DEPARTMENT OF CHEMICAL ENGINEERING

PETROLEUM REFINERY ENGINEERING LABORATORY

MANUAL

MALAVIYA NATIONAL INSTITUTE OF TECHNOLOGY

JAIPUR, RAJASTHAN

Lab Incharge : Dr. Shiv Om Meens

Technical Staff : Mr. Mohammad Ragib

 CONTENTS

SR.No. Name of the Experiment Page No.

1 PENSKY MARTENS APPARATUS 3-5

2 ABEL’S FLASH POINT APPARATUS 6-7

3 SAYBOLT VISCOMETER 8-11

4 DISTILLATION RANGE APPARATUS 12-15

5 SOFTENING POINT 16-18

6 SMOKE POINT 19-21

7 ANILINE POINT 22-23

8 CLOUD AND POUR POINT 24-27

9 REID VAPOR PRESSURE 28-30

10 CARBON RESIDUE APPARATUS 31-33

11 PENETRATION TEST 34-36

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 EXPERIMENT NO. 01
FLASH POINT AND FIRE POINT DETERMINATION USING

PENSKY MARTENS APPARATUS

AIM

To determine the flash point and fire point of fuel oils by using Pensky Martens apparatus
(closed type).

DEFINITION

FLASH POINT
The flash point of any oil is defined as the lowest temperature at which it forms vapors and
produces combustible mixture with air. The higher flash point temperature is always desirable
for any lubricating oil and lower flash point for any fuel. If the oil has the lower value of the
flash point temperature, it will burn easily and forms the carbon deposits on the moving parts.
The minimum flash temperature of the oil used in I.C engines varies from 2000C to 2500C.
When the oil is tested by using the open cup apparatus, the temperature is slightly more than
the above temperatures.

FIRE POINT
The fire point of any oil is the lowest temperature at which oil just begins to burn continuously.
Flash and fire point temperature differs by 300C to 500C when it is tested. However a greater
difference may be obtained if some additives are mixed with oil .The flash and the fire point
temperatures depends upon the volatility of the oil Fire and flash points are good indication of
relative flammability of the oil and also limits the operating temperature of oil. Except for the
safety from fire hazards, they do not have any significance for engine operation. However, fire
and flash points of lube oil are very good indication of the crankcase dilution. The fuel, which
leak into the crankcase, readily evaporate and burn at considerably lower temperature than the
temperature at which the oil would have burned, clearly indicates the degree of dilution. Flash
and fire point of the given light oil (Kerosene/Diesel) is determined by heating the oil in Pensky
Martens closed Cup apparatus and measuring the temperature at regular interval till it reaches
the temperature of flash and then the fire points is obtained and similarly by cooling the Flash
and fire points are observed.

SUMMARY OF METHOD

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 isthe
lowest temperature at which application of the test flame causes the vapour above the sample
to ignite.

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SIGNIFICANCE

 Flash point measures the response of the sample to heat and flame under controlled
laboratory conditions.
 It is only one of a number of properties which must be considered in assessing the
overall flammability hazard of a material.
 Flash point is used in shipping and safety regulations to define ‘flammable’ and
‘combustible’ materials.

APPARATUS

 Pensky Martens Closed Tester

 Sample of oil.

PROCEDURE

 Clean the cup and fill it with given sample of oil up to the filling mark.
 Cover the cup with lid.
 Thermometer is now inserted and should not touch the metallic cup.
 Heat the oil by means of electric heater so that the sample of oil gives out vapour at
the rate of 50C- 6 0C per minute.
 Stir the sample at one or two revolution per seconds.
 When the oil gives out vapour, introduce the test flame above the lid, wait for flash
with flickering sound.
 Introducing test flame should be continued at regular intervals until the first flash is
observed with peak flickering sound .The temperature corresponding to this flickering
sound is noticed and it is flash point temperature of the given sample of oil.
 Do not stir the sample while applying the test flame.
 Continue the process of heating and introducing the test flame until the oil will begins
to burn continuously ( for 5 seconds at least)and observe the temperature. This is the
fire point temperature of the given sample of oil.
 Repeat the test twice or thrice with fresh same sample of oil and observe the results.

