PETROLEUM REFINING & PETROCHEMICAL

TECHNOLOGY

Subject: Petroleum refining

Subject code: 03628302

Total credit Examination scheme

Teaching Scheme Theory Practical
Total
Marks Marks
Marks
Theory Tutorial Practical c ESE PA ESE PA
0 0 2 1 0 0 20 30 50

Sr no. Title of practical Page no.

1 Determine flash point by penskey martin 2
method
2 Determine fire point by penskey martin 5
method
3 Determine softening point and drop point of 7
grease
4 Determine aniline point of given sample 9
5 Determine penetration number of grease 11
6 Determine the carbon residue by conradson 13
method
7 Measure viscosity of lube oil by redwood 15
viscometer
8 Determine the cloud point of given oil 18
sample
9 Determine the pour point of given oil sample 20
10 Determine the smoke point of given oil 22
sample
11 Determine the kinematic viscosity of oil 23
sample using saybolt’s viscometer

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EXPERIMENT 1
DETERMINE FLASH POINT BY PENSKEY MARTIN METHOD

AIM: - Determination of flash point of a combustible liquid by Pensky-Martan’s

closed cup flash point apparatus.

THEORY: -
Flash point is defined as the lowest temperature of a liquid at which its vapours will
form a combustible mixture with air. At this point the lubricating oil gives off enough
vapors that ignite for a moment when tiny flame is brought near it. This is detected
by the appearance of momentary flash upon the application of small flame over the
surface of oil.

CHEMICALS
• Given lubricating oil
• Suitable organic solvent like CCl4, ether, petroleum spirit or benzene

APPARATUS
• Pensky Marten’s flash and fire point apparatus
• Match box
• Thermometer
• Filter paper

DESCRIPTION OF THE APPARATUS

A Pensky Martin apparatus consists of the following parts:
• Oil cup – it consists of a cup of brass which is about 5 cm deep and 5.5 cm in
diameter. The lid of cup is provided with four opening of standard size. One of
which is used for thermometer, second for a stirrer having two blades, third is
for introducing test flame and fourth is for admission of air. The level to which
oil is to be filled is marked inside the cup.
• Shutter – it is provided at the top of cup. By moving the shutter, opening in the
lid opens and flame is dripped into this opening, thereby bringing the flame
over the oil surface.
• Flame Exposure Device- it is a small flame connected to the shutters by a
lever mechanism. 
• Air Bath- oil cup is supported by its flange over an air bath, which is heated
electrically or a gas burner.
• Pilot Burner – when test flame is introduced in the opening, it gets
extinguished, but when the flame is returned to its original position, it is
automatically lighted by the pilot burner.

DIGRAM:

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PROCEDURE:
• Clean and dry all parts of the apparatus with the help of suitable solvent e.g.
CCl4, ether, petroleum spirit or benzene and dry it to remove any traces of
solvent.
• Fill the oil cup with the test oil up to the mark.
• Fix the lids on the top through which are inserted a thermometer and a stirrer.
Ensure that the flame exposure device is fixed on the top.
• Light the test flame and adjust it to about 4 mm in diameter.
• Heat apparatus as temperature of oil increases by 5 to 60 per min. as stirrer is
continuously rotated.
• At every 10 C rise of temp. Introduce test flame into the oil vapor. This is
done by operating the shutter. On moving knob of shutter, test flame is
lowered in oil vapors through opening.
• When test flame causes a distinct flame in interior cup, note temerature
which represent the flash point
• Further heat the oil at the rate of 10C/ min. and continue applying the test
flame as before.
• On observing a flash, stop the heating process and allow the temperature to
decrease.
• Check the occurrence of a flash at every 1 0C drop in temperature. Record the
lowest temperature at which the flash is observed as the flash point of the
sample.

OBSERVATION:
Table 1
Sr Increasing Inference (No flash or Flash
no. temperature(0C) observed)
1
2
3
4
5
6

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Table 2

Sr Decreasing Inference (No flash or Flash

no. temperature(0C) observed)
1
2
3
4
5
6

RESULT:
The Flash Point of given sample determined by Pensky Marten’s Flash Point
apparatus is found to be ------------- 0C.

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EXPERIMENT 2
DETERMINE FIRE POINT BY PENSKEY MARTIN METHOD

AIM: - To determine fire point of the given lubricating oil using Pensky Marten’s
apparatus.

