Experiment No. 5 2
Experiment No. 5 2
5
TEST OF OXYGEN BOMB CALORIMETER: OBTAINING THE CALORIFIC VALUE OF FUEL
Course Code: MEF420L2
Course Title: ME Laboratory 2
Section: ME42FA1
Members: 1. Zafra, Charles Jourdan M. (Leader)
2. Arcay, Andrew
3. Caringal, John Martin U. (Safety Officer)
4. Dela cruz, John Kelvin B.
5. Gaela, Vanjochris
6. Macapagal,Roel U. (Quality Control)
1. Objective(s):
Program: BSME
Date Performed: February 11, 2015
Date Submitted: March 1, 2015
Instructor: Engr. Nelson DelaPea Jr.
The activity aims to demonstrate how to determine the calorific value of different types of fuel.
2. Intended Learning Outcomes (ILOs):
The students shall be able to:
2.1 Perform the procedure of operating an oxygen bomb calorimeter.
2.2 Determine the calorific value of different types of fuel.
2.3 Develop professional work ethics, including precision, neatness, safety and ability to follow
instruction.
3. Discussion:
Calorimetry is a fundamental test of great significance to anyone concerned with the production or
utilization of solid or liquid fuels.
One of the most important tests in the evaluation of materials, which are burned, as fuels, is the
determination of the heat of combustion, or calorific value. These measurements can be made in the Bomb
Calorimeter Set for Testing Calorific Value of Fuels, TBCF.
The Bomb Calorimeter is a classic device used to determine the heating or calorific value of solid and liquid
fuel samples at constant volume. Basically, this device burns a fuel sample and transfers the heat into a
known mass of water. From the weight of the fuel sample and temperature rise of the water, the calorific
value can be calculated. The calorific value obtained in a bomb calorimeter test represents the gross heat
of combustion per unit mass of fuel sample. This is the heat produced when the sample burns, plus the
heat given up when the newly formed water vapor condenses and cools to the temperature of the bomb.
Determining calorific values is profoundly important; fuels are one of the biggest commodities in the world,
and their calorific value.
The Bomb Calorimeter study is carried out to gain a better understanding of the working principles behind
the bomb calorimeter and also to find out the gross calorific values of different types of liquid fuel.
Description:
The unit comprises the calorimeter, a calorimeter vessel, an outer double walled water jacket, control unit to
switch on/off the stirrer and the ignition device, a Beckman type thermometer, and charging unit with
pressure gauges to facilitate the charging of the calorimeter with oxygen. The particular features of the
calorimeter bomb are the method of sealing and the method of ensuring ignition. The calorimeter vessel
and outer jacket wall are manufactured in stainless steel. The calorimeter bomb is a container made of
stainless steel that can support high pressures. It is sealed by a screw top. The bomb is charged with gas
(oxygen) through the filling valve. This bomb is introduced inside a calorimeter vessel made of stainless
steel that is filled with water, and at the same time it is introduced inside a double walled water jacket.
The rod of the calorimeter supports a metallic crucible. The calorimeter bomb, which contains the fuel
sample to be burned, is hermetic to the gas by closing the filling valve and its cover. Combustion is started
through a thin wire that is red hot-heated up momentarily due to the passing of an electrical current that
flows through an isolated terminal and the rod, which is electrically connected to the cover.
The water in the calorimeter vessel is agitated automatically with a stirrer driven by a small motor. The top
of the double walled jacket is closed with a cover that has some orifices. A Beckman thermometer to
measure the temperature of the calorimeter vessel passes through one of these orifices. Other orifices are
used to fasten the jacket to the cover. Also, one of these holes is used to insert the wire that supplies the
electric current to the rod. The unit includes a control unit that switches on/off the stirrer and the ignition
device through the heating up of the thin wire, and a load unit with pressure gauges to make the filling with
oxygen of the calorimeter easier.
Specifications:
Calorimeter for testing calorific value of fuels, including:
1. Main metallic elements in stainless steel.
2. Diagram with a distribution of the elements similar than the one in the real unit.
3. Calorimeter bomb.
4. Calorimeter vessel. Characteristics:
o Stainless steel
Maximum volume: 4 litters.
