1.

FLASH POINT AND FIRE POINT

BY PENSKY MARTENS APPARATUS
AIM

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

DEFINITION

FLASH POI NT
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.

FI RE POI NT
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

Pensky Martens Closed Tester
Thermometers (Two standard thermometers shall be used with the Pensky-Martens
tester)
TABULATION


S.No.

SAMPLES

FLASH POINT (C)

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

The oil cup was cleaned using solvent.
The cup was filled with fresh sample up to the mark.
The cup was placed in the apparatus bath.
The lid is placed on the cup and the thermometer was also inserted.
The electrical heater was turned to 50% of input volts and oil is heated.
After that spring handle was rotated at every degree rise from this point.
The temperature was noted at which the flash occurs.
The fire point was noted at which the fuel burnt continuously for 5 seconds.
The experiment was repeated for different samples.
















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

Volume of Distillate collected (ml)

Temperature C


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,

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 in the 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.
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.












RESULT
The Distillation characteristics are studied for the given samples and the values are noted as
follows:
1. Initial boiling point = C
2. Middle boiling point = C
3. Percentage of recovery =
4. Percentage of non-volatile residue =
5. Film boiling point = C










API GRAVITY - DIAGRAM






3. DETERMINATION OF API GRAVITY OF CRUDE PETROLEUM AND
LIQUID PETROLEUM PRODUCTS BY HYDROMETER METHOD AND
SPECIFIC GRAVITY BOTTLE METHOD

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
o
C, and that of specific
gravity and API gravity to 15.6
o
C, 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
o
C is represented by:
API gravity, degrees = [141.5 /Specific gravity at 15.6/15.6
o
C] - 131.5
APPARATUS REQUIRED
Hydrometer
Hydrometer cylinders
Specific gravity bottle

OBSERVATIONS

Sl.No

SAMPLES
SPECIFIC GRAVITY
At room temperature
using Hydrometer
At room temperature
using Specific gravity
bottle method






SPECIFIC GRAVITY BOTTLE METHOD
Weight of the empty specific gravity bottle =
Weight of the specific gravity bottle with sample 1 =
Weight of the specific gravity bottle with sample 2 =
Weight of the specific gravity bottle with sample 3 =
Weight of the specific gravity bottle with sample 4 =








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
The samples were taken in each specific gravity bottle.
The specific gravity bottle with the samples and the weight of the empty specific
gravity bottle were measured.
The readings were tabulated and the specific gravity for different samples was
calculated. From the specific gravity values the API gravity for the given samples
were calculated.

RESULT
The API gravity of the given samples using hydrometer and specific gravity bottles
were calculated and tabulated as follows

Sl.No.

Samples
API gravity
Hydrometer method Specific gravity bottle
method






4. SOFTENING POINT

AIM

To determine the softening point of the given sample bitumen 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 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 heat-
resistant glass.
A Jacket-approximately 37 to 42mm in diameter and 175mm in length made of heat-
resistant glass.
A Stirrer-manually operated, approximately 2mm in diameter soft iron wire.
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
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 1-3C/min till
complete miscibility was obtained.
Stirring is continued and the mixture is allowed to cool at a rate of 0.5 to 1C/min.
Cooling is continued to a temperature of 1 to 2C below the first appearance of
turbidity.
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 =










6. CLOUD AND POUR POINT DETERMINATION
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 3C
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.



SAMPLES SHOWING CLOUD AND POUR POINT


CLOUD AND POUR POINT EXPERIMENTAL SETUP
CLOUD AND POUR POINT EXPERIMENTAL SETUP


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 1C, 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 100
o
C 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
The pour point of the given sample was found to be ---------
0
C.
The cloud point of the given sample was found to be ---------
0
C


7. 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 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
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 quality
control tool, and for use in development or research work on industrial aromatic
hydrocarbons 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 50
o
C constant temperature.
The bath is set at the desired working temperature and waits for 20 minutes of
time after the start.
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 ---------------------------
8. BOMB CALORIMETER
AIM:
To determine the calorific value of a given fuel
INTRODUCTION:
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
m
f
*CV = (m
w
+ m
c
) (T
2
-T
1
)*(Cp)
where
m
f
: mass of the fuel.
m
w
: mass of water in calorimeter.
m
c
: mass of water equivalent of the calorimeter which should be determined using a fuel of
know calorific value.
T
2
-T
1
: temperature rise.
Cp: specific heat of water.
PROCEDURE:
1. A small quantity of fuel (about 1 gram) is weighted.
2. The ignition wire is fixed and the bomb is closed.
3. The bomb is charged with oxygen to a pressure of about 30 bars.
4. The bomb is inserted in the calorimeter and about 2 Kg of water is poured.
5. The Beckman thermometer is inserted and the stirrer is started.
6. Temperature of water is recorded every 10 seconds.
EXPERIMENTAL SETUP:

