University of Petroleum and Energy Studies,

Dehradun

Manual
Petroleum Product Testing
Laboratory

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 Table of Contents

Sr. No. Experiment

1 Aniline Point
2 ASTM Distillation
3 Cloud and Pour Point
4 Drop Point
5 Flash and Fire Point
6 Redwood Viscometer
7 Reid Vapor Pressure
8 Smoke Point
9 Rust Preventing Characteristics
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11
12
13

EXPERIMENT NO. 1
ANILINE POINT

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AIM:
To determine the aniline point of the given petroleum product

APPARATUS REQUIRED:
 Thermometer
 Stirrer
 Water Bath
 Air jacket
 Aniline and Diesel

THEORY:
Definition:
 Aniline point is defined as the minimum temperature at which equal
volumes of anhydrous aniline and oil mix together.

 Cetane number is defined as the percentage by volume of n-cetane in a

mixture of n-cetane and α-methyl naphthalene.

Diesel fuels are mainly composed of paraffins and some amount of aromatics.
Aromatics present in the fuel cause abnormal ignition delay. So, aniline point test is to be
conducted in the fuel, thereby verifying the quality of the diesel fuel.

High aniline point indicates that the fuel is highly paraffinic and hence has a high
diesel index and very good ignition quality.

Aniline being an aromatic compound, it freely mixes with aromatics. So, a low
aniline point indicates low diesel index, because of high percentage of aromatics.

Diesel index is an indication of the ignition quality of a diesel fuel. Higher the
diesel index better is the ignition delay of the diesel fuel.

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 Self ignition temperature is low for paraffins but high for aromatics. Thus a fuel
rich in aromatics burns later causing ignition delay, which gives rise to diesel knock.

Heptamethyl nonane can be used in place of α-methyl naphthalene. The shorter

the ignition delay period higher is the cetane number of the fuel.

SIGNIFICANCE:
 To verify the quality and quantity of diesel fuel.
 To assess the paraffinic and aromatic content of fuel.
 Ignition delay, Diesel index, Cetane number of the fuel can be calculated.

FORMULA USED:
1. Conversion of Celsius to Fahrenheit:
˚F= (9/5) ˚C+32
Where, F - Temperature in Fahrenheit.
˚C - Temperature in Celsius.

2. API Gravity = (141.5/specific gravity)-131.5

3. Diesel index = (Aniline point * API Gravity)/100

4. Cetane number = Diesel index-3

OBSERVATION:

Miscibility temperature of aniline and sample (diesel)= ˚C

CALCULATION:

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 Conversion of Celsius to Fahrenheit: F = (9/5) ˚C+32 =
=

API Gravity = (141.5/Specific gravity)-131.5 =

=

Diesel index = (Aniline point * API gravity)/100 =

=

Cetane number = Diesel index – 3 =

=

PROCEDURE:
 A water bath was taken, in which the two tubes with holder and cork fitted
were to be placed.

 The test tube is filled with an equal volume of aniline and given sample.

 A stirrer and a thermometer is inserted inside the inner tube by means of a

cork.

 The air bath tube is placed between the test tube and the water bath. It is
left for air circulation and uniform heating.

 The sample is placed in a mantle and it is started heating. With a constant

stirrer the experiment was carried out.

 At a constant temperature the two liquids mixes or miscibility occurs. This

point of temperature is aniline point.

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  Diesel, aniline and water are taken in a weighed bottle one after the other
and the weights are found at 15.6˚C by using ice.

RESULT:
The aniline point of the sample was determined and thus the diesel index and
cetane number of the sample were determined.
 Aniline point of the sample =

 Diesel index of the sample =

 Cetane number of the sample =

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7
 EXPERIMENT NO.2

ASTM DISTILLATION

AIM:

To determine the distillation range of the given sample at atmospheric pressure.

APPARATUS REQUIRED:

 Distillation Apparatus
 Thermometer
THEORY:

The function of distillation is to separate by vaporization of liquid mixture of

miscible and volatile substances into individual components. Determination of
distillation range and characteristics are of great value in the evaluation of the
petroleum products. Distillation Parameters like boiling point, final boiling point, and
Middle Boiling Point are estimated by this experiment.

SIGNIFICANCE:

 For crude oil the atmospheric distillation data gives some idea of the fractions that
could be collected below 300 deg. C.

 For motor spirit the 10% distillation value gives an indication of engine start
condition, also the high Final Boiling Point Value indicates crankcase dilution.

