carbon atoms. Compounds with one double bond are
called monoolefins or alkenes. Monoolefins have a general
formula of CnH2n.

Olefins are uncommon in crude oils due to their reactivity with

hydrogen that makes them saturated; however, they can be
produced in refineries through cracking reactions.

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 OLEFINS

The absence of unsaturates to a large extent can be judged by

the probable catalytic activity of the earth’s crest in converting
unsaturates to saturates and ring structures.

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 NAPHTHENES

Naphthenes or cycloalkanes are ring or cyclic saturated

hydrocarbons with the general formula of CnH2n. Cyclopentane
(C5H10), cyclohexane (C6H12), and their derivatives such as n-
alkylcyclopentanes are normally found in crude oils.

Thermodynamic studies show that naphthene rings with five

and six carbon atoms are the most stable naphthenic
hydrocarbons. The content of cycloparaffins in petroleum may
vary up to 60%.
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 AROMATICS
Aromatics are an important series of hydrocarbons found in
almost every petroleum mixture from any part of the world.
Aromatics are cyclic but unsaturated hydrocarbons that begin
with benzene molecule (C6H6) and contain carbon-carbon
double bonds.

Some of the common aromatics found in petroleum and crude

oils are benzene and its derivatives with attached methyl, ethyl,
propyl, or higher alkyl groups. This series of aromatics is
called alkylbenzenes and have a general formula of CnH2n-6
(where n ≥ 6). CH 9029 PRPC
 AROMATICS
• Eventhough benzene is unsaturated, yet it follows the prinicple
of substitution with halogens rather than addition. This is
mainly due to symmetric grouping of closed ring structure and
resonance.

• Aromatics are usually having high boiling points, low pour

points, high octane number, high viscosity and high viscosity
index.

• In petroleum fractions aromatics beyond 3 – ring structure

(Anthracenes ) are probably non – existent.
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 SULFUR CONTENT

Sulfur is the most important heteroatom in petroleum and it

can be found in cyclic as well as noncyclic compounds such as

mercaptanes (R-S-H) and sulfides (R-S-R’), where R and R’ are

alkyl groups.

Sulfur in natural gas is usually found in the form of hydrogen

sulfide (H2S). Some natural gas contain H2S as high as 30% by

volume. The amount of sulfur in a crude may vary from 0.05

to 6% by weight.
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 OXYGEN AND NITROGEN

Oxygen and nitrogen do not occur in free state either in crude

or in fractions. Nitrogen presence in free form is well known
in natural gas only.

Oxygen occurs as oxygenated compounds like phenols,

cresols, napthenic acids, sulphonates, sulphates and sulfoxides.

Nitrogen compounds gives problems in processing and

stability of products. Catalytic deactivation or poisoning, gum
formation are some of the offshoots of nitrogen.
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 LESS INORGANICS

The other element present in crude are nickel, vanadium, iron,

silica, sodium, magnesium and halogens,etc.,

The ash formation is mainly due to the metal and inorganic

content.

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 GAS-TO-OIL RATIO

The most important characteristic of a reservoir fluid in

addition to specific gravity (or API gravity) is its gas-to-oil
ratio (GOR), which represents the amount of gas produced at
SC in standard cubic feet (scf) to the amount of liquid oil
produced at the SC in stock tank barrel (stb). Generally,
reservoir fluids are black oil, volatile oil, gas condensate, wet
gas, and dry gas.

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 CRUDE OIL

The crude oil produced from the atmospheric separator has a

composition different from the reservoir fluid from a
producing well. Two important characterisitics of a crude that
determine its quality are the API gravity (specific gravity) and
the sulfur content.

If the sulfur content of a crude is less than 0.5 wt% it is called

a sweet oil.

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 API GRAVITY

Crude oil is classified as light, medium or heavy, according to

its measured API gravity.

1. Light crude oil is defined as having API gravity higher than

31.1 °API.
2. Medium oil is defined as having API gravity between 22.3
°API and 31.1 °API.
3. Heavy oil is defined as having API gravity below 22.3 °API.