PRINCIPLE: -.
Fire point is the lowest temperature at which the vapors of the oil burn continuously
for at least five seconds when a tiny flame is brought near it.

CHEMICALS
• Given lubricating oil
• Suitable organic solvent like CCl4, ether, petroleum spirit or benzene

APPARATUS
A Pensky Martin apparatus consists of the following parts:
• Oil cup – it consists of a cup of brass which is about 5 cm deep and 5.5 cm in
diameter. The lid of cup is provided with four opening of standard size. One of
which is used for thermometer, second for a stirrer having two blades, third is
for introducing test flame and fourth is for admission of air. The level to which
oil is to be filled is marked inside the cup.
• Shutter – it is provided at the top of cup. By moving the shutter, opening in the
lid opens and flame is dripped into this opening, thereby bringing the flame
over the oil surface.
• Flame Exposure Device- it is a small flame connected to the shutters by a
lever mechanism. 
• Air Bath- oil cup is supported by its flange over an air bath, which is heated
electrically or a gas burner.
• Pilot Burner – when test flame is introduced in the opening, it gets
extinguished, but when the flame is returned to its original position, it is
automatically lighted by the pilot burner.

DIGRAM:

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PROCEDURE: -
• Clean and dry all parts of the apparatus with the help of suitable solvent e.g.
CCl4, ether, petroleum spirit or benzene and dry it to remove any traces of
solvent.
• Fill the oil cup with the test oil up to the mark.
• Fix the lids on the top through which are inserted a thermometer and a stirrer.
Ensure that the flame exposure device is fixed on the top.
• Light the test flame and adjust it to about 4 mm in diameter.
• Heat apparatus as temperature of oil increases by 5 to 60 per min. as stirrer is
continuously rotated.
• At every 10 C rise of temp. Introduce test flame into the oil vapor. This is done
by operating the shutter. On moving knob of shutter, test flame is lowered in
oil vapors through opening.
• When test flame causes a distinct flame in interior cup, note temperature
which represent the flash point
• Further heat the oil at the rate of 10C/ min. and continue applying the test
flame as before.
• The temperature at which the vapors of the oil give a clear and distinct blue
flash for five seconds is recorded as the fire point of the oil. C.

RESULT: - The fire point of given oil sample= C.

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EXPERIMENT 3
DETERMINE SOFTENING POINT AND DROP POINT OF GREASE

Objective:-To determination of softening point and drop point of grease

Theory
Softening point
It is the temperature at which the substance attains a particular degree of softening
under specified conditions of test.

Dropping point
The dropping point of soap-thickened lubricating grease is the temperature at which it
passes from a semi-solid to a liquid state under specific test conditions. It is an
indication of the type of thickener used, and a measure of the cohesiveness of the oil
and thickener of grease

Apparatus
• The test apparatus consists of a grease cup with a small hole in the bottom,
test tube, two thermometers, a container, stirring device if required and
an electric heater.
• The inside surfaces of the grease cup are coated with the grease to be tested.
• A thermometer is inserted into the cup and held in place so that the
thermometer does not touch the grease.
• This assembly is placed inside a test tube.
• The test tube is lowered into the container which is filled with oil in D-566 and
has an aluminium block in D-2265.
• Another thermometer is inserted into the oil/block.

DIAGRAM

PROCEDURE
• To execute a test, the oil/block is heated, while being stirred, at a rate of 8 °F
(4.4 °C) to 12 °F (6.7 °C) per minute until the temperature is approximately
30 °F (17 °C) below the expected dropping point.
• The heat is reduced until the test tube temperature is at most 4 °F (2.2 °C)
less than the oil/block temperature.
• Once the temperature has stabilized the sample is inserted.

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• The dropping point is the temperature recorded on the test tube thermometer,
plus a correction factor for the oil/block temperature, when a drop of grease
falls through the hole in the grease cup.
• If the drop trails a thread, the dropping temperature is the temperature at
which the thread breaks.

RESULT: - The softening point and drop point of grease is............................

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EXPERIMENT 4
DETERMINE ANILINE POINT OF GIVEN SAMPLE

OBJECTIVE: - To Determine of aniline point of given sample.

