Professional Documents
Culture Documents
Flash Point and Fire Point - Final
Flash Point and Fire Point - Final
Flash Point and Fire Point - Final
1.When you handle chemicals wear eye protection (chemical splash goggles or full
Face shield).
2. When you work with furnaces for heat treatment procedures or other thermally
activated equipment you should use special gloves to protect your hands.
3. Students should wear durable clothing that covers the arms, legs, torso and feet.
4. To protect clothing from chemical damage or other dirt, wear a lab apron or lab coat. Long
hair should be tied back to keep it from coming into contact with lab chemicals Or flames.
5. In case of injury (cut, burn, fire etc.) notify the instructor immediately.
6. In case of a fire or imminently dangerous situation, notify everyone who may be
affected immediately; be sure the lab instructor is also notified.
7. If chemicals splash into someone's eyes act quickly and get them into the eye wash station,
do not wait for the instructor.
8. In case of a serious cut, stop blood flow using direct pressure using a clean towel, notify the
lab instructor immediately.
9. Eating, drinking and smoking are prohibited in the laboratory at all times.
10. Never work in the laboratory without proper supervision by an instructor.
11. Never carry out unauthorized experiments. Come to the laboratory prepared. If you are
unsure about what to do, please ask the instructor.
Preparation means coming to the lab classes with neatly drawn circuit diagram
/experimental setup /written programs /flowchart, tabular columns, formula, model
graphs etc in the observation notebook and must know the step by step procedure
to conduct the experiment.
Observation means taking correct readings in the proper order and tabulating the
readings in the tabular columns.
Result means correct value of the required parameters and getting the correct
shape of the characteristics at the time of reporting of the faculty.
Viva voice means answering all the questions given in the manual pertaining to the
experiments.
Full marks will be awarded if the students performs well in each case of the
above component
CONTENT
Sl.
No.
Date
Page
Marks
Staff
Initials
1.
2.
Distillation Characteristics
3.
API Gravity
4.
Softening Point
5.
Aniline Point
6.
7.
8.
Bomb Calorimeter
9.
KFR Titration
10.
Centrifuge
11.
12.
Determination of Kinematic
viscosity
13.
AIM
To determine the flash point and fire point of fuel oils by using Pensky Martens apparatus
(closed type).
DEFINITION
FLASH POINT
The lowest temperature of the sample, corrected to a barometric pressure of 101.3 kPa 760
mm Hg , at which application of a test flame causes the vapour of the sample to ignite under
specified conditions of test.
FIRE POINT
The fire point, is defined as the temperature at which the vapour continues to burn after being
ignited.
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 is
the lowest temperature at which application of the test flame causes the vapour above the
sample to ignite.
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
TABULATION
S.No.
SAMPLES
FIRE POINT(C)
PREPARATION OF SAMPLE
Samples of asphalts or very viscous materials may be warmed until they are reasonable fluid
before they are tested. However, no sample should be heated more than is absolutely
necessary. It shall never be heated above a temperature of 17C ( 30F ) below its expected
flash point.
APPARATUS SPECIFICATIONS
A typical assembly of the apparatus, gas heated, is shown in Fig. The apparatus shall consist
of a test cup, cover, and stove conforming to the following requirements.
Cup - The cup shall be of brass, or other non-rusting metal of equivalent heat conductivity,
and shall conform to the dimensional requirements
Cover Proper - The cover shall be brass, and shall have a rim projecting downward almost to
the flange of the cup. The rim shall fit the outside of the cup with a clearance not exceeding
0.36 mm 0.014 in on the diameter.
Shutter - The cover shall be equipped with a brass shutter approximately 2.4 mm ( 3/32 in )
thick operating on the plane of the upper surface of the cover. cover openings shall be exactly
open and the tip of the exposure tube shall be fully depressed.
Flame Exposure Device - The flame-exposure device shall have a tip with an opening 0.69
to 0.79 mm (0.027 to 0.031 in) in diameter. This tip shall be made preferably of stainless
steel, although it may be fabricated of other suitable metals
Pilot Flame - A pilot flame shall be provided for automatic relighting of the exposure flame.