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EXPERIMENTAL SETUP

OBSERVATION TABLE

(Yes/No) (Yes/No)
S.No. SAMPLES FLASH POINT (ºC) FIRE POINT(ºC)

RESULT
The flash point of the given oil is ……………0C
The fire point of the given oil is ……………..0C

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 EXPERIMENT NO. 02
FLASH AND FIRE POINT DETERMINATION USING

ABLE’S CLOSED CUP APPARATUS

AIM
To determine the flash and fire point temperatures of the given sample of oil using Able’s
closed Cup apparatus.

APPARATUS REQUIRED

1. Able’s closed cup apparatus 2. Sample of oil.

THEORY

Flash point of the oil is the lowest temperature at which the oil gives sufficient amount of
vapors resulting in a flash when a flame is brought near to it.

Fire point is the lowest temperature at which the oil gives sufficient amount of vapors
resulting in a continuous burning of the oil when the flame is brought near to it.

PROCEDURE

 Clean the cup and fill it with given sample of oil up to the filling mark.
 Insert the thermometer in the holder. Make sure that the thermometer should not
touch the metallic cup.
 Heat the oil by means of electric heater so that the sample of oil gives out vapour
at the rate of 100C per minute.
 When the oil gives out vapour, introduce the test flame above the oil, without
touching the surface of the oil and watch for flash with flickering sound.
 Introducing test flame should be continued at regular intervals until the first flash
is observed with peak flickering sound .The temperature corresponding to this
flickering sound is noticed and it is flash point temperature of the given sample of
oil.
 Continue the process of heating and introducing the test flame until the oil will
begins to burn continuously and observe the temperature. This is the fire point
temperature of the given sample of oil.
 Repeat the test twice or thrice with fresh same sample of oil and observe the
results.
 The observation is tabulated.

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EXPERIMENTAL SETUP

OBSERVATION TABLE

(Yes/No) (Yes/No)
S.No. SAMPLES FLASH POINT (ºC) FIRE POINT(ºC)

RESULT:
The flash point of the given oil is ……………0C
The fire point of the given oil is ……………..0C

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 EXPERIMENT NO. 03

SAYBOLT VISCOMETER

AIM

To determine the viscosity of the given petroleum products and to study the variation of
viscosity with respect to temperature.

APPARATUS REQUIRED
 Saybolt viscometer apparatus
 Thermometer (0 – 100 deg)
 Sample
 Stop watch
 Beaker (100 ml capacity)

THEORY
Viscometers are used to define the viscous properties of a fluid at ambient or defined
temperatures. They are commonly available in the form of a calibrated capillary tube through
which a liquid is allowed to pass at a controlled temperature in a specified time period. Other
methods include rotational viscometry and falling ball tests. Viscometers can have a few
different technologies by which they operate.

For rotational viscometry, torque is required to rotate a spindle at constant speed while
immersed into the sample fluid. The torque is proportional to the viscous drag on the immersed
spindle, and thus to the viscosity of the fluid. For falling ball technology, the viscosity is
proportional to the time required for a ball to fall through the test liquid contained in a precise
an temperature controlled glass tube. Capillary viscometers measure the flow rate of a fixed
volume of fluid through a small orifice at a controlled temperature.

The time it takes for a specific volume of fluid to pass through the orifice is proportional
to the fluid viscosity. However, it also depends on the density of the fluid since the denser the
fluid, the faster it will flow through the orifice. The property being measured is then the
kinematic viscosity and not the dynamic viscosity.

FORMULA
Kinematic viscosity, ν = At-B/t
Where, A=0.00226, B=1.95
A and B are constants.

SAFETY PRECAUTIONS
Do not connect bath to a power supply unless the bath is filled with oil.
Do not leave unit unattended, especially when operating at high bath temperatures.

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This could create a potential fire hazard.

SIGNIFICANCE
 It is used to find the viscosity of the fluid.
 Pump design can be done with the help of viscosity.
 Pump operation of one engine depends on the proper viscosity of fuels.
 Conveying of fluids can be done with the help of viscosity data.
 It is very important to know about the fluid flow through various objects.