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API GRAVITY - DIAGRAM

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 UOP – K FACTOR
The Watson characterization factor (Kw) is one of the
oldest characterization factors originally defined by
Watson et al. of the Universal Oil Products (UOP) in
mid 1930s. For this reason the parameter is sometimes
called UOP characterization factor and is defined as

Tb1/ 3
Kw  where Tb  normal boiling point oR
SG
The naphthenic hydrocarbons have Kw values between
paraffinic and aromatic compounds. In general,
aromatics have low Kw values while paraffins have high
values.
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 PETROLEUM FRACTIONS

Some of the petroleum fractions produced from distillation

columns with their boiling point ranges are given in Table
below. These fractions may go through further processes to
produce desired products.

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 PETROLEUM STANDARDS

There are a number of international standard organizations that

recommend specific characteristics or standard measuring
techniques for various petroleum products. Some of these
organizations are as follows:
1. ASTM (American Society for Testing and Materials) in the
United States
2. ISO (International Organization for Standardization), which
is at the international level
3. IP (Institute of Petroleum) in the United Kingdom
4. API (American Petroleum Institute) in the United States

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 CRUDE

Distillation of crude yields number of cuts of varying boiling

ranges. In order of increasing boiling points , the main
fractionation from distillation of crude,

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 GAS

Gas from petroleum is classified under several names like

 Natural Gas,

 Associated Gas,

 Dissolved Gas ,

 Casing Head Gas

 Off Gas From Refinery

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 LIQUEFIED PETROLEUM GAS

This is a mixture of propane and butane, two hydrocarbons

which are gaseous at atmospheric pressure but liquid if higher
pressure is applied.

They are obtained from natural gas at natural gasoline plants

and also from refinery gases.

A large volume of the gas can be compressed into a small

volume of liquid, simplifying handling problems.

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 LIQUEFIED PETROLEUM GAS

Liquefied petroleum gas, or "bottled gas" as it is sometimes

known, is an important domestic fuel in rural communities and
even in small communities which have a central distributing
system, where the LP-Gas is supplied consumers through the
gas lines.

LP-Gas is also widely used as an intermediate material in

petrochemical manufacturing,

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 LIQUEFIED PETROLEUM GAS

The propane and butane constituents of liquefied petroleum

gas are obtained from natural gas at natural gasoline plants and
also from gases produced at refineries when crude oil is
processed.
The propane and butane hydrocarbons are separated from the
gas stream by distillation. The presence of ethane is avoided
because this light hydrocarbon does not liquefy under pressure
at atmospheric temperatures.

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 LIQUEFIED PETROLEUM GAS

If the LP-Gas contains pentane, a liquid hydrocarbon heavier

than butane, this component may separate in a liquid state in
the gas lines

Natural gas and natural gasoline contain no unsaturated

hydrocarbons, but these may be present in refinery gas
streams. The unsaturated hydrocarbons have a tendency to
polymerize and form gummy deposits, making their presence
undesirable in liquefied petroleum gas.

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 LIQUEFIED PETROLEUM GAS

Care is taken by manufacturers to keep the propane and butane

free of hydrogen sulfide, which is corrosive and on burning
produces sulfur dioxide, a gas having a pungent odor.

However, a minute quantity of ethyl mercaptan, a sulfur

compound having an exceptionally strong and disagreeable
odor, is added to the odorless propane and butane to warn the
customer of gas leaks.

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 TEST METHOD FOR LPG

Reid vapor pressure

This test is also the standard
test for low boiling point
distillates.
It is used for naphthas,
gasolines, light cracked
distillates and aviation
gasolines.

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 REID VAPOR PRESSURE

In the diagram A represents the vapor chamber which has a

length of 254 mm and a diameter of 51 mm. The ratio of the
volume of the vapor chamber A to the liquid chamber B shall
be between 3.8 and 4.2. The diameters of both the vapor
chamber and the liquid chamber shall be the same. The liquid
test sample is placed in the liquid chamber to fill the vessel.
The liquid chamber is then connected to the vapor chamber

and the pressure gage inserted as shown in the diagram.

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 REID VAPOR PRESSURE

The assembled apparatus is then immersed vertically in a

water bath up to a level of 190 mm of the vapor chamber. The
water bath is kept at a temperature of 100◦F for 30 min and
then removed tilted once or twice and replaced for a further 15
min. At the end of this time the vapor pressure of the test
sample is read from the pressure gage to the nearest 0.2 psi.

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REID VAPOR PRESSURE

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 GASOLINE

Naptha or gasoline is the next fraction to follow gas.

This is a volatile fraction and is known as motor spirit.

The boiling ranges from 37 °C to 180°C.

Gasoline is a finished product , while raw fraction is termed as

naptha or light boiling fractions.

