DE LA SALLE UNIVERSITY

Gokongwei College of Engineering

Chemical Engineering Department

Engineering Thermodynamics Laboratory

Final Laboratory Report

Experiment # 9
Bomb Calorimetry, Orsat Analysis and Properties of Solid Fuels

Group Name N3P Section EA1

NAME SIGNATURE Criteria Score

1. Cellona, Kimberley B. Content (50%)
2. Dar, Lloyd Ross M. Presentation (25%)

3. Javier, Mona Lyndsay C. Relevance (25%)

4. Lopez, Maristela Ann F. Total (100%)

5. Soriano, Elijah Jeremie D. Percentage Equivalent

24 July 2018 31 July 2018

Date of performance Date of Submission

Dr. Lawrence P. Belo

Instructor
Engineering Thermodynamics Laboratory

Bomb Calorimetry, Orsat Analysis and

Properties of Solid Fuels
Kimberley B. Cellona, Lloyd Ross M. Dar, Mona Lyndsay C. Javier,
Maristela Ann F. Lopez, Elijah Jeremie D. Soriano
Department of Chemical Engineering, Gokongwei College of Engineering, De La Salle University,
2401 Taft Avenue, Manila 1004, Philippines

ARTICLE INFO ABSTRACT

AY 2017–2018 | Term 3
LBYCHED EA1
Final Laboratory Report
Experiment # 9
Date Performed: July 24, 2018
Date Submitted: July 31, 2018
Keywords
Bomb calorimetry, orsat analysis,
calorific value
Fuels come in various forms, gaseous, liquid, and solid fuels, and requires extensive
knowledge to correctly identify what the proper type of fuel is to be used that
provides that most economical and efficient performance Coal is one of the
commonly used valuable sources of energy for steam or electric generation and its
quality is determined by its carbon content. High levels of carbon produce more heat
when the coal is heated. The objectives of this two-part experiment are to determine
the solid fuels’ proximate analysis and heating value and to identify the heat capacity
of a bomb calorimeter as well as to successfully operate the bomb calorimeter under
a constant volume reaction in order to determine the heat of combustion of an
unknown solid fuel. The fuel was observed to have a high heating value for the
reason that it contained mostly volatile matter, which is found to be 38.18%.
Meanwhile, in the second part, the heat capacity of the bomb calorimeter was
calculated to be 18, 515.94 J/℃ against the theoretical value of 20,920 J/℃ .