EXPERIMENTAL PROCEDURE
 The viscometer was turned on after making sure that the bath was filled with oil.
 The bath was heated by means of water heater.
 The power switch was turned on. The bath temperature was maintained at various
temperatures.
 The bath was allowed to reach a steady temperature.
 The cork stopper is used to block off the outlet of one of the Saybolt viscometer
tubes.
 A measured quantity (+60 ml) of the sample was poured into the tube.
 The sample temperature was allowed to equilibrate with that of the bath (about 25
minutes).
 Simultaneously the Saybolt tube was uncorked (using the pull chain) and the
stopwatch was started.
 When the oil has reached the 60 ml mark, the stopwatch was stopped. The time was
recorded. The experiment was repeated for various temperatures.

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EXPERIMENTALSETUP

OBSERVATION TABLE

S. No. Temperature (0C) Time (Seconds) Kinematic viscosity

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GRAPH
1. Temp. Vs Time
2. Temp. Vs Kinematic viscosity

RESULT
Thus, the kinematic viscosity for given sample was determined for different temperatures and
tabulated. The graph was plotted and it was found that the kinematic viscosity decreases with
increase in temperature.

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 EXPERIMENT NO. 04

DISTILLATION APPARATUS

AIM
To determine the distillation characteristics (boiling range) of the given sample using
the distillation apparatus.

DISTILLATION
Thismethod of test covers the distillation of motor gasoline, aviation gasoline, aviation
turbine fuels, special boiling point spirits, naphtha, white spirit, kerosene, gas oils, distillate
fuel oils and similar petroleum products. A 100 ml sample is distilled under prescribed
conditions which are appropriate to its nature. Systematic observations of thermometer
readings and volumes of condensate are made, and from the data, the results of the test are
calculated and reported.
The distillation (volatility) characteristics of hydrocarbons have an important effect on their
safety and performance, especially in the case of fuels and solvents. The boiling range gives
information on the composition, the properties, and the behavior of the fuel during storage and
use. Volatility is the major determinant of the tendency of a hydrocarbon mixture to produce
potentially explosive vapors.
The distillation characteristics are critically important for both automotive and aviation
gasoline, affecting starting, warm-up, and tendency to vapor lock at high operating temperature
or at high altitude, or both. The presence of high boiling point components in these and other
fuels can significantly affect the degree of formation of solid combustion deposits.
Distillation limits are often included in petroleum product specifications, in commercial
contract agreements, process refinery/control applications, and for compliance to regulatory
rules.
This test method can be applied to contaminated products or hydrocarbon mixtures. This is
valuable for fast product quality screening, refining process monitoring, fuel adulteration
control, or other purposes including use as a portable apparatus for field testing.

TERMINOLOGY

Initial Boiling Point

The thermometer reading which is observed at the instant that the first drop of condensate falls
from the lower end of the condenser tube,

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End-Point or Final Boiling Point
The maximum thermometer reading obtained during the test. This usually occurs after the
evaporation of all liquid from the bottom of the flask. The term ‘maximum temperature’ is a
frequently used synonym.

Dry Point
The thermometer reading observed at the instant the last drop of liquid evaporates from the
lowest point in the flask. Any drops or film of liquid on the side of the flask or on the
thermometer are disregarded.

Decomposition Point
The thermometer reading which coincides with the first indication of thermal decomposition
of the liquid inthe flask.

Percent Recovered
The volume in ml of condensate observed in the receiving graduate, in connection with a
simultaneous thermometer reading.

Percent Recovery
The maximum percent that is recovered.

Percent Total Recovery

The combined percent recovery and residue in the flask.

Percent Loss
100 minus the percent total recovery.
Percent Residue
The percent total recovery minus the percent recovery, or the volume of residue in milliliters
if measured directly.
Percent Evaporated
The sum of the percent recovered and the percent loss.

PROCEDURE

 The given flask is to be thoroughly cleaned using solvent and dried.

 The given test sample is then 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 condensers with a cork.
The asbestos board is raised of lowered till the flask is properly supported.

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  The 100cc measuring cylinder is placed below the condenser outlet. The heater is then
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 process is at a uniform state.
 Middle boiling point is the temperature at which 50% of oil distills off.