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 THE PARAMETERS OF GASOLINE

Parameters affecting engine performance

The following parameters are the major criteria in the

production of finished gasoline with respect to its
performance. These are:
 Octane number
 Thermal efficiency
 Volatility of the gasoline
 Engine deposits
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 TESTS FOR GASOLINE

• ASTM Distillation

• Reid vapour pressure

• Octane number

• Gum content

• Sulfur content

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 ASTM DISTILLATION

There are two types of ASTM distillations that are used in the
refinery for plant control and finished product quality.
These are the ASTM D86 for naphtha and equivalent and for
the kerosenes. D156 is used for the ASTM distillation of
atmospheric gas oils (heating oil and diesel).
The major difference between the two tests are the volume of
sample used. In the case of the D86 the sample will be 100 ml
while that for D156 the sample will be 200 ml.

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ASTM DISTILLATION

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 OCTANE NUMBER

Octane numbers are a measure of a gasoline’s resistance to

knock or detonation in a cylinder of a gasoline engine. The
higher this resistance is the higher will be the efficiency of the
fuel to produce work.

A relationship exists between the antiknock characteristic of

the gasoline (octane number) and the compression ratio of the
engine in which it is to be used. The higher the octane rating of
the fuel then the higher the compression ratio of engine in
which it can be used.

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 OCTANE NUMBER

An octane number is that percentage of isooctane in a blend of

isooctane and normal heptane that exactly matches the knock
behavior of the gasoline.

Thus, a 90 octane gasoline matches the knock characteristic of

a blend containing 90% isooctane and 10% n-heptane.

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 OCTANE NUMBER

The knock characteristics are determined in the laboratory

using a standard single cylinder test engine equipped with
a super sensitive knock meter.

The reference fuel (isooctane blend) is run and compared

with a second run using the gasoline sample.

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 OCTANE NUMBER

Two octane numbers are usually determined. The first is the

research octane number (ON res or RON) and the second is
the motor octane number (ON mm or MON).

The same basic equipment is used to determine both octane

numbers, but the engine speed for the motor method is much
higher than that used to determine the research number.

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 OCTANE NUMBER
The actual octane number obtained in a commercial vehicle
would be somewhere between these two. The significance of
these two octane numbers is to evaluate the sensitivity of the
gasoline to the severity of operating conditions in the engine.
The research octane number is usually higher than the motor
number, the difference between them is termed the ‘sensitivity
of the gasoline.’
Isoparaffins and aromatics have high octane numbers while n-
paraffins and olefins have low octane numbers

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 OXYGENATES

Oxygenates were used originally simply as a additive to

improve octane number.

However, because of their oxygen content they are now added

also ton reduce the carbon monoxide and hydrocarbon in the
emission gases. There are a number of oxygenates now used in
gasoline manufacture

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OXYGENATES COMMONLY USED IN GASOLINE

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 OXIDATION STABILITY (GUM CONTENT)

Motor gasoline are often stored for six months or even longer
before use. So it is essential that they should not undergo any
deleterious change under storage conditions.

Gasoline manufactured by cracking processes contain

unsaturated components which may oxidise during storage and
form undesirable oxidation products.

An unstable gasoline undergoes oxidation and polymerisation

under favourable ambient conditions , forming gum, a resinous
material.
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 OXIDATION STABILITY (GUM CONTENT)
Gum formation appears to be the result of a chain reaction
initiated by radicals such as peroxides and catalysed by the
presence of metals, particularly copper, which might have been
picked up during refining and handling operations.

Some inhibitors are generally added to retard the oxidation of

the olefin content of the fuel.

Inhibitors normally phenols or amine compounds and small

quantities between 0.001and 0.02 percent by weight are
sufficient to ensure good stability.
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 OXIDATION STABILITY (GUM CONTENT)

Gum content of gasoline is evolved by oxidising the sample

with oxygen under restricted conditions, thus accessing
possible gum formation during storage.

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 KEROSENE

Petroleum is the general name applied to the group of refined

petroleum fractions employed as fuel and illuminant.

Low in viscosity, with a good degree of refinement to be fairly

stable, light in colour, and free from smoky ill smelling
substances.

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 TEST AND PROPERTIES OF KEROSENE

i. Flash and fire point

ii. Smoke point (burning quality)

iii. Volatility

iv. Sulfur content

v. Aniline point.

