department of petroleum engineering lab manual...
TRANSCRIPT
Department
of
PETROLEUM ENGINEERING
Lab Manual for
PETROLEUM PRODUCT TESTING LAB
(IV-B.Tech I-Sem )
Prepared by
Dr T SRINIVAS
HOD & Asst. Professor
Department of Petroleum Engineering
NRI INSTITUTE OF TECHNOLOGY
LIST OF EXPERIMENTS
S.NO: NAME OF THE EXPERIMENT NAME OF THE EQUIPMENT PAGE NO:
1 DETERMINATION OF DISTILLATION
CHARACTERISTICS OF CRUDE OIL & ITS PRODUCTS
PETROLEUM DISTILLATION APPARATUS, THERMOMETER
1-3
2 DETERMINATION OF REID VAPOR
PRESSURE OF CRUDE OIL AND GASOLINE GASOLINE CHAMBER, AIR
CHAMBER, PRESSURE GAUGE, WATER BATH
4-6
3 DETERMINATION OF VISCOSITY OF DIESEL
AND TRANSFORMER OILS CANNON FENSKE VISCOMETER 7-9
4 DETERMINATION OF SMOKE POINT OF
KEROSENE SMOKE POINT APPARATUS 10-11
5 DETERMINATION OF CARBON RESIDUE
(CONRADSON) TEST CARBON RESIDUE CONRADSON
APPARATUS 12-15
6 DETERMINATION OF FLASH AND FIRE POINTS OF GASOLINE, KEROSENE AND
OTHER PRODUCTS
FLASH AND FIRE POINT APPARATUS
16-19
7 ESTIMATION OF WATER CONTENT IN
PETROLEUM PRODUCTS DEAN & STARK APPARATUS 20-22
8 ESTIMATON OF CALORIFIC VALUE OF
LPG/GASOLINE
JUNKER’S GAS CALORIMETER 23-29
9 DETERMINATION OF ANILINE POINT OF
GASOLINE AND DIESEL OIL ANILINE POINT TESTER 30-33
10 DETERMINATION OF SOFTENING POINT OF
BITUMEN RING AND BALL APPARATUS 34-37
11 DETERMINATION OF CLOUD AND POUR
POINT OF PETROLEUM PRODUCTS CLOUD AND POUR POINT
APPARATUS 37-39
12 DETERMINATION OF COROSSIVENESS OF
PETROLEUM PRODUCTS (VISUAL METHOD)
COPPER CORROSION APPARATUS
40-41
1
EXPERIMENT NO.1
Determination of Distillation characteristics of crude oil & its products
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.
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.
2
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:
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 ………………
3
Distillation Apparatus Schematic Diagram
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 ………………
Thermometer
Distillation Flask
Condenser Bath
Receiver
Heat Source
Sample
4
EXPERIMENT NO. 2
DETERMINATION OF REID VAPOR PRESSURE OF CRUDE OIL AND GASOLINE
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.
Vapor pressure is an important physical property.
It is used in the consideration of storage and transportation.
5
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.
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………………
6
Vapour Pressure (Reid Method)
Gauge
Connector
Sample Container
Barrel
Connector
Vapour Pressure (Reid
Method)
Gauge
Constant
Temperature
Bath
Temperature
Controller
Stirrer
7
EXPERIMENT NO. 3
DETERMINATION OF VISCOSITY OF DIESEL AND TRANSFORMER OILS
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.
υ =0.0026 – 1.175/t
Where,
υ - Kinematic Viscosity
t - Time in seconds to collect 50 cc of oil.
8
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.
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:
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.
Sl.
No.
Temperature
( ºC )
Time taken to collect 50cc of
oil ( Sec )
Kinematic Viscosity (υ )
( Centistokes )
9
10
EXPERIMENT NO. 4
DETERMINATION OF SMOKE POINT OF KEROSENE
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.
11
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:
S.No.