5. Double walled outer jacket in stainless steel, with water inlet and outlet.
6. Electric stirrer with one rod and two blades. Characteristics: 330rpm.
7. Control unit to switch on/off the stirrer and the ignition device
8. Beckman thermometer. Range: 6C.
9. Charging unit with pressure gauges.
10. One nickel crucible.
11. Reel of Nickel-Chrome wire.
Theoretical Consideration:
Almost all chemical reactions adsorb or release energy, generally as heat. Heat is the thermal energy
transfer between two bodies whose temperatures are different. Heat flow from a hot body to a cold one is
frequently mentioned. Generally, absorbed heat or released heat is used to describe the energy
changes that take place during a process.
Reactions that take place during a process can be endothermic, if they absorb heat, or exothermic, if they
release heat. Endothermic changes are expressed with a positive sign, and exothermic changes with a
negative sign, according to the first law of thermodynamics. The enthalpy change occurred in the direct
reaction is exactly opposed in the inverse reaction. This thermal effect is the same regardless whether the
reaction takes place in one or several stages. The magnitude of the change depends on the composition,
the physical state of the reagents and products and the stoichiometric expression.
Thermal changes can happen at constant pressure or at constant volume and are expressed with the
following equations:
H = qp = 0
E = qv = 0
Where: H represents the enthalpy change and E represents the energy change. The H can be
experimentally determined by measuring the heat flow that accompanies a constant pressure reaction, and
the E a constant volume.
Heat changes of physical or chemical processes are measured with a calorimeter, which is a closed vessel
specifically designed for that purpose. The calorimetry study, that is to say, the measurement of heat
changes, depends on the understanding of specific heat and heat capacity. The specific heat (c p) of a
substance is the amount of heat required to increase one Celsius degree the temperature of one gram of
the substance. The heat capacity (Q) of a substance is the amount of heat required to increase one Celsius
Degree the temperature of a certain amount of substance. The relationship between the heat capacity and
the specific heat of a substance is:
Q = mcp
Where m is the mass of the substance in grams and c p is the specific heat of a substance
reliable to perform the bomb calorimeter test, as it is a direct measure of the heat of combustion.
Bomb calorimeters for rapid combustion are composed of a combustion chamber (bomb) and a calorimeter
vessel, usually a cylinder surrounding the bomb and containing a known quantity of water. The elevation in
temperature of that water will be measured. The combustion is made in oxygen, pure or diluted.
Combustion chambers are either under a constant pressure or with a constant volume. The results
obtained with a calorimeter of constant volume are not exactly the same as those obtained with constant
pressure, but for solid or liquid substances the difference is too small to consider.
thermometer. The agitator is used to maintain a uniform temperature in the water and aids the heat transfer
from the bomb. The thermometer measures the water temperature (its range is from 24C to 30C with
0.01C accuracy). There is an air gap between the water vessel and the water jacket, which is an excellent
heat insulator. When the calorimeter is running, the temperature of the calorimeter body is automatically
maintained at the same temperature than that of the water container that holds the bomb. This provides an
adiabatic condition and, thus, no heat is transferred to or from the container of water, except from the heat
released in the bomb.
5. Procedure:
1. Prepare the fuel sample by placing it in a crucible and weighing it on a balance. Ensure that the
weight of the fuel does not exceed 1.1 g. Note down the weight of the fuel sample (mf) and
place the crucible containing the fuel gently in the loop holder. When starting tests with new or
unfamiliar materials, it is always best to use samples of less than 0.7 of a gram, with the
possibility of increasing the amount if a preliminary test indicates no abnormal behavior.
2. The bomb head has been pre-attached with a 10 cm long fuse wire between the two electrodes.
Bend the fuse wire down just above the liquid fuel sample. The wire must not make contact with
the fuel crucible. To attach the fuse to quick-grip electrodes, insert the ends of the wire into the
eyelet at the end of each stem and push the cap downward to pinch the wire into place. No
further threading or twisting is required.