Stirring Device - The cover shall be equipped with a stirring device mounted in the centre of
the cover and carrying two 2-bladed metal propellers.
Stove
Heat shall be supplied to the cup by means of a properly designed stove which is equivalent
to an air bath. The stove shall consist of an air-bath and a top plate on which the flange of the
cup rests.
Air Bath
The air bath shall have a cylindrical interior and shall conform to the dimensional
requirements in Fig.
Top Plate
The top plate shall be of metal, and shall be mounted with an air gap between it and the air
bath.
PROCEDURE
RESULT
Flash point and fire point of given samples are ________________
is _______ oC
2. DISTILLATION CHARACTERISTICS
SCOPE
To determine the distillation characteristics (boiling range) of the given sample using
the distillation apparatus.
DISTILLATION
This method 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.
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.
OBSERVATION
S.No
Temperature C
TERMINOLOGY
PROCEDURE
RESULT
The Distillation characteristics are studied for the given samples and the values are noted as
follows:
1. Initial boiling point
3. Percentage of recovery
AIM
To determine the API gravity of crude petroleum and liquid petroleum products by
hydrometer method and specific gravity bottle method.
THEORY
This method covers the laboratory determination, using a glass hydrometer, of the
density, relative density, or API gravity of crude petroleum, petroleum products, or mixtures
of petroleum and non-petroleum products normally handled as liquids and having a Reid
vapour pressure of 1.8 bar (179 KPa) or less. The values are measured on a hydrometer at
convenient temperatures, readings of density being reduced to 15 oC, and that of specific
gravity and API gravity to 15.6 oC, by means of international standard tables.
CLASSIFICATIONS OR GRADES
Crude oil is classified as light, medium or heavy, according to its measured API gravity.
Light crude oil is defined as having API gravity higher than 31.1 API.
Medium oil is defined as having API gravity between 22.3 API and 31.1 API.
Heavy oil is defined as having API gravity below 22.3 API.
SIGNIFICANCE
Accurate determination of density, relative density, or API gravity of petroleum and
its products is necessary for the conversion of measured volumes to volumes at standard
temperature of 15C.
FORMULA
API Gravity
A special function of specific gravity at 15.6/15.6 oC is represented by:
API gravity, degrees
APPARATUS REQUIRED
Hydrometer
Hydrometer cylinders
Specific gravity bottle
OBSERVATIONS
SPECIFIC GRAVITY
Sl.No
SAMPLES
PROCEDURE
Hydrometer method
The samples were transferred to hydrometer cylinders without any splashing to avoid
air bubbles.
The cylinders containing samples were placed in vertical position in a location free
from air currents.
The hydrometer was gently lowered into the sample in cylinders such that the
hydrometer should not touch the walls of the cylinder.
The hydrometer was allowed to float and when it comes to rest, the specific gravity
indicated by the hydrometer for different samples at room temperature were noted.
From the specific gravity values the API gravity for the given samples were
calculated.
Specific gravity bottle method
RESULT
The API gravity of the given samples using hydrometer and specific gravity bottles
were calculated and tabulated as follows
API gravity
Sl.No.
Samples
Hydrometer method
4. SOFTENING POINT
AIM
To determine the softening point of the given sample bitumen using ball and ring
apparatus.
APPARATUS REQUIRED
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 temperature at which the substance attains a particular degree of softness under
specified condition of test is called softening point.
Bitumen is specified by softening point. Bitumen being amorphous does not melt
sharply but gradually becomes softer and less viscous as the temperature rises.
For this reason, the determination of the softening point must be made by fixed
arbitrary and closely defined method.
The softening point of bitumen is rounded out by the ball and ring test.
APPLICATION
Used in annealing of bitumen.
Processing of plastics.
Determining the quality of bitumen.
PROCEDURE
A beaker is taken and filled with of it with water.
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.
RESULT
The softening point of given first sample
=
The softening point of given second sample =
5. ANILINE POINT
AIM
To determine the aniline point of the given sample.
APPARATUS
The tube approximately 25mm in diameter and 150mm in length made of heatresistant glass.