 For diesel fuel the presence of higher boiling compounds and hence the carbon
deposit formation in the engine.

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PROCEDURE:

 The given flask is thoroughly cleaned using solvent and dried.

 The given test sample is taken inside the flask and the cork with appropriate
thermometer is placed on the neck of the flask.

 The flask is placed on the asbestos board and fixed to the metal condenser with a
cork. The asbestos board is raised or lowered till the flask is properly supported.

 The 100 cc measuring cylinder is placed below the condenser outlet.

 Heater is switched ON and the temperature variation is noted. The temperature at

which the first drop of distillate is collected in the measuring cylinder is noted
and reported as the initial boiling point.

 Heat is controlled so that the distillation proceeds at a uniform rate

 Middle boiling point is the temperature at 50% of oil distillates off.

 The volume of residue left after the distillation is measured and reported as non-
volatile substance.

OBSERVATIONS:

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 The Temperature at which First Drop Fall ………………
 The Temperature at which Middle Drop Fall ………………
 Percentage of Recovery ………………
 Percentage of Non – Volatile Residue ………………
 The Temperature at which Final Drop Fall ………………

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Distillation Apparatus Schematic Diagram

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RESULT:

The distillation characteristics of the given test sample is studied and reported below,

 Initial Boiling Point ………………

 Mid Boiling Point ………………
 Final Boiling Point ………………
 Percentage of Recovery ………………
 Percentage of Non – Volatile Residue ………………

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 EXPERIMENT NO.3
CLOUD AND POUR POINT
AIM:
To determine the cloud point and pour point of the given sample.

APPARATUS REQUIRED:

 Constant temperature bath

 Thermometer
 Flat bottomed test tube

DEFINITION:
Cloud point:
The cloud point of petroleum is the temperature at which a cloud or haze of
crystals appear at the bottom of the test jar, when the sample is cooled under prescribed
conditions.
Pour point:
Pour point is the lowest temperature expressed in multiples of 3 0C at which the
oil is observed to flow when cooled and examined under prescribed conditions.

THEORY:
The cloud point and the pour point are related to the flow conditions of crude and
its products at low temperature.
The cloud point gives the rough idea of the temperature above which the oil can
be handled safely, without any fear of congealing or filter clogging.

The pour point is determined to estimate the temperature at which a sample of oil
becomes sufficiently solid to prevent its movement by pumping.
The pour point temperature depends to a large extent on the thermal history of the
sample. Also the pour point indicates the waxy nature of the sample.

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PROCEDURE:
 Oil is poured into the test jar up to the level mark of 51 to 57 mm. If
necessary the oil is heated until it is sufficiently enough to flow.
 The test jar is closed with the cork carrying the thermometer. The cork
position is adjusted to make it fit properly into the tube.
 The thermometer bulb is immersed so that the beginning of the capillary is
3mm below the oil surface.
 The test jar surrounded by the air jacked is kept in the freezing mixture and
it is allowed to cool.
 The falling temperature was observed with every degree fall of temperature
in the given sample. The tube was withdrawn from the air jacket for a
moment of about (2-3sec) and examined. It was then replaced immediately.
 The temperature at which the cloudiness appeared was noted as the cloud
point.
 The test tube was cooled continuously. The test tube was withdrawn often
for 5 0C fall of temperature to observe the flow or pour point of the sample.
 The temperature at which the oil does not flow in the tube even when kept
horizontal for 5sec is recorded as pour point.

STANDARD POUR POINTS OF CRUDES USED IN INDIA:

Sl.No. Crude name Pour point degC

1. Ankleshwar 18
2. North/Gujarat 27
3. Bombay high 30
4. Basrah -15
5. UMM Shaiff -15
6. High speed diesel 6

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RESULT:

Thus the pour point of the given sample was found.

(i) The cloud point of the sample _____0C.

(ii) The pour point of the sample _____0C.

EXPERIMENT NO. 4
DROP POINT
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AIM:
To determine the drop point of the given sample.

APPARATUS REQUIRED:
 Drop Point Tube
 Drop Point Cup
 Thermometer
 Stirrer
 Stand

THEORY:
Drop point is the temperature which the given sample drops its characteristics
physically. It may also define as the temperature at which the thickener is so soluble in
the base oil that the sample become substantially fluid.

Clay and dye thickened greases have no measurable drop point. It cannot be
used to which upper operating temperature limit for grease the drop point is the
temperature at which the greases gives a drop.