3. It is not necessary to submerge the wire in a powdered sample. In fact, better combustions will
usually be obtained if the loop of the fuse is set slightly above the surface. When using pelleted
samples, bend the wire so that the loop bears against the top of the pellet firmly enough to keep
it from sliding against the side of the capsule.
4. Care must be taken no to disturb the sample when moving the bomb head from to the
calorimeter bomb. Check the sealing ring to be sure that it is in good condition and moisten it
with a bit of water so that it will slide freely into the body of the calorimeter bomb, then slide the
head into the bomb and push it down as far as it will go. Set the screw cap on the bomb and
turn it down firmly by hand to a solid stop. When properly closed, no threads on the bomb
should be exposed.
5. Oxygen for the bomb can be drawn from a standard commercial oxygen cylinder. Connect the
regulator to the cylinder, keeping the 0-55 atm. in an upright position.
6. The pressure connection to the bomb is made with a slip connector on the oxygen hose which
slides over the gas inlet fitting on the bomb head. Slide the connector onto the inlet valve body
and push it down as far as it will go.
Close the outlet valve on the bomb head; then open or crack the oxygen tank valve not more
than one-quarter turn. Open the filling connection control valve slowly and watch the gage as
the bomb pressure rises to the desired filling pressure (30 atm.); then close the control valve.
The bomb inlet check valve will close automatically when the oxygen supply is shut off, leaving
the bomb filled to the highest pressure indicated on the 0 - 55 atm. Release the residual
pressure in the filling hose by pushing downward on the lever attached to the relief valve. The
gage should now return to zero.
7. Fill the calorimeter vessel by first taring the empty vessel; then add 3700 grams of water. Note
the exact mass of the water.
8. Introduce the bomb calorimeter inside the calorimeter vessel. Handle the bomb carefully during
this operation so that the sample will not be disturbed.
9. Check the bomb for leaks before firing. If any gas leakage is indicated, no matter how slight, DO
NOT FIRE THE BOMB. Instead remove it from the water bath; release the pressure and
eliminate the leak before proceeding with combustion test.
10. Fill the jacket with water.
11. Put the cover on the jacket. Turn the stirrer by hand to be sure that it runs freely and start the
motor. Install the Beckman thermometer; this thermometer should be immersed in water and
not close to the bomb.
12. Let the stirrer run for at least 5 minutes to reach equilibrium before starting a measured run.
13. The scanning of the temperature data is pre-set to be done once a minute. At the start of the
5th minute, fire the charge by pressing the firing button on the control unit, keeping the circuit
closed for about 5 seconds.
14. The vessel temperature will start to rise within 20-30 seconds after firing. This rise will be rapid
during the first few minutes; then it will become slower as the temperature approaches a
stable maximum as shown by the typical rise curve shown in Figure. Accurate time and
temperature observations must be recorded to identify certain points needed to calculate the
calorific value of the sample.
15. Usually the temperature will reach a maximum; then it will drop very slowly. But this is not
always true since a low starting temperature may result in a slow continuous rise without
reaching a maximum. As stated above, the difference between successive readings must be
noted and the readings continued until the rate of the temperature change becomes constant
over a period of 5 minutes.
16. After the last temperature reading, stop the stirrer. Let the bomb stand in the calorimeter
vessel for at least 3 minutes. Then, remove the jacket cover and extract the bomb
calorimeter. Wipe the bomb with a clean towel.
17. Open the valve knob on the bomb head slightly to release all residual gas pressure before
attempting to remove the screw cap. This release should proceed slowly over a period of not
less than one minute to avoid entrainment losses. After all pressure has been released,
unscrew the cap; lift the head out of the cylinder. Do not twist the head during removal. Pull it
straight out to avoid sticking. Examine the interior of the bomb for soot or other evidence of
incomplete combustion. If such evidence is found, the test will have to be discarded.
18. Remove all unburned pieces of fuse wire from the bomb electrodes.
19. On completion of experiment, wash all inner surfaces of the bomb and the combustion
crucible with a jet of distilled water and collect the washings. Keep the bomb set dry and
clean with some wiping tissue.