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
Diesel index
Diesel index is an indication of the ignition quality of a diesel fuel. This is determined
by calculation from the specific gravity and the aniline point of the sample. Although it is of
the same order as the cetane number, it may differ widely from the cetane number. Higher the
diesel index better is the ignition quality of the diesel fuel. It is normally used as a guide to
ignition quality of the diesel fuel in the absence of test engine for the direct measurement of
cetane number.
The diesel index is calculated as follows:
(a) Diesel index = (Aniline point,F API)/100
(b) Diesel index = (Aniline gravity constant)/100
(c) Diesel index = (Cetane number 10)/0.72
Cetane number
Cetane number is related to the ignition delay of a fuel in a diesel engine, i.e. how
rapidly combustion begins after injection of the fuel into the combustion chamber.
The shorter the ignition delay period, higher is the cetane number of the fuel
Cetane number is the index of the ignition quality of a fuel. High cetane number
fuels will facilitate easy starting of compression ignition engines, particularly in cold
weathers, and faster warm up. These also result in increased engine efficiency and power
output, reduced exhaust smoke and odour and combustion noise. In the absence of test
engine, the diesel index or the calculated cetane index will give an approximate idea of the
ignition quality of the fuel.
Cetane number= 0.72Diesel index + 10
PROCEDURE
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.
Stirring is continued and the mixture is allowed to cool at a rate of 0.5 to 1C/min.
The temperature at which the mixture suddenly became cloudy throughout is recorded
as the aniline point.
RESULT
Results for the aniline point experiment were found to be
Aniline point =
Diesel index
Cetane number =
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.
1. The test sample is first poured into a test jar to a level approximately half full.
2. A cork carrying the test thermometer is used to close the jar.
3. The thermometer bulb is positioned to rest at the bottom of the jar.
4. The entire test subject is then placed in a constant temperature cooling bath on top of
a gasket to prevent excessive cooling.
5. At every 1C, the sample is taken out and inspected for cloud then quickly replaced.
6. Successively lower temperature cooling baths may be used depending on the cloud
point.
7. 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 the thermometer. The sample is
then cooled and then inspected for pour point as per the usual pour point method
RESULT
---------0C.
---------0C
7.
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 corrosion
standards. 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
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 --------------------------8. BOMB CALORIMETER
AIM:
The heating value or calorific value of a substance, usually a fuel or food, is the amount of
heat released during the combustion of a specified amount of it. The calorific value is a
characteristic for each substance. It is measured in units of energy per unit of the substance,
usually mass, such as: kcal/kg, kJ/kg, J/mol, Btu/m. Heating value is commonly determined
by use of a bomb calorimeter.
The bomb calorimeter is the most common device for measuring the heat of combustion or
calorific value of a material. With this apparatus a test specimen of specified mass is burned
under standardized conditions. The heat of combustion determined under these conditions is
calculated on the basis of the observed temperature rise while taking account of heat loss. The
combustion process is initiated inside an atmosphere of oxygen in a constant volume
container, the bomb, which is a vessel built to withstand high pressures. It is immersed in a
stirred water bath, and the whole device is the calorimeter vessel. The calorimeter vessel is
also immersed in an outer water bath. The water temperature in the calorimeter vessel and
that of the outer bath are both monitored
THEORY:
The calorific value of a fuel is the amount of energy liberated by burning completely unit
quantity of fuel. A small amount is burned under high pressure oxygen. The calorific value
calculated by measured the energy liberated.
Heat liberated = Heat gained by water and calorimeter
mf *CV = (mw + mc) (T2-T1)*(Cp)
where
mf : mass of the fuel.
mw : mass of water in calorimeter.
mc : mass of water equivalent of the calorimeter which should be determined using a fuel of
know calorific value.
T2-T1: temperature rise.
Cp: specific heat of water.
PROCEDURE:
Figure shows the experiment setup: bomb calorimeter and Beckman thermometer.
An adiabatic bomb calorimeter has the metal bomb inside of a metal bucket containing water.