Sample
Smoke point (mm)
SMOKE POINT APPARATUS
12
Chimney
Scale
Flame
Lamp
Stand
Lamp Holder
Flame Shape
13
EXPERIMENT NO. 5
DETERMINATION OF CARBON RESIDUE (CONRADSON) TEST
AIM: To determine the carbon residue of the given sample of lubricating oil / Fuel.
APPARATUS:
Carbon residue (Conradson) apparatus,
Analytical balance with Weight box.
THEORY
Most of the lubricant oils are containing high percentage of carbon in combined form and fuels
containing less percentage of carbon in combined form. On heating, they decompose depositing a
certain amount of carbon. The deposition of such carbon in machine is intolerable, particularly in
internal combustion engines and air compressors. A good lubricant should deposit least amount
of the carbon in use.
PROCEDURE
1. The weighed porcelain or silica crucible with approximately 2 grams of sample is placed in the
center of skid more crucible.
2. The skid more crucible is provided with lid, having a small tube type opening for the escape of
volatile matter.
3. The combination is then placed in a wrought iron crucible covered with chimney shaped iron
hood.
4. The wrought iron crucible is heated slowly till flame appears. Slow heating continues for 5
minutes more.
5. Finally, strong heating is done for about 15 minutes till vapors of all volatile matter are burnt
completely.
6. Apparatus is then allowed to cool and weight of residue left is determined.
7. The result is expressed as percentage of the original weight of oil taken.
14
15
16
EXPERIMENT NO. 6
DETERMINATION OF FLASH AND FIRE POINTS OF GASOLINE, KEROSENE AND
OTHER PRODUCTS
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
(closed cup)
Fuel oils and lubricating
oils, bitumen other than
cutback bitumen.
>49
Cleveland
(open cup)
Petroleum products except
fuel oils
<79
17
SIGNIFICANCE:
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.
18
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 =
19
FLASH AND FIRE POINT APPARATUS
20
EXPERIMENT NO. 7
ESTIMATION OF WATER CONTENT IN PETROLEUM PRODUCTS
AIM: To Estimate the Moisture Content of the given Liquid Fuel using Dean & Stark
Apparatus.
APPARATUS REQUIRED:
Dean & Stark Apparatus
Appropriate Solvent
Fuel Sample
Glass pieces
DEAN & STARK METHOD:
The Classical Method of Determining the Water content in oil is Dean & Stark
Distillation Method (ASTM D95) This method is easy and requires a comparatively large volume
of sample to ensure accuracy, which is rarely used in oil analysis.
A known volume of fuel sample is placed in a flask with equal volume of organic solvent
such as xylene or toluene. An organic solvent must be insoluble with water. It should have a
higher boiling point than water. It should be less dense than the water and it should to be safe
to use. The flask containing the sample and with the organic solvent is attached to a condenser by
a side arm and the mixture is heated up. The water in the sample gets evaporates and moves up
into the condenser where it is cooled and converted back into liquid water, which then trickles
into the graduated tube. When no more water is collected in the graduated tube, distillation is
stopped and the water present in the liquid fuel is measured.
THEORY:
Water perhaps the most harmful of all contaminants with the exception of particles.
While the presence of water is often overlooked as the primary root cause of machine problems,
21
excess moisture contamination can lead to premature oil degradation, increase in corrosion
due to the increased water content.
PROCEDURE:
The given sample was added with organic solvent (Xylene or Toluene) are mixed in
proper proportion
Then it is taken into the flask of Dean & Stark Apparatus.
Glass beads may be added to reduce bumping if necessary.
The mixture of sample was heated and the vapours is comes out at the top and it is
condensed in the condenser.
The condensate of water and the solvent at the bottom of the graduated tube. Due to the
difference in density water content settles at the bottom of the tube.
The amount of water collected was measured.
The data was noted and recorded.
RESULT:
The amount of moisture content in the given sample was found to be …………ml.
22
EXPERIMENTAL SETUP FOR MOISTURE CONTENT DETERMINATION
23
EXPERIMENT NO. 8
ESTIMATON OF CALORIFIC VALUE OF LPG/GASOLINE
AIM
To find the calorific value of given gaseous fuel.