SIGNIFICANCE
 Distillation (volatility) characteristics of petroleum products are indicative of
performance in their intended applications.
 Petroleum product specifications generally include distillation limits to ensure products
of suitable volatility performance.
 The empirical results obtained by use of this distillation method have been found to
correlate with automotive equipment performance factors and with other characteristics
of petroleum products related to volatility.
 For motor spirit the 10% distillation value gives an indication of the engine start
conditions, also the final boiling point.

EXPERIMENTAL SETUP

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OBSERVATION TABLE

S.No Volume of Distillate collected (ml) Temperature ºC

RESULT
The Distillation characteristics are studied for the given samples and the values are noted as
follows:
1. Initial boiling point = ºC
2. Middle boiling point = ºC
3. Final boiling point = ºC
4. Amount of distillate collected = mL
5. Vapor loss = mL

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 EXPERIMENT NO. 05

SOFTENING POINT

AIM

To determine the softening point of the given sample bitumen/grease using ball and ring
apparatus.

APPARATUS REQUIRED

 Ring and ball apparatus

 Steel balls
 Brass rings
 Thermometer
 Stirrer
 Water bath

SIGNIFICANCE

 To find the consistency of bitumen

 It is regarded by same indication of viscosity
 It is used in the designation of hard as oxidized bitumen.

THEORY

The softening point of bitumen or tar is the temperature at which the substance attains a
particular degree of softening. As per IS:334-1982, it is the temperature (in o C) at which a
standard ball passes through a sample of bitumen in a mould and falls through a height of 2.5
cm, when heated under water or glycerin at specified conditions of test. The binder should have
sufficient fluidity before its applications in road uses. The determination of softening point
helps to know the temperature up to which a bituminous binder should be heated for various
road use applications. Softening point is determined by ring and ball apparatus

APPARATUS

 Softening Point apparatus

 Steel balls-two numbers each of 9.5 mm dia. and weighing 0.05g.
 Brass rings-two numbers each having depth of 6.4 mm. The inside diameter at bottom
and top is 15.9 mm and 17.5 mm respectively.

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EXPERIMENTAL SETUP

PROCEDURE

 A beaker is taken and filled with ¾ of it with water/silicon oil/glycerine.

 The sample is placed in the ring and the steel ball is kept over the sample at the
middle of the ring.
 The whole ring and ball is immersed into the beaker which is filled with water.
 The water in the beaker is heated by electrical coil.
 A thermometer is inserted to note the temperature.
 As the temperature increase, the sample gets softens and the steel ball over the sample
gets immersed and finally drops out.
 The temperature at which the ball falls down from the ring is noted as softening point
of the sample.
 The ring is washed and replaced with another sample and the process is repeated.

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OBERVATION TABLE

Test 1 Test 2 Average

Temperature when
the ball touches
bottom in OC

RESULT

 The softening point of given sample is…OC

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 EXPERIMENT NO. 06

SMOKE POINT
AIM

This method is intended for the determination of smoke point of kerosene and other
volatile liquid fuels including gas turbine (jet) fuels.

DEFINITION

The maximum flame height in millimetres at whichkerosene or other volatile liquid

fuels including gas turbine (jet) fuelswill burn without smoking, when determined in the
apparatus and underspecified conditions.

OUTLINE OF THE METHOD

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

REQUIREMENTS:

 Smoke point apparatus

 Fuel samples

 Wick

Smoke Point Lamp - Constructed according to the specification given. The lamp consists of
an oil container provided with a wick tube and air vent, a gallery fitted with a wick guide and
provided with air inlets, a lamp body, and a chimney provided with a 50-mm scale specified

PRECAUTIONS

 The test shall normally be carried out at a room temperature of not less than 15°C; it is
recommended that the room temperature and the barometricpressure be recorded.
 Place the lamp in a vertical position completely protected from draughts.