THEORY
The aniline point is a physical characteristic of hydrocarbon compounds, such as
oils, and refers to the minimum temperature at which the hydrocarbon and the same
amount of the compound aniline (C5H5NH2) are perfectly miscible. High aniline
point the greater the aniline point, the lower the aromatics in diesel oil. A higher
aniline point also indicates a higher proportion of paraffin. At temperatures below this
point, a mixture of the compound and an equal volume of aniline will not dissolve
together.
APPARATUS
• Beaker
• Test tube
• Stirrer
• Stand and clamp
• heating bath
• Thermometer
CHEMICALS
• Aniline
• Lubricating oil
DIAGRAM

PROCEDURE:
• At first Clean and dry the ‘beaker’
• Then we add 20 ml of distilled aniline and 20ml of given sample (lubricating
oil) in the ‘beaker’, it will form two layers.

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• Then heat the sample in the beaker on heating bath with continuous stirring.
• The minimum temperature at which two layers give a single phase is noted as
aniline point.
• Now stirring of ‘U’ tube mixture is stopped, and mixture is allowed to cool.
• Temperature at which two layers are formed is also considered as aniline
point.

Result and Calculation:

Recording the aniline point (AP) of the samples
℉ = 32 + (1.8 ℉ ℉)
℉ = (℉ − 32) ℉ 0.55
Test sample Aniline point℉ Aniline point℉
Lubricating oil

Result
The aniline point of the given sample is..........

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EXPERIMENT 5
DETERMINE PENETRATION NUMBER OF GREASE

AIM: - To determine penetration number of Grease

THEORY
Penetration is defined as the depth of penetration (expressed in 10th of milimeters)
of a metallic cone with standardized shape and dimension into a solid grease sample
for a period of 5 seconds. The penetration is determined with the Cone Penetrometer
or Richardson Penetrometer
In this experiment, the sample is melted and cooled under controlled conditions. The
penetration is measured with a penetrometer by means of which standard needle is
applied to the sample under specific conditions.

APPARATUS
Penetration Apparatus
Bitumen
Water bath
Sample container

PROCEDURES
• The sample been heated with care, it has been stirring as soon as possible to
prevent local over-heating until it become sufficiently fluid to pour. Avoid
incorporating bubbles into samples.
• The sample been poured into sample container to a depth such that, when
cooled to the depth of sample is at least 10mm greater than the depth to
which the needle is expected to penetrate.
• Covers have been loosely for each container as a protection against dust and
allow to cooling the atmosphere for 1 to 1½ hour
• The sample been placed in the water bath for an hour at around 25 oC of
temperature.

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• A penetration needle has been cleaned with toluene or other suitable solvent,
dry with dried clean cloth and inserted the needle in the penetrometer.
• The needle position has been slowly lowering it until its tip just makes contact
with the surface of the sample.
• The reading of the penetrometer has been noted or brought the pointer to
zero.
• The needle holders has been quickly released for the specified period of time
and adjust the instrument to measure the distance penetrated in tenth of
a millimetre.
• At least made three determinations at points on the surface of the sample not
less than10mm from side of the container and not less than 10mm apart. The
needle has beencleaned before repeating the test

Sample Penetration
Readings Mean

RESULT
Mean Penetration Value is

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EXPERIMENT 6
DETERMINE THE CARBON RESIDUE BY CONRADSON METHOD

TITLE: To determine the carbon residue by conradson method

APPARATUS:
1. Porcelain crucible
2. Skidmore crucible
3. Chimney wire support
4. Sand bath
5. Kerosene oil (sample)

THEORY: Carbon residue is what the leftover particles of a fuel product are
transformed into. The carbon residue of a fuel is the tendency to form carbon
deposits under high temperature conditions in an inert atmosphere. This is an
important value for the crude oil refinery, and usually one of the measurements in a
crude oil assay. Carbon residue is an important measurement for the feed to the
refinery process fluid catalytic cracking and delayed coking. High amounts of carbon
residue can be damaging to the environment.
DIAGRAM

PROCEDURE:
• Weight approximately one gram of sample oil free of moisture and suspended
material in the crucible.
• Place this crucible in the centre of skidmore level the sand in the sand bath
and set skidmore crucible on triangle right in centre of sand bath.
• Apply covers to both skidmore and porcelain air crucible. The covers must
have arrangement of free exist of vapors as they formed.
• Heat from strong flame from gas burner so that free ignition occurs in 10
minutes and a blue flame appear on the alimony immediately.
• Moves or tie the gas burner so that gas flame plays on the side of the
chimney for the purpose of ignition of vapors. When vapors cease to burn and
no more blue flame appear. Read just the burner and increase the heat so