That metal bucket sits loosely inside an insulated jacket. There is a stirrer that sticks into the
water in the bucket and is driven by a motor outside of the calorimeter. A thermometer also
sticks into the water in the bucket and is the device that will be used to determine the change
in temperature during the reaction. Two electrical leads connect to the top of the bomb from
outside and they will deliver the current that initiates the reaction.
The metal bomb provides a constant-volume system in which the combustion will reaction
take place. The sample pellet is placed in the ignition cup and the fuse wire is carefully
arranged to touch the pellet but not the cup. The bomb is sealed by screwing the cap on and
then filled with a high pressure of pure oxygen. The electrical connections are made at the top
and the bomb is placed into the water bucket. Figure 2 shows a sketch of the bomb
calorimeter cross section.
Tim
e
Temperatu
re
Tim
e
Temperatu
re
[s]
[oC]
[s]
[oC]
250
10
260
20
270
30
280
40
290
Figure 2
a sketch of the bomb
calorimeter cross section
50
300
Data observed
60
310
Table 1:
70
320
80
330
90
340
100
350
110
360
Mass of water = 2 Kg
120
370
Mass of fuel = 1 g
130
380
140
390
Sample calculation:
150
400
160
410
mf
170
420
* C.V = ( mw + mc ) ( T2 T1 ) (cp )
180
430
C.V =
190
440
200
450
210
460
220
470
230
480
240
[ J / Kg ]
The calorific value of the given sample in this experiment is found to be -----------9. KFR TITRATION
AIM:
To determine the water content in the given petroleum sample.
APPARATUS REQUIRED:
Base unit consists of rear panel and front panel. Front panel has stirrer on switch.
Stirrer speed regulator 3 LED and MVP set potentiometer
Green LED O- equipment on
Yellow LED P- nearing end point indication
Red LED E. - endpoint indication
Rear panel has main ON switch. Plug socket, fuse 500 mA and electrode terminals e.
Magnetic stirrer:
Stirrer on - off switch is located on the front panel. Use regulator to set the required speed.
After setting required speed, use on off switch only for operating the stirrer. Avoid using the
regulator frequently.
SETTING UP THE EQUIPMENT FOR OPERATION:
Fix stand rod to the base unit and mount the burette assembly on the instrument.
The burette assembly will freely slide up and down and revolve around the standard
Reaction assembly.
Pressure filling auto zero setting burette assembly.
KFR bottle can be screwed on the plastic cap.
Operate bellow holding vertically and closing the T joint connection tube.
Air pressure in the KFR bottle increases and lifts KFR to fill the burette.
When the level crosses o mark remove the finger zero level sets automatically.
Reaction vessel can be filled or removed by lifting the burette assembly.
Reaction vessel is connected to the electrode terminals on rear panel through pair of
connecting jack wires.
Using methanol bottle instead of KFR bottle can wash the burette assembly.
If you want to adjust the zero level, adjust the Teflon tip I.e. just pull out or insert the
Teflon tip and set to zero.
PROCEDURE:
1. Neutralization of KFR.
2. Place magnetic stirring paddle into reactor carefully, using the forceps.
3. Never drop the Teflon magnetic paddle into the reactor after mounting on the
magnetic stirrer.
4. The paddle will be pulled down with great force and damage the reaction flask.
5. Pour about 20 ml grade methanol into the reactor.
6. Fill the burette with KFR.
7. Connect jack wire to the reactor and electrode terminals marked e.
8. Lift the burette assembly by 50 cm and place the reactor on the magnetic stirrer lower
the burette assembly and allow it to rest on the reactor.
9. Switch on the equipment power on o green LED will glow.
10. Switch on the stirrer.
11. Set required speed for vigorous stirring with minimum spurting and wait for10 to 15
seconds for uniform stirring.
12. Add KFR reagent by drops into the burette valve.
13. Add KFR reagent until pre end point p yellow LED glows, this will indicate nearing
end point.
14. Now add KFR by drops slowly giving 10-20 seconds between additions until E red
LED glows continuously for 30 seconds.