APPARATUS
i)Calorimeter
a)Main calorimeter body
b)Three thermometers
ii)Gas flow meter
a)Main gas flow meter body
b)Inlet / outlet nozzles
c)Union net with washer for thermometers
iii)Pressure governor
a)Pressure governor body
b)Balancing beam arrangement
c)Counter balance tube
d)Inlet and outlet union nuts with washers and
iv) Jars 2000ml & 50 ml.
PROCEDURE
1. Pour water into the governor till water starts overflowing through the overflow passage.
2. Replace and tighten the over flow nut.
3. Insert three thermometers provided with calorimeter into the rubber corks.
4. Insert rubber corks with thermometers into their places in calorimeter.
5. Insert burner into its support rod in the bottom of the calorimeter and turn the knurled knob so
that the burner is fixed tightly. The burner must go into the center of the calorimeter body.
6. Connect the calorimeter, the flow meter and the pressure governor as shown in figure using
rubber tubing provided. Do not connect gas supply line. Take care to see that the water regulator
of calorimeter is in OFF position.
24
7. Turn water regulator knob on calorimeter to ON position. Allow water to flow through the
calorimeter from overhead tank/ tap. Allow water to flow for 3 to 4 min into laboratory sink,
through the calorimeter.
8. Ensure that outlet tap of governor is closed. Connect gas supply line to governor inlet. Remove
burner from calorimeter then open governor outlet tap. Allow gas to pass through the burner.
9. Light up the burner by holding a lighted match stick near the mesh at the top.
10. Adjust the air regulator sleeve at the bottom of the burner to get a blue, non-luminous flame.
Fix the lighted burner back into position.
11. Adjust water regulator on calorimeter to get a temperature difference of 12C to 15 C between
the inlet water & outlet water as indicated by the respective thermometers at the top of the
calorimeter.
12. Allow 20 to 30 min for outlet water temperature to become steady.
13. Measure the water flow rate with the help of measuring jar. Simultaneously, note the flow
meter reading.
14. Note down the inlet &outlet water temperatures.
15. Repeat the test with same volume of gas 3 or 4 times and take average temperatures of inlet
and outlet water.
CALCULATIONS
The formula to be used to calculate the calorific value to the test gas is as follows
25
PRECAUTIONS
1. Test reading are to be taken only after steady condition are reached
2. Formation of steam should not be allowed. If there is formation of steam, then increase the flow
of water or reduce the gas flow rate
3. Water flow rate should be steady.
4. The inner float of the pressure governor should not be removed since the outlet pressure may
vary when refitted.
RESULT
The calorific value gaseous fuel is _____________ Kcal/m3
JUNKER’S GAS CALORIMETER
26
JUNKER’S GAS CALORIMETER
27
EXPERIMENT NO. 9
DETERMINATION OF ANILINE POINT OF GASOLINE AND DIESEL OIL
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. 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
28
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:
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 =
=
29
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.
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 =
30
Aniline Point
Apparatus
Outer Jacket
TestTube
Thermometer
Sample
Aniline
Stirrer
Rubber Bank
31
EXPERIMENT NO. 10
DETERMINATION OF SOFTENING POINT OF BITUMEN
Aim:
To determine the softening point of the given semisolid bituminous substance.
THEORY:
Penetration Index:
It is defined as the depth of penetration
Penetration index = 1/10th mm of the penetration needle depth
PENETRATION TEST:
Penetration apparatus – any apparatus which permits the needle holder to move vertically
without friction and is capable of indication of the depth of penetration to the nearest 0.1mm
The weight of the spindle shall be 47.5 ± 0.05 g. The total weight of the needle and
spindle assembly shall be 50 ± 0.05 g provided for total load. The surface on which the sample
container rests shall be flat.
PENETRATION BITUMEN:
Bitumen compromise of mixture of hydrocarbon molecules and thermoplastic
behaviour. There are a number of different classes of bitumen’s derived from crude oil refining.