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PROCEDURE

 20 ml of the previously filtered sample is introduced in the clean, dry oil container.
 A piece of wick is extracted, not less than 12’5 cm in length, with a suitable volatile
solvent and it is dried for half an hour at 100 to 110°C.
 The wick is soaked in the sample under test and is placed in the wick holder, carefully
easing out any twists arising from this operation. It is advisable to re-soak the burning
end of the wick in the sample.
 The wick holder is placed in the container and ensured that the air inlet is free from oil.
The wick is cut horizontally and trimmed to free the frayed ends so that 6 mm of wick
projects from the container.
 The oil container is maintained at a temperature of 20 to 25°C for 10 minutes. The lamp
is inserted and the wick is lighted.
 The wick is adjusted so that the flame is about 1 cm high and allows the lamp to burn
for 5 minutes. The wick is raised until a smoky tail appears, then lowered slowly
through the following stages of flame appearances:
 A long tip, smoke slightly visible, erratic and jumpy flame.

 An elongated pointed tip with the sides of the tip appearing concave upward.

 The pointed tip just disappears leaving a very slightly blunted flame Jagged, erratic,
luminous flames are sometimes observed near the true flame tip. These are to be
disregarded.

 The height flame is estimated to the nearest millimetre.

 The smoke point is recorded as observed. To eliminate errors due to parallax, the eye
of the observer should be slightly to one side of the centre line, so that a reflected image
of the flames seen on the scale on one side of the central vertical white line, and the
flame itself is seen against the other side of the scale. A sighting device may also be
used to eliminate parallax and to facilitate reading the flame height.
 The reading for both observations should be identical.

SIGNIFICANCE

 This is an important test for illumination oils for their ability to burn without producing
smoke.
 It is used in the assessment of burning quality of aviation fuel. Higher the smoke point
better is its domestic use.
 To find aromatic content of the kerosene.
 This test method provides an indication of the relative smoke producing properties of
kerosene’s and aviation turbine fuels in a diffusion flame. The smoke point is related
to the hydrocarbon type composition of such fuels.

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  Generally the more aromatic the fuel the smokier the flame. A high smoke point
indicates a fuel of low smoke producing tendency.
 The smoke point (and Illuminometer number with which it can be correlated) is
quantitatively related to the potential radiant heat transfer from the combustion
products of the fuel. Because radiant heat transfer exerts a strong influence on the
metal temperature of combustor liners and other hot section parts of gas turbines, the
smoke point provides a basis for correlation of fuel characteristics with the life of
these components.

EXPERIMENTAL SETUP

OBSERVATION TABLE

S. No. Sample(ml) Smoke Point(mm)

RESULT

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 EXPERIMENT NO. 07

ANILINE POINT

AIM

To determine the aniline point of the given sample.

APPARATUS
 Aniline Point Apparatus
 Aniline
 Oil sample

THEORY

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.

Equal volumes of the sample and aniline (5 ml each) are heated or cooled with stirring
in a jacketed test tube and temperature at which complete miscibility occurs is noted.

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

PROCEDURE

 The apparatus was dried and cleaned.

 10ml of aniline and 10ml of the sample were dried and pipetted into the test tube fitted
with stirrer and thermometer.

 The thermometer in the test tube was centered to make the immersion mark at the liquid
level; it is assured that the thermometer bulb does not touch the side of the tube.

 In the case of not mixing of aniline-sample at normal temperature, heat is applied

directly to the jacket tube so that the temperature raised at a rate of 1-3ºC/min till
complete miscibility was obtained.

 Stirring is continued and the mixture is allowed to cool at a rate of 0.5 to 1ºC/min.

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  Cooling is continued to a temperature of 1 to 2ºC below the first appearance of turbidity.

 The temperature at which the mixture suddenly became cloudy throughout is recorded
as the aniline point.

EXPERIMENTAL SETUP

OBERVATION TABLE

SR NO. Temperature ºC Aniline point (Yes/no)

RESULT

Result for the aniline point was found to be

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 EXPERIMENT NO. 08

CLOUD AND POUR POINT

AIM

To determine the Cloud point and pour point of the given sample.

REQUIREMENTS

Cloud and pour point apparatus, Thermometer, Ice crystals.

DEFINITIONS

The cloud point of a fluid is the temperature at which dissolved solids are no longer completely
soluble, precipitating as a second phase giving the fluid a cloudy appearance. This term is
relevant to several applications with different consequences.