SIGNIFICANCE:

Drop point is the most important test for the petroleum products. It is used find
the lubricant property of the given sample (Bitumen, Wax, and Grease).Drop point is also
used to know the viscosity of the sample.

PROCEDURE:

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  The appropriate beaker is taken and filled with a ¾ portion of water.

 The given sample is filled in the Drop point Cup and fixed inside the Drop
point tube.

 The tube is kept inside the water bath.

 The water bath is heated electrically.

 The thermometer is inserted in a beaker to note the temperature.

 As the temperature increases, the sample gets melted and becomes liquid

 The temperature at which the semisolid substance becomes liquid is noted

and recorded.

RESULT:

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The Drop points of the given samples are determined as follows,

SAMPLE I ……………………

SAMPLE II ……………………

SAMPLE III ……………………

DROP POINT APPARATUS

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 THERMOMETER

RUBBER
CORK

SAMPLE CUP

EXPERIMENT NO. 5

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 FLASH AND FIRE POINT

AIM:
To determine the flash and fire point of given samples.

THEORY:
Flash point and fire point can be taken as an indirect measure of volatility of
products.
Flash point:
The flash point is the lowest temperature at which application of test flame causes
the vapor above the oil to ignite.
Fire point:
The fire point is the lowest temperature at which the oil ignites and continues to
burn for 5 seconds.

The determination of flash point of petroleum products consists of heating a given

volume of liquid at standard rate of temperature rise until vapors is product to such a
degree as to give a flammable mixture with air in an enclosed space or with air in an open
cup, ignition resulting from the application of a small flame.

APPARATUS SAMPLE USED RANGE ( O C )

Abel apparatus Petroleum Products 19-49
Pensky-Martens Fuel oils and lubricating >49
(closed cup) oils, bitumen other than
cutback bitumen.
Cleveland Petroleum products <79
(open cup) except fuel oils

SIGNIFICANCE:

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 1. It can predict the possible fire hazards during transportation, storage and handling.
2. Petroleum products having low flash are potential to fire hazards.
3. Flash point can indicate the possible presence of highly volatile and flammable
material in relatively non-volatile or non-flammable.

CLEVELAND OPEN CUP

The test cup is filled to a specified level with test sample. The temperature of
sample is increased fairly rapidly at first and then at a slow constant rate as the flash point
is approached. At a specified intervals, a small test flame is passed across the cup. The
lowest temperature at which the application of the test flame causes the surface of the
liquid to ignite momentarily is taken as the flash point.

**To determine the fire point, the test is continued until the application of the test
flame causes the oil to ignite and burn for at least 5 seconds

PENSKY – MARTENZS APPARATUS

The sample is heated in a test cup at a slow and constant stirring. A small test
flame is directed into the cup at regular intervals with simultaneous interruption of string.
The test point is taken as the lowest temperature at which the application of the test flame
causes the vapor above the sample to ignite momentarily.

If the sample is known to have a flash point of 1050C or below, apply the test
flame when the temperature of the sample is a whole number not higher than 170C below
the flash point , and thereafter at each degree rise of temperature. Apply the test flame by
operating the mechanism on the cover which controls the shutter and test flame burner so
that the test flame is lowered into the vapor space of the cup in 0.5 second, left in its
lowered position for one second and quickly raised to its higher position. Do not stir the
sample while applying test flame.

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 If the sample is known to have a flash point above 1050C apply the test flame at each
temperature, that is, a multiple of 300C,beginning at a whole number temperature reading
not higher than 17 0 C below the flash point.

PROCEDURE:

1. The fuel was filled up to the marked level in the cup.

2. The fuel that had been held up in the cup was heated and test for flash was
conducted for every 30 seconds.

3. In case of closed cup the knob was used to open and external ignition was
provided.

4. The valves for flashpoint were first found and then the valves for fire point
were also obtained.

5. The experiment was repeated for other given samples and the valves were
tabulated.

RESULT:
Thus the flash and fire point of the given sample are given as,
Flash Point =
Fire Point =

FLASH AND FIRE POINT APPARATUS

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 EXPERIMENT NO. 8
REDWOOD VISCOMETER

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AIM:
To determine the Kinematic Viscosity of the given sample of oil at various
temperatures and to 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 centre 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. The 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 50 CC of oil is noted. With this arrangement variation of viscosity with
temperature can be studied.

FORMULA:

In the case of Red wood viscometer, the kinematic viscosity (υ) of

liquid and the time (t) required to pass 50 CC of liquid are correlated by expression.