These include penetration bitumen, viscosity graded asphalts, oxidized bitumen, air blown
bitumen, hard bitumen and cut back bitumen.
The grades of product in each class are generally defined on the basis of a combination
of two of three characteristics – penetration value at 250oc. These bitumens are defined by the
upper and lower limits of penetration values. Common grades of penetration bitumen in use vary
from 15 to 450 penetrations. Specific ranges of softening point are required for particular
penetration grade bitumen. This ensures the penetration index in the range from -1 to +1.
32
SAMPLE CONTAINER:
A metal or glass cylindrical flat bottomed container of essentially the
following dimensions shall be used.
Penetration below 200 - diameter 55 mm
Internal depth 35mm
Penetration between 200-300 - diameter 70 mm
Internal depth 45 mm
TIME DEVICE:
Time for a count interval must be 5 +/- 0.1 seconds
PRECAUTION:
Don’t insert the needle /cone before going to do the experiment.
The needle should make contact with surface of sample
SIGNIFICANCE:
It is used to measure of consistency of a bituminous material.
Higher the value Softer the material.
The Penetration index of a sample determines its application.
PROCEDURE:
The needle holder and penetration needle was examined and inserted.
Given sample was placed in the sample container under standard conditions.
The needle was positioned so that its tip just makes contact with the surface of
sample.
The needle holder was released and the distance penetrated in tenth of millimeter
was noted.
33
The experiment is repeated for different samples and for different temperature
conditions.
RESULT:
The penetration test is performed and the following results are obtained.
S.No.
Temperature
( º C )
Penetration Index 1/10th of mm
Solid cone
Hollow cone
Needle
OBSERVATION:
S.No.
Temperature
( º C )
Penetration Index 1/10th of mm
Solid cone
Hollow cone
Needle
34
Schematic Representation
Gauge in tenths of mm
Needle Release Mechanism, 5 seconds
Loaded Weight to 100g
Standard Penetration Needle
Asphalt Sample at 250 C
Needle Penetration
35
EXPERIMENT NO. 10
DETERMINATION OF SOFTENING POINT OF BITUMEN
AIM: This test method covers the determination of softening point of bitumen in range from 30-
80C using the ring-and-ball apparatus immersed in distilled water.
Apparatus Required:
Rings - Two square-shouldered brass rings conforming to the standard dimensions
Pouring Plate - A flat, smooth, brass plat approximately 50 by 75 mm (2 by 3 in.)
Balls - Tw3o steel balls, 9.5 mm (3/3 in.) in diameter, each having a mass of 3.50
0.05 g.
Ball-Centering Guides - Two brass guides for centering the steel balls, on for each ring.
Bath - A glass vessel, capable of being heated, not less than 85 mm in inside diameter
and not less than 120 mm in depth from the bottom of the flare.
Ring Holder and Assembly - A brass holder designed to support the two rings in a
horizontal position.
Thermometers - An ASTM Low Softening Point Thermometer, having a range from -
2 to +80 C.
Preparation of Test Specimen:
1. Do not start unless it is planned to complete preparation and testing of all asphalt
specimens within 6 h.
2. Heat bitumen sample with care, stirring frequently to prevent local over heating,
until it has become sufficiently fluid to pour.
3. Stir carefully to avoid incorporation of air bubbles in the sample.
4. Take no more than 2 h to heat an asphalt sample to its pouring temperature; in no
case shall this be more than 110 C above the expected softening point of the asphalt.
5. Heat the two brass rings (but not the pouring plate) to the approximate pouring
temperature, and place them on the pouring plate treated with one of the release
agents.
36
6. Pour a slight excess of the heated bitumen into each ring, and then allow the
specimens to cool in ambient air for at least 30 min.
7. When the specimens have cooled, cut away the excess bitumen cleanly with a
slightly heated knife or spatula, so that each disk is flush and level with the top of
its ring.