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that sand bath sheet is cherry red and maintain exactly for 7 minutes. The
total time for this is approximately 28 to 32 minutes.
• Remove the burner and allow the apparatus to cool until no smoke appear
and then removed the cover of skidmore crucible
• Take out crucible with tongs and placed it in desiccators. Cool and weight the
crucible. Carbon residue

CALCULATION
• Weight of crucible = 24.3g
• Weight of crucible with oil = 47.4g
• Weight after experiment = 24.31g
• Weight of carbon residue = 0.01g

RESULT:
Amount of carbon residue = 0.01g

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EXPERIMENT 7
MEASURE VISCOSITY OF LUBE OIL BY REDWOOD VISCOMETER

AIM:-To determine the kinematic viscosity of the given sample of oil at various
temperatures and study corresponding variation with respect to temperature.

APPARATUS REQUIRED
Red wood viscometer with accessories
Measuring flask
Thermometer
Stop watch

THEORY
• Red wood viscometer is based on the principle of laminar flow through the
capillary tube of standard dimension under falling head. The
viscometer consists of vertical cylinder with an orifice at the center of the base
of inner cylinder.
• The cylinder is surrounded by a water bath, which can maintain temperature
of the liquid to be tested at required temperature. The water bath is heated by
electric heater.
• Cylinder which is filled up to a fixed height with liquid whose viscosity is to be
determined is heated by water bath to the desired temperature.
• Then orifice is opened and the time required to pass the 50cc of oil is noted.
With this arrangement variation of viscosity with temperature can be studied

DIAGRAM

PROCEDURE
• The instrument was levelled with the help of the circular bubble and by
levelling foot screws.
• The water bath was filled with water.
• The orifice is closed with the ball valve and the cylinder is filled up to index
mark with oil.
• The steady state temperature of oil was recorded.
• The procedure is repeated for different by heating oil with water bath

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CALCULATION
In this case of red wood viscometer, the kinematic viscosity (v) of liquid andthe time
(t) required to pass 50cc of liquid are correlated by expression.
v =0.0026 – 1.175/t
Where,
v = Kinematic viscosity
t = time in seconds to collect 50 cc of oil

OBSERVATION
Sr no. Temp. of oil time in seconds to collect 50 cc of Kinemetic viscosity
bath oil (sec) (centistrokes)

Observation:
(A) (1) Temp. of paraffin bath = ---------- 0C
(2) Temp. of oil bath = --------- 0C

Sr. Number Vol. collected ml. . Time in sec.

1 50
2 50
3 50

Plot the graph of K.V. Vs Flow time.

Sr. Numbe Time in sec. K.V. Centi stock

1 106.4 22
2 115 24
3 123.7 26
4 132.5 28
5 141.3 30
6 150.2 32.0
7 186.0 40
8 195.3 42
9 204.4 44
10 213.7 46
11 222.9 48
12 232.1 50

RESULT
The kinematic viscosity for the given sample was determined and the graph
was plotted and it was observed that the kinematic viscosity of the given sample
decreases with increases in temperature.

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EXPERIMENT 8
DETERMINE THE CLOUD POINT OF GIVEN OIL SAMPLE

OBJECTIVE: - To Determine the Cloud point Of Given Oil Sample

APPARATUS:
• Given oil sample
• Thermometer
• Beaker
• Cooling bath
• Cork
• Testing jar

THEORY:
Cloud point is the temperature at which oil becomes cloudy or hazy when oil is
cooled at specified rate. Cloud point is related to low temperature characteristics of
fuel and tells the behaviour of fuel at low temperatures Cloud point indicates the
tendency of oil to plug filters or small orifices at cold operating temperatures.
Diagram

PROCEDURE:
• Clean and dry the test tubes and fill it with heavy petroleum product to
minimum required level.
• Heat the test tube on a burner to get clear & uniform consistency.
• Seal the test tube with a cork having thermometer of required range, the bulb
of thermometer should be dipped in the sample.
• Now place the test tube in the ice bath in vertical position.
• At an interval of 20C minimum decreasing observe the cloudiness at the
bottom of test tube, bringing it out in vertical position from the apparatus.