Also, the pour point can be defined as the lowest temperature expressed in multiples of 3ºC at
which the oil is observed to flow when cooled and examined under prescribed conditions.

THEORY

Cloud point and pour point are indicators of the lowest temperature of utility for petroleum
products. Cloud Point gives a rough idea of temperature above which the oil can be safely
handled without any fear of congealing or filter clogging. The sample is periodically examined
while it is being cooled in the cloud and pour point apparatus. The highest temperature at which
haziness is observed (cloud point), or the lowest temperature at which the oil ceased to flow is
observed (pour point), is reported as the test result.

The cold filter plugging point test is used to determine the extent to which diesel fuel or gas oil
will flow, even though the temperature is below that at which wax crystals normally appear,
i.e. cloud point.

Pour point is a well established test to estimate the temperature at which a sample of oil
becomes sufficiently solid to prevent its movement by pumping. The pour point indicates the
waxy nature of the oils.

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 SAMPLES SHOWING CLOUD AND POUR POINT

PROCEDURE

Measuring cloud point of petroleum product:

 The test oil is required to be transparent in layers 40mm in thickness (in accordance
with ASTM D2500). The crystals of the sample typically first form at the lower
circumferential wall with the appearance of a whitish or milky cloud. The cloud point
is the temperature at which these crystals first appear.
 The test sample is first poured into a test jar to a level approximately half full. A cork
carrying the test thermometer is used to close the jar. The thermometer bulb is
positioned to rest at the bottom of the jar. The entire test subject is then placed in a
constant temperature cooling bath on top of a gasket to prevent excessive cooling.
 At every 1°C, the sample is taken out and inspected for cloud then quickly replaced.
Successively lower temperature cooling baths may be used depending on the cloud
point. Lower temperature cooling bath must have temperature stability not less than 1.5
K for this test.
Measuring pour point of petroleum product:

 Two pour points can be derived which can give an approximate temperature window
depending on its thermal history. Within this temperature range, the sample may appear
liquid or solid. This peculiarity happens because sample crystals form more readily
when it has been heated within the past 24hrs and contributes to the lower pour point.
 The upper pour point is measured by pouring the test sample directly into a test jar. The
sample is then cooled and then inspected for pour point as per the usual pour point
method.
 The lower pour point is measured by first pouring the sample into a stainless
steel pressure vessel. The vessel is then screwed tight and heated to above 100oC in an
oil bath. After a specified time, the vessel is removed and cooled for a short while. The
sample is then poured into a test jar and immediately closed with a cork carrying

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 the thermometer. The sample is then cooled and then inspected for pour point as per the
usual pour point method

EXPERIMENTAL SETUP:

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OBSERVATION TABLE

CLOUD POINT (ºC) POUR POINT(ºC)

S.No. SAMPLES (Yes/No) (Yes/No)

RESULT

The pour point of the given sample was found to be ---------0C.

The cloud point of the given sample was found to be ---------0C

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 EXPERIMENT NO. 09
REID VAPOR PRESSURE

AIM
Determination of the Reid vapor pressure of petroleum products.

APPARATUS
Reid vapor pressure bomb, Air chamber, liquid chamber, Bourdon pressure gauge, water
bath etc

INTRODUCTION

The objectives of this experiment is to determine the vapour pressure of petroleum products
and to compare the Reid vapour pressure of different petroleum products. Basically, there are
three types of oils that we used to differentiate the vapour pressure. They are kerosene, petrol
and lubricating oil. Meanwhile, the apparatus that was used to determine the Reid vapour
pressure was ASTM D323. The apparatus consist of two chambers which are the vapour
chamber (upper section) and liquid chamber (lower section), pressure gauge and water bath.
Each of the oil were poured into 3 different liquid chamber. When the water bath reached
37.8˚C, the vapour pressure apparatus will be placed in the water bath. When the reading is
stable or 5 minutes only then we can take the pressure reading. This step is performed for 3
times until 15 minutes to achieve the average pressure. Reid Vapour Pressure is the method to
test the measurement and volatility of crude oil and other petroleum products. RVP is stated in
kilopascal. Volatility is the property of a liquid fuel that defines its evaporation characteristics
where the volatility must be high enough to avoid vapor lock, vaporization loses, air pollution
and unsafe storage and handling. The average of RVP for diesel, kerosene and petrol are 3.0
kPa, 2.3 kPa and 32.7 kPa, respectively. Petrol has the highest RVP among these three
petroleum products, followed by diesel and kerosene, where kerosene has the lowest RVP.
Petrol is a high volatile petroleum product that can vaporize easily. Thus explained why it has
the highest vapour pressure.(Pandey et al., 2004). But, petrol has a lower viscosity. The lower
the viscosity, the higher the RVP. As a conclusion, the actual value obtained were different
with expected RVP value from the theory. It is because the device was worn out. Hence, does
not producing an accurate result. Next, the petroleum product that was contaminated and
influenced the result.