6. Data and Results:
Method of Obtaining the Calorific Value from the Obtained Data:
To illustrate the method of working out the calorific value, the following example of a test is given:
Weight of fuel oil = Weight of crucible and fuel sample - Weight of crucible
Total equivalent weight of water = Weight of water in calorimeter + Water value of unit
Thermometer Readings
(C)
25.3
25.3
25.4
25.5
25.6
25.6
Rise Period:
Time
(minutes)
5.30
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
Thermometer Readings
(C)
25.9
26
26.1
26.2
26.3
26.4
26.5
26.6
26.6
26.6
26.6
26.6
26.6
26.6
26.6
26.6
26.6
26.6
26.6
26.6
26.6
26.6
26.6
26.6
26.6
26.6
26.7
26.7
26.7
26.7
26.6
Radiation Correction:
The radiation correction is calculated from the knowledge of the rates of change of temperature of the
water before igniting the fuel sample and after the attainment of the maximum temperature.
Let:
n= number of minutes between the ignition and the attainment of the maximum temperature
tf= rate of temperature fall in degrees per minute at the end of the exercise
tr= rate of temperature rise in degrees per minute at the beginning of the exercise.
This is an approximation to the Renault-Stohman-Pfaundler formula, and is sufficiently accurate for all
purposes other than research.
Product
H2O(g) = 44.0 KJ
3H2O(L)
LHV = 132.0 KJ
Mass of Water:
Q = mw Cpw (T2 T1)
HVacidmacid = mw Cpw (T2 T1)
mw =
HV acid macid
Cp w (T 2 +T 1)
mw =
J
(26 430 x 0.7 g)
g
J
(4.187
x1C )
gC
mw = 4 418.677 g or 4.4187 kg
Higher Heating Value:
HHV = LHV + LH mw
HHV = 132.0 KJ + (2257
KJ
kg )(4.4187 kg)
HHV = 10 104.95 KJ
C7H6O2
0.7 gram
J
g
26 430
4.4187 kg
4.186
J
gC
Temperature Change
1 C
LHV
132.0 KJ
HHV
10 104.95 KJ
26.5
26
Temperature, Celcius
25.5
25
24.5
0
10
15
20
25
30
35
Time, minute
In this given graph, the result successfully show that the fuel (Benzoic Acid) was
burned correctly. Though it only rises 1 C due to the mass of the fuel because the fuel
40
contain in the crucible was less than one gram. The graph of the fuel presents the before
and after burning the fuel. The first five minutes shows the graph of the initial temperature
of the water. The next minutes show the rising temperature of the water; this is the time
when the fuel is burning. And the higher temperature shows the after burned of the fuel.
2.3.1
discuss them what they task. I listen to my instructor so we can perform our experiment
right, and to avoid accident. Before we start the experiment I read the procedures the
things we must do.
2.3.2
2.3.3
3. Based on Observation:
During we perform the activity we can say that the temperature difference after and
before we turning on the machine is very little almost no difference so we say that the
amount of the fuel being burn is too small and the amount of water inside the bomb
calorimeter is too big thats why the heat transfer of the fuel is very small, we suggest that
the amount of the fuel put inside the bomb calorimeter must increase so that the
temperature will also increase and the data being gathered is more precise and accurate.
Group Pictures:
a.
b.
Result of the experiment:
Fig.a. The crucible.
Fig.b. The inside vessel.
9. Assessment Rubric:
T I P - V PAA 0 5 4 D
Revision Status/Date:0/2009 September 09
CRITERIA
Laboratory Skills
Manipulative Members do not
Skills
demonstrate needed
skills.
Experimental Members are unable to
Set-up
set-up the materials.
Process
Skills
Members do not
demonstrate targeted
process skills.
Members occasionally
demonstrate needed
skills.
Members are able to
set-up the materials
with supervision.
Members occasionally
demonstrate targeted
process skills.
Members always
demonstrate needed
skills.
Members are able to
set-up the material with
minimum supervision.
Members always
demonstrate targeted
process skills.
Safety
Precautions
SCORE
time.
Work Habits
Time
Management/
Conduct of
Experiment
Cooperative
and
Teamwork
times.
TOTAL SCORE
RATING=
x 100%