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•Note down the temperature at which cloud or crystals are observed. Report it
as cloud point of the sample.
RESULTS:
• Cloud point of given oil sample = ................................... 0C

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EXPERIMENT 9
DETERMINE THE POUR POINT OF GIVEN OIL SAMPLE

OBJECTIVE: - To Determine the Pour Point Of Given Oil Sample

APPARATUS:
• Given oil sample
• Thermometer
• Beaker
• Cooling bath
• Cork
• Testing jar

THEORY:
Pour Point is the temperature at which oil just ceases to flow. The pour point of a
liquid is the lowest temperature at which it becomes semi solid and loses its flow
characteristics. Pour point is related to low temperature characteristics of fuel and
tells the behaviour of fuel at low temperatures. . Pour point tells us the temperature
below which oil cannot be used as lubricant.
Diagram

Procedure
• Clean and dry the test tubes and fill it with heavy petroleum product to
minimum required level.
• Heat the test tube on a burner to get clear & uniform consistency.
• Seal the test tube with a cork having thermometer of required range, the bulb
of thermometer should be dipped in the sample.

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• Now place the test tube in the ice bath in vertical position.
• At an interval of 20C minimum decreasing observe the cloudiness at the
bottom of test tube, bringing it out in vertical position from the apparatus.
• Note down the temp. at which cloud or crystals are observed. Report it as
cloud point of the sample.
• Continue the cooling of test tube in the same manner until temperature
reaches at which the sample in test tube does not show any movement for at
least 5 sec, when brought to the horizontal position. Note this as pour point of
the sample.

RESULTS:
• Poue point of given oil sample = ................................... 0C

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EXPERIMENT 10
DETERMINE THE SMOKE POINT OF GIVEN OIL SAMPLE

AIM: Determination of smoke point of light petroleum products.

REQUIREMENTS:
• Smoke point apparatus
• Beaker
• Petroleum sample.

THEORY:
Smoke Point is the maximum flame height in mm at which the sample burns without
smoke. Smoke point is related with the aromatic content of the liquid and it is
inversely proportional to the aromatic content. Smoke point is used to determination
of smoking tendency.
Smoking tendency is proportional to the aromatic content and is given by Eq.
Smoking tendency = 320 / smoke point in mm.

PROCEDURE:-
• Clean the sample container with suitable solvent and dry it.
• Fill the sample container up to desired level and introduce a wick in the
container.
• Place this assembly in the burning chamber of the apparatus.
• Open the glass door, light the flame and closed the glass door.
• By adjustment of sliding screw observe the condition and height of the flame.
If it is giving smoke, reduce the flame height to stage I, them a further to
stage II and also familiarised with the flame height decrease to IIIrd stage.
• Adjust the point of the flame so that it burns without smoke.
• Note this height in mm using scale on the back side. Repeat it to get a
constant reading.

Results:
Smoke point of given petroleum product is..................

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EXPERIMENT 11
DETERMINE THE KINEMATIC VISCOSITY OF OIL SAMPLE USING
SAYBOLT’S VISCOMETER
Aim: To determine the kinematic viscosity of oil sample using Saybolt’s viscometer.

Requirements:
• Say bolt’s viscometer
• Stop-watch, 60 ml.
• collection flask
• thermometer
• oil sample
• Paraffin oil etc.

Procedure
• Clean and dry the oil cylinder of viscometer.
• Insert the cork tightly enough to prevent any air escape.
• Fill the cylinder upto the mark with oil.
• Take out excess oil with the help of pipette.
• Insert a thermometer both in a oil bah and the paraffin bath.
• Start heating at a controlled rate and stir the oil and paraffin bath continuously
for uniform heating.
• As the oil sample is at desired temperature open the cork at bottom and note
down the time required to fill 60 ml. of oil.
• Repeat the process for constant reading. Find out a constant flow time at
difference temperature.
Results:

Sr. Number Temp. of oil bath Time in sec . Kinematic viscosity

1

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2
3
4

Observation:
(A) (1) Temp. of paraffin bath = ---------- 0C
(2) Temp. of oil bath = --------- 0C

Sr. Number Vol. collected ml. . Time in sec.

1 50
2 50
3 50

Plot the graph of K.V. Vs Flow time.

Sr. Numbe Time in sec. K.V. Centi stock

1 106.4 22
2 115 24
3 123.7 26
4 132.5 28
5 141.3 30
6 150.2 32.0
7 186.0 40
8 195.3 42
9 204.4 44
10 213.7 46
11 222.9 48
12 232.1 50

RESULT
The kinematic viscosity for the given sample was determined and the graph
was plotted and it was observed that the kinematic viscosity of the given sample
decreases with increases in temperature.

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