15. At the end point of the titration P yellow LED will go off and E red LED will glow
continuously at the point wait and watch for 30 seconds indicating current flow is
steady and continuous.
STANDARDIZATION OF KFR:
1. For finding out the factor of water equivalent.
2. Fill the burette
3. Weigh 1 ml of distiller water using electronic balance in a syringe.
4. Close the reaction vessel with stopper .start magnetic stirrer and allow the contents to
dissolve for some time.
5. Distilled water dissolves immediately.
6. Fill the burette and titrate up to the end point as described in neutralization.
7. After completion of cycle, note the burette reading.
F factor of equivalent = M/A
M is the weight of the water
A is the volume of KFR
ESTIMATION OF WATER CONTENT IN UNKNOWN SAMPLE:
Viscous liquids can be weighed and dropped into the reactor using droppers, light liquids
can be measured and added into the reactor using pipettes or syringe.
Percentage of water content = B *F
______
V*D* 10
B is the volume of KFR
F is the factor of water equivalent
V is the volume of the sample
D is the density of the sample.
TABULATION:
Neutralization of KFR
Burette reading (KFR volume)
Standardization of KFR
Weight of water M
Volume of KFR A
=
=
=
=
= 1 mg/ml
B*F =
----V*D*10
RESULT:
The percentage of water present in the given petroleum sample is -----------.
10. DETERMINATIONOF WATER AND SEDIMENTS BY CENTRIFUGE METHOD
AIM:
To determine the amount of the sediments present in the given sample
APPARATUS REQUIRED
Centrifuge, Centrifuge tubes (8inch), Bath, Toluene, Demulsifier solution (phenol or
Naphthenic acid)
THEORY
Centrifugal forces enhance the dissipation of colloidal particles from colloidal solution, an
equal volume of crude and water saturated xylene were placed into a cone shaped centrifuge.
After Centrifugation, the higher gravity water and sediments separates at the bottom of the
tube. The water and sediment content of the crude oil are important because they can cause
corrosion of the equipment and problems in processing. It is important to measure accurately
the net volumes of actual oil in sales taxation exchanges and custody transfers.
PROCEDURE
1. Fill two centrifuge tubes to the 50 millilitre (ml) or 100 part mark with the homogeneous
sample to be tested. Read the top of the meniscus (the curved upper surface of a liquid
column).
2. Fill the two tubes with 50 ml of solvent which brings the total contents of the tubes to the
100 ml or the200 parts mark. The acceptable solvents are Stoddard, kerosene, toluene, and
xylene. Note that toluene and xylene should be water-saturated at test temperature.
3. Invert the tubes 10 times to mix the sample and solvent. This should be done below eye
level for safety, and safety glasses are highly recommended. Solvents can be hazardous and
should be handled with caution. Material Safety Data Sheets (MSDS) and handling
precautions recommended by the chemical manufacturer should be followed.
4. Place the tubes in the preheater and heat to 140 F +/- 5 F.
5. Invert the tubes ten times again to mix.
6. Place the tubes on opposite sides of the centrifuge to balance the load. Close the centrifuge
lid.
7. Centrifuge for a minimum of 5 minutes.
8. When the centrifuge comes to a stop, test the temperature of the tube contents without
disturbing the oil water interface.
9. If the temperature of the sample is 125 F or above, read and record the combined sediment
and water content at the bottom of each tube. If the temperature is below 125 F, the tubes
must be reheated and the test repeated without further agitation until two consecutive
consistent readings are obtained.
10. If an emulsion is visible, add a solvent containing a demulsifier to the sample and retest it.
11. Compare the readings from the two tubes. If the results vary by more than one
subdivision of the centrifuge tube, the sample was not homogeneous. Thus the test should be
repeated with two fresh samples. By following the procedure closely, the results obtained will
be reliable and accurate.
CALCULATION:
1. Record the final volume of water and the sediment in each tube and take the average.
2. Express the average as a percentage by volume of water and the sediment.
Sample Size
If the centrifuge tube is filled with any proportion other than 50/50 sample/solvent, the results
cannot be read directly from the centrifuge tube. The following equation must be utilized to
adjust for the incorrect mixture.