Procedure:
1. Take freshly boiled distilled water. The starting bath temperature shall be 5 1 C.
2. Assemble the apparatus with the specimen rings, ball-centering guides, and
thermometer in position, and fill the bath so that the liquid depth will be 105 3
mm with the apparatus in place.
3. Place the bath in the ice water, and using forceps, place the two steel balls in the
bottom of the bath and maintain the starting temperature of 5 1 C for 15 min.
4. Again using forceps, place a ball from the bottom of the bath in each ball-centering
guide.
5. Heat the bath from below so that the temperature indicated by the thermometer rises
at a uniform rate of 5 C . The maximum permissible variation for any 1-min. period
after the first 3 min shall be 0.5 C.
6. Record for each ring and ball the temperature indicated by the thermometer at the
instant the bitumen surrounding the ball touches the bottom plate.
Experimental Data and Results: Tabulate the data in the given Test Data Sheet. When using
ASTM Thermometer, report to the nearest 0.2 C.
The single-operator standard deviation has been found to be 0.41 C. Therefore, results of two
properly conducted tests by the same operator on the same sample of bitumen should not differ by
more than 1.2 C.
Discussion: Discuss about the results in the given Test Data Sheet.
37
TABLE
SOFTENING POINT OF BITUMEN
Sample No. __________ Description of Material: ____________________________________
Tested by: _______________________________ Date of Testing: _______________________
Test Temperature: ___________ C; Rate of Heat: ___________ C;
Ring No. Instant Temperature, C Softening Point, Average C
1
2
Ring No. Instant Temperature, C Softening Point, Average C
1
2
Ring No. Instant Temperature, C Softening Point, Average C
1
2
Discussion of Test Results: _______________________________________________________
_____________________________________________________________________________
_____________________________________
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EXPERIMENT NO.11
DETERMINATION OF CLOUD AND POUR POINT OF PETROLEUM PRODUCTS
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.
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.
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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:
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.
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
40
EXPERIMENT – 12
COPPER STRIP CORROSION TEST
AIM
To detect the corrosiveness of the given sample using copper strip corrosion test.
PRINCIPLE
The method covers the detection of corrosiveness to copper of aviation gasoline from tractor fuel,
solvent, kerosene, diesel, fuel oil, lube oil, certain other petroleum products. a polished copper
strip is immersed in a given quantity of sample and heated at a temperature and for a time
characteristics of the material being tested. At the end of
this period, the copper strip is removed, washed and compared with copper strip corrosionstandar
ds. It is particularly important that all types of feed sample which should pass a tarnished strip
classification. We collected clean glass bottles, plastic bottles or other suitable containers that will
not affect the corrosiveness properties of the sample.
REQUIREMENTS
Copper strip corrosion test bomb
constant temperature water bath
polishing ice
glass test tube
polishing paper
SIGNIFICANCE AND USE
This test method is suitable for setting specifications, for use as an internal
qualitycontrol tool, and for use in development or research work on industrial aromatichydrocarb
ons and related materials. It also gives an indication of the presence of certain corrosive substances
which may corrode equipment, such as acidic compounds or sulfur compounds.
PROCEDURE
The test is to be operated at 50oc constant temperature.
The bath is set at the desired working temperature and waits for 20 minutes of time after
the start.
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The copper strip is prepared for performing test. It is washed properly with solvent
(acetone) and surface of strip is prepared by rubbing with silicon carbide grid paper.
Clamp the strip with ice and polish it until uniform rubbing, when strip is clean immerse it
in prepared sample.
The strip is kept into 30 ml of sample which is kept inside the test bomb and the lid is
screwed tight.
After two hours in the bath the bomb is withdrawn and it is cooled with water.
The bomb is opened, the test tube is taken out and carefully the strip is
withdrawn from the sample.
The strip is compared with ASTM corrosion standards comparison chart and report the
tarnish level.
Result
The corrosiveness of the given sample is found out using the copper strip and comparing it with
ASTM standards and its value is found to be --------------------------