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 υ =0.0026 – 1.175/t
Where,

υ - Kinematic Viscosity
t - Time in seconds to collect 50 cc of oil.

SIGNIFICANE:

 Pump design can be done with the help of viscosity.

 Pump operation of the engine depends on the proper viscosity of liquid

fuel.

 It is very important to know about the fluid flow through various objects.

 Conveying of fluid can done effect by means of viscosity data.

PROCEDURE:

 The Instrument is leveled with the help of the circular bubble and by
leveling foot screws.

 The water bath is 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 is recorded.

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  By Lifting the ball valve, 50 cc of the liquid is collected in the measuring
flask and the time required is measured for the same.

 The procedure is repeated for different temperatures by heating oil with

water bath.

OBSERVATION:

Sl. Temperature Time taken to collect Kinematic Viscosity

No. ( ºC ) 50cc of oil ( Sec ) (υ )
( Centistokes )

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 increase in temperature.

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EXPERIMENT NO. 9

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 REID VAPOR PRESSURE

AIM:
To determine the Reid Vapor Pressure of the given sample and for the
determination of vapor pressure of volatile non viscous petroleum products.

DEFINITION:

Vapor pressure is defined as the pressure exerted by the vapor of the liquid on
the walls of the closed container.
Or

It is the force which must be exerted on the liquid to prevent it from vaporizing
further

APPARATUS REQUIRED:
.
 Gasoline chamber
 Air chamber
 Pressure Gauge
 Cooling bath
 Water bath
 Thermometer.

SIGNIFICANCE:

 The temperature at which the vapor pressure of liquid equals 1 (one) atmospheric
pressure is designated as boiling point of liquid.

 In case of motor sprit, higher vapor pressure will lead to vapor lock of engine.

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  Vapor pressure is an important physical property.

 It is used in the consideration of storage and transportation.

PROCEDURE:

 Vapor pressure of all volatile fractions is measured by the testing apparatus at

(38+0.1 C).

 The apparatus consist of two chambers. The lower chamber is in the form of
cylindrical bomb for holding the test sample.

 Above this, there is air chamber which is a hollow cylindrical space, designed to
possess four times the bomb volume.

 The top portion of the chamber is fitted with the bourdon gauge for pressure
indication.

 For the test, the bomb is fist filled with the sample up to the brim and immediately
the valve is closed and connected to the air chamber.

 The apparatus is now immersed in a water bath kept at the mentioned

temperature. The maximum pressure indicated by the gauge is counted as the
Reid vapor pressure of the sample.

 LPG, gasoline, naphtha, jet fuels are tested like this. It is found that true vapor
pressure in most cases is higher than the indicated RVP, and the variation for
different fractions is different.

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  Maximum difference is indicated in the case of crude oils. Relative
expression ‘true vapor pressure to RVP’ is also some times indicated and
for gasoline it is in the range of 1.03 to 1.45, while for crude’s it goes up to
10.

RESULT:

The Reid vapor pressure of the given sample (gasoline) was found to
be………………

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31
 EXPERIMENT NO. 10
SMOKE POINT

AIM:
To determine the smoke point of the given samples.

THEORY:

Definition:
Smoke point is defined as the maximum height of flame in mm at which the
hydrocarbon will burn with out smoke.
The smoke point apparatus comprises four parts namely lamp body, candle socket
candle and stand. The lamp body with chimney is filled on the inside with a polished
block engraved scale mark in white. A gallery is secured in the lower part of the body. To
candle socket assembly is designed to give a smooth rise and fall over the total distance
of travel. To ensure interchangeability the candle is finished to close tolerance. The
assembly is mounted on a stand. The sample is burned in a standard lamp with a specified
wick for five minutes. The height of the flame is read when it leaves on smoky tail.

SIGNIFICANCE:

 This is an important test for evaluation of illuminating oils for their ability to burn
with out producing smoke ( For kerosene smoke point is 18mm )
 Used in the assessment of burning quality of aviation fuel. Higher the smoke point
better is its domestic use.
 It also serves as a guide to assess the aromatic content of kerosene. The tendency
of kerosene to smoke is mainly dependent upon types of hydrocarbon present.
Aromatic kerosene will smoke more readily than paraffinic kerosene.

 Aromatic > Napthene > Iso paraffin > Paraffin.

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PROCEDURE:

 The sample which is to be tested for smoke point was filled in the candle socket.

 The candle socket with wick was placed inside the apparatus.