Sediment and Water % = (S/V) * 100
Where:
S = Volume of sediment & water found, ml
V = Volume of oil tested, ml
RESULT:
The amount of sediments present in the given sample is found to be ............. %
11. DETERMINATION OF FLASH POINT AND FIRE POINT BY OPEN CUP
APPARATUS
AIM:
To determine the flash point and fire point of the given lubricant or liquid petroleum
products.
APPARATUS REQUIRED:
Open cup apparatus, LPG supply, testing sample, thermometer etc.
THEORY:
Flash point is the lowest temperature at which sufficient amount of vapor are given
off by an oil, so us to give a flash. When the vapor come into contact with test flame.
Fire point is the lowest temperature at which the vapor of oil burn continuously for at
least 5 seconds. When a small flame is brought near it. Generally the fire point is 5-40
C higher than the flash point. Though these points are not released to the lubricating
properties of oil, knowledge of these is helpful to provide safety measures against the
fire hazards during and storage.
This test method is applicable to all petroleum products with flash points above 79C (175F)
and below 400C (752F) except fuel oils
PROCEDURE:
1. The cup is cleared using a solvent to remove oil and dried well.
2. The cup is filled with the test oil up to the indicator level.
3. The thermometer is immersed into the cup and the test flame in it. The heating device
is switched on and the temperature of the sample is carefully is greased by 2-3 degree
c per minute.
4. The sample in the cup is well stirred constantly to keep the temperature uniform
throughout.
5. A test flame is introduced into the cup at every 1 degree c rise in temperature.
6. The temperature at distinct flash is seen in the interior of the cup is noted as the flash
point.
7. The heating of the sample and the periodical introduction of the test flame are
continued.
8. When the oil vapor catches flame and continues to burn at least 5 seconds; the
temperature of the oil is noted and it is taken as fire point.
TABULATION:
S.No
RESULT:
The flash point of the given petroleum product is _______
The fire point of the given petroleum product is _______
12. DEAN AND STARK APPARATUS
AIM:
To determine the water in the given crude sample.
APP ARATUS:
A glass distillation flask, condenser, graduated glass tube and heater.
CHEMICALS REQUIRED:
Volume % is
Weight % is
RESULT:
13. MEASUREMENT OF KINEMATIC VISCOSITY USING U-TUBE VISCOMETER
AIM:
To determine the kinematic viscosity and dynamic viscosity by using u-tube
viscometer.
APPARATUS:
U-tube viscometer
Viscometer thermostat and bath
A rubber bung
A stop watch
THEORY:
Kinematic viscosity (V): is a measure of the resistance to gravity flow of a fluid, the pressure
head being proportional to its density.
The unit used is the stoke which equals cm2/sec, the common unit used the centistoke = 10-2
stokes.
PROCEDURE:
1. Place the viscometer vertically into the bath liquid such that the filling mark A is 3 cm
below the surface of the water.
2. Allow the viscometer to reach the bath temperature and then pour sufficient amount of
the filtered crude into the filling tube to a point just below the filling mark A avoiding
wetting the glass above A.
3. Allow the crude to flow through the capillary taking care that the liquid column
remains unbroken until it reaches a position about 5 mm below the filling mark B and
stop its flow by closing the timing tube with the rubber bung.
4. Add more crude to the filling tube to bring the crude level to just below mark A.
5. Wait for 30 minutes to allow the sample to reach the bath temperature and any air
bubbles to rise to the surface.
6. Open the timing tube slightly to allow the crude level to rise to mark B and close it
again add more crude to the filling tube to bring its level to mark A, wait for 5
minutes.
7. Open the timing tube and allow the liquid to flow under its own head and measure the
time in seconds for the upper most level of the crude to rise from mark C to mark D.
2- Calculate the viscosity from the calculated kinematic viscosity V and the density P by
means of the following equation
= pV
where,
3- Report test results for both the kinematic and dynamic viscosity rounded to the nearest one
part per thousand of the value measured or calculated, respectively.
RESULT:
The dynamic viscosity and kinematic viscosity of the given sample is found to be --------