THEORY

Vapor pressure is very important physical property of volatile liquids. This is because it is used
to determine the vapor pressure at 37.8oC of petroleum products and crude oils at above 0oC
initial boiling point. At atmospheric pressure, when the liquid has reached its boiling point, the
liquid changes its state from liquid to a gas through its bulk and it’s called normal boiling point.

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The tendency of molecules to escape from the liquid phase to gases phase depends on the
temperature, vapor pressure and volatility. The higher volatility and higher vapor pressure, will
be low tendency of molecule to escape its phase. Petroleum products are usually grouped into
three categories which are Light distillates (LPG, gasoline, naphtha), Middle distillates
(kerosene, diesel), and lastly Heavy distillates (heavy fuel oil, lubricating oils, wax, asphalt)
which result kerosene and diesel are classified under middle distillate and petrol is light
distillate. The classification of petroleum product distinguish the carbon contain. Heavy
distillate contains high number of carbon than the others. The lower the number of carbon,
which at the top of the fractionating column have lower boiling points, which means the higher
the vapour pressure and the higher volatility of a fuel by increasing the temperature, which
means a highly volatile fuel will vaporize more at a faster rate than a fuel with a lower volatility.
High volatile oil which are petroleum product at top distillate tend to flame and explode easily
than the fractions at the bottom. The RVP for petrol is typically in the range from 40 to 60 kPa
or 6 to 9 psia (Joseph E. Shepherd, 2007).

EXPERIMENTALSETUP

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PROCEDURE

 With everything in readiness take the chilled sample container, uncap it and insert the
chilled transfer connection and air tube.
 Quickly place chilled liquid chamber in an inverted position over delivery tube of sample
transfer apparatus.
 Invert entire system rapidly so that liquid chamber is finally in an upright position with
delivery tube touching the bottom of liquid chamber. Immediately attach air chamber to the
liquid chamber.
 Turn the assembled vapor pressure apparatus upside down to allow sample in liquid
chamber to run into air chamber.
 With apparatus still inverted, shake vigorously 8 times in a direction parallel to length of
apparatus.
 Immerse assembled apparatus in bath maintained at 37.8°C.
 Repeat the above procedures at the intervals of not less than 2 min until last 2 readings
are constant, indicating that state of equilibrium has been obtained.
 Take the pressure reading on bourdon pressure gauge.

OBSERVATIONTABLE

S.NO. Temperature (℉/oC) Barometric

Pressure(mmHg)

1
2
3
4
5

RESULT:

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 EXPERIMENT NO. 10
CARBON RESIDUE APPARATUS
AIM
To be able to predict and study the carbon deposit in lubricating oils under high
temperature condition in inert atmosphere.

INTRODUCTION
Carbon residue is the amount of carbon that is made by a chemical process, such as heating up
oil. It is mainly considered to be a by-product of fuel. When gasoline is burned and used by a
motor vehicle engine, it produces exhaust that contains Carbon Monoxide.
Carbon residue is what the leftover particles of a fuel product are transformed into. There are
tests that can determine the amount of residue that remains after certain fuels are heated or
burned.