Figure shows the experiment setup: bomb calorimeter and Beckman thermometer.
The Beckmann thermometer was invented by Ernest Otto Beckmann (1853-1923), also noted
for the Beckmann transformation in organic chemistry, as a result of his work with oximes.
His interest in the physical properties of these molecules lead him to invent a number of
ingenious apparatus for measuring colligate properties based on the theoretical work of
Francois Marie Raoult (1830-1901). He began publishing this work around 1888. Beckmann
developed the differential thermometer bearing his name, which could accurately measure
temperatures to about 0.001 C, in order to measure the very small temperature changes
found in boiling point and freezing point determinations of molecular weight.
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.

Figure 2 a sketch of the bomb calorimeter cross section
Data observed
Table 1:
Change of temperature with time
Time
[ s ]
Temperature
[
o
C ]
Time
[ s ]
Temperature
[
o
C ]
0 28.4 250 32.5
10 28.5 260 32.5
20 28.7 270 32.5
30 29.1 280 32.5
40 29.6 290 32.6
50 29.9 300 32.6
60 30.7 310 32.6
70 31.0 320 32.6
80 31.4 330 32.6


Pressure in =30 bar
Mass of water = 2 Kg
Mass of fuel = 1 g
Sample calculation:
Heat liberated from fuel = Heat gained by water and calorimeter
m
f
* C.V = ( m
w
+ m
c
) ( T
2
T
1
) (c
p
)
1 * 10
-3
* C.V = (2 + 0.856) (32.5 28.4) (4186)
C.V = 49016385.6 [ J / Kg ]


90 31.5 340 32.6
100 31.6 350 32.6
110 31.8 360 32.6
120 31.9 370 32.6
130 32.0 380 32.6
140 32.1 390 32.6
150 32.2 400 32.5
160 32.2 410 32.5
170 32.3 420 32.5
180 32.3 430 32.5
190 32.4 440 32.5
200 32.4 450 32.5
210 32.4 460 32.5
220 32.4 470 32.5
230 32.5 480 32.5
240 32.5
Results and discussion
The change of temperature with the time can be shown in figure 2.

Figure 3. Water Temperatures versus Time
Figure 2 shows that the temperature of water increased very fast in the first 80 seconds, this
may happen according to the sudden change in temperature between the bomb and
calorimeter. Eighteen second represents an infection point so the increase in water
temperature becomes slowly and it goes to finish the transient change in water temperature
until it becomes constant at 200 seconds.
The heat transferred to water is stored in the water and calorimeter and increase the
temperature so in the sample calculation the value of calorific value of the diesel is found as
49016.4 [KJ/Kg].

Conclusions
The calorific value of the diesel in this experiment is 49016.4 [KJ/Kg] which effected by
many sources of errors. This value can be compared with others values for fuels to select
best option.
The experiment show that water (in liquid phase) stored energy by increasing its
temperature.







28
28.5
29
29.5
30
30.5
31
31.5
32
32.5
33
0 100 200 300 400 500
Time [ s ]
T
e
m
p
e
r
a
t
u
r
e


[

C

]
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 LEDP- 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:
Neutralization of KFR:
Place magnetic stirring paddle into reactor carefully ,using the forceps. Never drop the Teflon
magnetic paddle into the reactor after mounting on the magnetic stirrer.
The paddle will be pulled down with great force and damage the reaction flask
Pour about 20 ml grade methanol into the reactor.
Fill the burette with KFR.
Connect jack wire to the reactor and electrode terminals marked e.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.
Switch on the equipment power on o green LED will glow.
Switch on the stirrer.
Set required speed for vigorous stirring with minimum spurting. Wait for10 to 15 seconds for
uniform stirring.
Add KFR reagent by drops into the burette valve.
Add KFR reagent until pre end point p yellow LED glows, this will indicate nearing end
point. Now add KFR by drops slowly giving 10-20 seconds between additions until E red
LED glows continuously for 30 seconds. 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
For finding out the factor of water equivalent
Fill the burette
Weigh 1 ml of distiller water using electronic balance in a syringe.
Close the reaction vessel with stopper .start magnetic stirrer and allow the contents to
dissolve for some time. Distilled water dissolves immediately.
Fill the burette and titrate up to the end point as described in neutralization.
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.

Result
The percentage of water present in the given petroleum sample is -----------.







TABULATION:
Neutralization of KFR
Burette reading ( KFR volume) =
Standardization of KFR
Weight of water M =
Volume of KFR A =
Factor of water equivalent F= M
------
A
Estimation of water content in the unknown sample
Volume of KFR =
Volume of sample =
Density = 1 mg/ml
Percentage of water content = B*F
-----
V*D*10