 The wick had ignited and height of the flame without smoke was adjusted.

 The reading was noted in the scale and the experiment was repeated for different
gives samples.

RESULT:

The smoke point of the given samples were observed and tabulated.

S.No. Sample Smoke point (mm)

OBSERVATION:

33
S.No. Sample Smoke point (mm)

SMOKE POINT APPARATUS

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 EXPERIMENT NO. 11

RUST PREVENTING CHARACTERISTICS

Aim: To evaluate the ability of inhibited mineral oils, particularly steam-turbine oils, to
aid in preventing the rusting of ferrous parts should water become mixed with the oil.
Apparatus: Rusting test apparatus which consists of an oil bath, beaker with cover,
stirrer, test rod assembly, oven, thermometer etc.
Reagents and Materials: Distilled water, ISO VG 32 oil, tissue paper, ASTM
precipitation naphtha or isooctane.
Significance and Use: In many instances such as in the gears of steam turbine, water can
become mixed with the lubricant and rusting of ferrous parts can occur. This test indicates
how well inhibited mineral oils aid in preventing this type of rusting. This test method is
also used for testing hydraulic and circulating oils, including heavier-than-water fluids. It
is used for specification of new oils and monitoring of in-service oils.
Summary of the Test Method:
A mixture of 300 mL of the oil under test is stirred with 30 mL of distilled water at a
temperature of 60+-10C with a cylindrical steel test rod completely immersed therein. It is
recommended to run the test for 4 hr. The test rod is observed for signs of rusting.

Apparatus:
Oil bath: A thermostatically controlled liquid bath capable of maintaining the test sample
at a temperature of 60+_10C. An oil having a viscosity of approximately ISO VG 32 is

36
suitable for the bath. The bath shall have a cover with holes to accommodate the test
beakers.
Beaker: A 400 mL, Berzelius-type, tall-form heat resistant glass beaker without pourout.
Beaker Cover: A flat beaker cover of glass or polymer, kept in position by suitable means
such as a rim or groove. Two holes shall be provided on any diameter of the cover; one
for a stirrer and the other for the test rod assembly. In addition a third hole for a
thermometer.

Stirrer: A stirrer constructed entirely from stainless steel in the form of an inverted T.
Stirring Apparatus: Capable of maintaining a speed of 1000+-50 rpm.
Oven: Capable of maintaining a temperature of 650C.

Procedure:
1] Clean the beaker in accordance with good laboratory procedure, wash with distilled
water and dry in an oven.
2] Clean glass beaker cover and a glass stirrer by the same procedure.
3] Pour 300 mL of the oil to be tested into the beaker and place the beaker in the oil bath
held at a temperature that will maintain the oil sample at 60+_10C.
4] Insert the beaker into a hole of the bath cover and suspend in the hole with the beaker
rim resting on the bath cover. The oil level in the bath shall not be below the oil level in
the test beaker.
5] Cover the beaker with the beaker cover with the stirrer in position in the proper
opening.
6] Adjust the stirrer so that the shaft is 6 mm off center in the beaker containing the oil
sample and the blade is not more than 2 mm from the bottom of the beaker.
7] Suspend the thermometer through the hole in the cover .
8] Start the stirrer and when the temperature reaches 60+_10C, insert the steel test rod
such that its lower end is 13 to15 mm from the bottom of the beaker.
9] Continue stirring for 30 min to ensure complete wetting of the steel test rod.
10] With the stirrer in motion, remove the thermometer temporarily and add 30 mL of
distilled water through its hole and replace thermometer.

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11] Continue stirring at a speed of 1000+-50 rpm for 4 h from the time water was added,
maintain the temperature of the oil-water mixture at 60+_10C.
12] Stop stirring at the end of the 4-h period, remove the test rod, allow to drain and then
wash with ASTM precipitation naphtha or isooctane.

Interpretation of Results:
1] Perform all inspections at the end of the test to determine the condition of the test rod
without magnification under normal light. A rusted test rod is one on which any rust spot
or rust streak is visible.
2] In order to report an oil as passing or failing, conduct test in duplicate.
3] Report an oil as passing the test if both test rods are rust-free at the end of the test
period.
4] Report an oil as failing the test if both test rods are rusted at the end of the test period.
5] If one test rod is rusted while the other is free of rust, test two additional test rods. If
either of these latter test rods shows rusting, report the oil as not passing the test.

Result:
Thus, the oil passes/fails the test.

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Rusting Test Apparatus

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