THEORY
The carbon residue of a fuel is the tendency to form carbon deposits under high temperature
conditions in an inert atmosphere. It may be expressed as Ramsbottom Carbon Residue
(RCR).The carbon residue value is considered by some to give an approximate indication of
the combustibility and deposit forming tendency. The carbon residue provides information on
the carbonaceous deposits which will result from combustion of the fuel. For fuels with a high
carbon- high carbon/hydrogen ratio, it is proved more difficult to burn them fully, which results
in increased deposits in the combustion and exhaust spaces. Fuels with a high carbon residue
value may cause problems in older engines when they are operating under part load conditions.
The carbon residue value of a fuel depends on the refinery processes employed in its
manufacture.

If lubricating oil is heated to a high temperature in an enclosure where there is a limited

supply of air, the greater part of the oil will be distilled and there will remain a residue of
carbon. The amount of this carbon residue in lubricating oil is an indication of the extent of its
decomposition when used for high-temperature lubrication

DESCRIPTION
This test method covers the determination of the amount of carbon residue left after evaporation
and pyrolysis of an oil, and it is intended to provide some indication of relative coke-forming
propensity. This test method is generally applicable to relatively nonvolatile petroleum
products which partially decompose on distillation at atmospheric pressure.

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This test method also covers the determination of carbon residue on 10 % (V/V) distillation
residues. Petroleum products containing ash-forming constituents as determined by Test
Method D482, will have an erroneously high carbon residue, depending upon the amount of
ash formed.

EXPERIMENTAL SETUP

PROCEDURE
 Weight the coking bulb glass while it's empty, and record it.
 Inject the sample by syringe to the bulb and weight the bulb with the sample.
 Put the bulb with the sample at 550 C for 20min. Until the sample is burning.
 Cool the coking bulb in the dryer for 10 min, then weight it.

APPARATUS & REAGENT REQUIRED

 Ramsbottom Carbon Residue Tester

 Balance with a set of weight
 Lubricating oil
 10 ml syringe with needle
 glass coking bulb
 Tongs

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OBSERVATION
Weight of empty coking bulb = W1 gms
Weight of coking bulb with sample = W2 gms
Weight of coking bulb with Residue = W3 gms

Percentage of Carbon Residue = (W3-W1) / (W2-W1) X 100

RESULT
Percentage of Carbon Residue…..

PRECAUTION

 The device is working at extremely hot temp. 550 C, avoid any direct contact by hand

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 EXPERIMENT NO. 11
PENETRATION TEST

AIM

To determine the penetration of the given sample with the help of Penetrometer.

APPARATUS
 Penetrometer,
 Needle,
 Sample,
 Cup,
 Weights.

DESCRIPTION
Consistency or yield value is expressed in terms of penetration, which is defined as “the
distance in tenth of millimeter that a standard cone or needle penetrates vertically into the
sample,under the standard conditions of load, temperature and time. Consistency of a sample
depends onthe structure and interaction of the gelling elements in it and to some extent on the
viscosity of oilused.The consistency is determined by using Penetrometer. The apparatus
consists of

 Heavybase (of cast iron alloy): It is one which is provided with spirit level, leveling
screws and a plain table, over which a box containing the sample under test is placed.

 Vertical support is an iron rod fitted to the base. On this are slotted marks, around
which a holder can be moved up and down. The holder has a screw, which can be
tightened in any of the slots.

 Circular dial: The holder carries a circular dial gauge, which is graduated in
Millimeters

 Moving dial rod: It is arranged behind the dial by a mechanical mechanism. The rod
is provided with a clutch arrangement for disconnecting or connecting it to the
circular dial.

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EXPERIMENTAL SETUP

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 PROCEDURE

 The apparatus is leveled, the cone or needle cleaned and the sample under-test,
in a box, is placedbelow the cone or needle.
 The height of the cone or needle is so adjusted, that the tip of the cone orneedle
just touches the sample.
 Initial dial reading is noted.
 The cone is then released for exact 2 sec,by pressing a button is released and
final dial reading is noted.
 The differences of the two dial readings given the penetration.This is repeated
for three times and noted the total penetration in 6sec.

OBERVATION TABLE

Time Initial Reading Final Reading Penetration

(sec) Of Dial Of Dial d2-d1 mm
d1 mm d2 mm

RESULT

Penetration is found to be decreased with increasing temperature and time.

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