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FLASH POINT

The lowest temperature of the sample, corrected to a

barometric pressure of 101.3 kPa 760 mm Hg , at which
application of a test flame causes the vapour of the sample to
ignite under specified conditions of test.

FIRE POINT

The fire point, is defined as the temperature at which the

vapour continues to burn after being ignited.

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 FLASH POINT

i. Tag Closed Cup method (commonly known as the ABEL

flash point) - kerosene cut range materials and lighter
distillates ; flash of between 68◦F and 148◦F

ii. The Pensky Marten Closed Cup method – other distillates

and residuum products with flash points above 148◦F.

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 FLASH POINT

Used to establish the flammable criteria in transporting the

material.

Generally shipping and safety regulations will be based on the

flash point criteria.

The flash point should NOT however be used to describe or

appraise the fire hazard or risk under actual fire conditions.

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PENSKY MARTEN CLOSED CUP
The sample is heated at a
slow, constant rate with
continual stirring. A small
flame is directed into the
cup at regular intervals with
simultaneous interruption of
stirring. The flash point is
the lowest temperature at
which application of the test
flame causes the vapour
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above the sample to ignite
FLASH POINT

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 FLASH POINT
Flash point should not be mistaken with fire point, which is
defined as the minimum temperature at which the
hydrocarbon will continue to burn for at least 5 s after being
ignited by a flame.

Autoignition temperature is the minimum temperature at

which hydrocarbon vapor when mixed with air can
spontaneously ignite without the presence of any external
source. Values of autoignition temperature are generally
higher than flash point. This is particularly important from a
safety point of view when hydrocarbons are compressed.
Standard test is ASTM D 2155.

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POUR POINT AND CLOUD POINT

Pour points are determined

initially by heat treating the
petroleum specimen above it’ s
expected pour point and then
to cool the specimen in
controlled stages until the pour
point is observed.
The pour point is the
temperature of the material
that it ceases to flow.

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SAMPLES SHOWING CLOUD AND POUR POINT

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 ANILINE POINT
Aniline is a poor solvent for aliphatic hydrocarbons and
excellent one for aromatics. This property is used in the aniline
point test. Aniline point of oil is the lowest temperature at
which the oil is completely miscible with an equal volume of
aniline.

High aniline point indicates that the fuel is highly paraffinic

and hence has a high diesel index and very good ignition
quality. In case of aromatics the aniline point is low and the
ignition quality is poor
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ANILINE POINT

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 ANILINE POINT

Diesel index is an indication of the ignition quality of a diesel

fuel. This is determined by calculation from the specific
gravity and the aniline point of the sample. Although it is of
the same order as the cetane number, it may differ widely from
the cetane number. Higher the diesel index better is the
ignition quality of the diesel fuel. It is normally used as a guide
to ignition quality of the diesel fuel in the absence of test
engine for the direct measurement of cetane number.
The diesel index is calculated as follows:
Diesel index = (Aniline point,ºF ׺API)/100
Diesel index = (Aniline gravity constant)/100
Diesel index = (Cetane number −10)/0.72

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 SMOKE POINT

The maximum flame height in millimetres at which kerosene

or other volatile liquid fuels including gas turbine (jet) fuels
will burn without smoking, when determined in the apparatus

and under specified conditions.

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SMOKE POINT

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 SMOKE POINT

The sample is burned in a standard lamp in which it is possible

to adjust the flame height against a background of a graduated
millimetre scale. The smoke point is measured by raising the
wick until a smoky flame is produced and then lowering to the
point where the smoky tail just disappears. This flame height,
measured to the nearest millimetres, is the smoke point of the
sample

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 KINEMATIC VISCOSITY

The kinematic viscosity of an oil is obtained by measuring the

time required for a sample of the oil to flow, under gravity
through a capillary.

The capillary is a part of the calibrated viscometer and the

flow through it of the oil is at a known temperature.

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 UNITS - VISCOSITY

Centistokes ,

Seconds Saybolt Universal,

Seconds Saybolt Furol, Or Seconds Redwood.

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SAYBOLT VISCOMETER ENGLER VISCOMETER

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 CONRADSON CARBON RESIDUE

The amount of carbon residue left after complete evaporation

and pyrolysis of an oil.

The degree of this carbon content is indicative of the coke

forming properties of the oil.

The value of the Conradson carbon content is important in

most heavy oil hydrotreating, and most cracking processes.

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CONRADSON CARBON RESIDUE

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 DIESEL FUEL

Diesel fuels are in the boiling range of 250 – 320 °C and fall
under gas oil fractions

These are classified into two classes as high speed diesels and
low speed diesels.

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 PARAMETERS OF DIESEL FUEL

• The cetane number

• Aromatic content – Aniline Point

• Density

• Sulfur content

• Distillation

• Viscosity

• Cloud and pour points

• Flash point
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 CETANE NUMBER

This is the result of an engine test that compares the ignition

delay for a fuel. For this test two reference fuels are chosen.
The first is normal cetane (C16) and the second is an isomer of
cetane which is heptamethylnonane.
The normal cetane is arbitrarily given the cetane number of
100, while the isomer as the second reference fuel is assigned
a cetane number of 15. The fuel being tested is run in a
standard test engine.
The cetane number is derived by comparing the ignition delay
of the test diesel with a blend of the two reference fuels. The
cetane number is then calculated using the equation:

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 CETANE NUMBER

Higher cetane numbers indicates that the fuel has a shorter

ignition delay. The higher the cetane number also results in
less CO and unburnt hydrocarbons in the engine emission
gases. This has a greater effect in the older diesel engine.
Modern engines are equipped with retarded ignition timing
and increasing the cetane number has a smaller effect on these
more modern engines.

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 CETANE NUMBER

The simplest way to improve cetane number is to use an

appropriate ignition improvement additive. These are mainly
alkyl nitrates.
The effectiveness of cetane improvement additives tend to be
linear with addition rate, however the improvement can vary
with different diesel blend stock.
Paraffins which already have high cetane value respond best to
the additives. Aromatics on the other hand, which have a low
cetane number have a poorer response.
About 500 wppm of standard alkyl nitrate will increase the
cetane value by 2–5 numbers. Another way to increase cetane
number is to modify the hydrocarbon type in the diesel blend.
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CETANE NUMBER OF HYDROCARBON

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 LUBE OIL

Fraction that is left after lighter components, namely gasoline,

kerosene, diesel oil during crude distillation.

Main products from VDU.

Composed of paraffins, napthenes, aromatics and unsaturated

bodies

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 TEST FOR LUBE OIL

1. Flash Point

2. Viscosity

3. Pour point

4. Oxidation stability

5. Carbon residue

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 CATEGORIES OF LUBE OIL

1. Machine and engine oils (neutral oils)

2. Compounded oils

3. Turbine oils

4. Cold test oils

5. Transformer oils

6. Colour oils

7. Corrosive oils

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 DISTILLATION

For a crude oil or a petroleum fraction of unknown

composition, the boiling point may be presented by a
curve of temperature versus vol% (or fraction) of
mixture vaporized.
There are several methods of measuring and reporting
boiling points curves of crude oil and petroleum
fractions:
1- ASTM Distillation
2- True Boiling Point (TBP)

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 ASTM D 86

ASTM D 86 is one of the simplest and oldest methods of

measuring and reporting boiling points of crude oil and
petroleum fractions. The test is conducted at atmospheric
pressure with 100 mL of sample and the result is shown as a
distillation curve with temperatures at 0, 5, 10, 20, 30, 40, 50,
60, 70, 80, 90, 95, and 100% volume vaporized.

For crudes and heavy products, temperatures are reported at

maximum of 90, 70, or even 50% volume vaporized. This is
due to the cracking of heavy hydrocarbons at high
temperatures.

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ASTM D 86

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 TRUE BOILING POINT

ASTM D 86 distillation data do not represent actual boiling

point of components in a petroleum fraction. Atmospheric true
boiling point (TBP) data are obtained through distillation of a
petroleum mixture using a distillation column with 15-100
theoretical plates at relatively high reflux ratios (1-5 or greater).

The high degree of fractionation in these distillations gives

accurate component distributions for mixtures. The lack of
standardized apparatus and operational procedure is a
disadvantage, but variations between TBP data reported by
different laboratories for the same sample are small.

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 TRUE BOILING POINT
The IBP from TBP curve is less than the IBP from ASTM D 86
curve, while the FBP of TBP curve is higher than that of ASTM
curve. Therefore, the boiling range based on ASTM D 86 is
less than the actual true boiling range.

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PERFECT TBP FRACTIONATION

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LOW SELECTIVITY FRACTIONATION

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