I. INTRODUCTION unknown solid fuel.

Fuels are essential in many different processes, both
in the everyday functions of humans, and in specific
usages, such as in industries and manufacturing plants.
Fuels come in various forms, gaseous, liquid, and solid
fuels, and requires extensive knowledge to correctly
identify what the proper type of fuel is to be used that
provides the most economical and efficient performance.
Solid fuels are commonly used for cooking and in power
generation but is also used as rocket engine fuels and in
internal combustion engines. However, these uses of
solid fuels do not specifically correlate to a better
performance, since at times the engine parts get damaged
when the abrasive action of the fuel’s particles gets into
contact with those parts [1].
In this two-part experiment, the students are tasked to
determine the solid fuels’ proximate analysis and heating
value. Similarly, the students are required to identify the
heat capacity of a bomb calorimeter, under a constant
volume reaction, and successfully operate the bomb
calorimeter to determine the heat of combustion of an
[1]
1.1 Analysis and Heating Value of Solid Fuels
There are different types of solid fuels, some of
which are wood and wastes, particularly agricultural
wastes. The most commonly used solid fuel is coal,
mainly consisting of compact plant debris, formed
through biochemical action of both pressure and heat,
which accumulated over a long span of time. Coal are
further classified into ranks, which depends on the
amount of change it has undergone, type of carbon it
contains, and amount of heat it produces. Based on this,
peat, having the lowest heating value is ranked at the
bottom, while anthracite, having the highest heating
value, is ranked at the top [1,2].
The analysis of coal can be done in two ways, the
proximate analysis and ultimate analysis. The proximate
analysis is based on the volatilization characteristics of
coal and is much simpler to accomplish. In this analysis,
moisture content, volatile combustible matter or the
released gases upon heating, ash or impurities, and fixed
carbon are determined. On the other hand, the ultimate ∆ H =∆ U + ∆ ( PV )=∆ U +(∆ n) RT (1)
analysis is a more precise identification of the six basic where P is the pressure, V being the volume of the
components of coal, particularly carbon, hydrogen, system, ∆n is the change in moles in the reaction, R is the
sulfur, nitrogen, ash, and oxygen [1,2]. gas constant and T is the temperature [4].
Other properties are also essential for coal. Caking On the other hand, to calculate for Qv, the following
properties, which is uniquely found in bituminous coals. expression is used:
Coals that don’t cake produce non to weakly coherent Qv =(C ¿¿ v )(∆ T )¿ (2)
characteristics, while successful cokes should be strong where Cv is the heat capacity of the calorimeter and
while not being powdery. The coal’s grindability is also ∆T is the temperature rise of the water.
essential, since reducing its particle size would require
sufficient work and time, hindering the combustion
Before calculation of Qv, Cv must first be determined.
process to immediately occur [1].
This is done by using a substance of known heat of
combustion; then, solving the corresponding heat
1.2 Bomb Calorimetry and Heat of Combustion capacity of the calorimeter, by using both Equations 1
and 2. To validate the calculated Cv, benzoic acid and a
Calorimetry is used to measure the quantities of heat fuse wire, whose weights are both known, are introduced
evolved or absorbed in a particular physical or chemical in the calorimeter. The obtained heats of combustion are
process or reaction. Calorimeters may either operate at then compared with theoretical values given below [1]:
constant pressure, in which the measured heat is
J J
equivalent to the change in enthalpy, or at constant ∆ Hc of benzoic acid=−26425
∆ Hc of fuse wire=−5858
g g
volume, in which the measured heat is equivalent to the
change in internal energy of the system [1]. Generally,
the use of a coffee-cup calorimeter is often used, since it
II. METHODOLGY
operates easier than the bomb calorimeter. Nevertheless,
bomb calorimeters are preferred, whenever more
2.1 Materials and Reagents
accurate measurements are required, and whenever the
For the first part of the experiment, a weighing
heat evolved in a combustion reaction is needed to be
balance was used to accurately measure the mass of
determined [3]. The invention of the bomb calorimeter
the solid fuel. A porcelain crucible, clay triangle,
dates back to 1881, when Berthelot devised the
stand was used for the heating setup. For the second
equipment, based on the idea that numerous substances,
part of the experiment, a 2000 mL graduated
including hydrocarbons, readily reacts with oxygen
cylinder or beaker was used, a stopwatch, an oxygen
found in the atmosphere.
cylinder was used for the calorimetric process.
The typical bomb calorimeter consists of the
Similarly, benzoic acid was the sample used for the
following: steel bomb, containing the reactants, steel
bomb calorimeter.
bucket, containing the known amount of water,
thermometer and the bomb, a motorized stirrer, and the
2.2 Equipment
outer jacket for insulation [1,3].
In experiment 9A, a Meker burner was used to heat,
Bomb calorimeters operate in a high-pressure
the sample continuously until the formation of ash.
oxygen, which is done inside a stainless-steel container,
Figure 1 shows the setup for the Meker burner.
surrounded by a known amount of water. This water
absorbs the heat evolved from the reaction, and by
determining its temperature change, the heat evolved, or
Qv is calculated. Since bomb calorimeters function in a
constant volume system, the heat is considered to be the
change in internal energy or ΔU [1]. To calculate for the
change in enthalpy for this process, the First Law of
Thermodynamics is applied, and is mathematically stated
as:
Cruz, Dela Cruz, Francisco(your last names only) Dr. Lawrence P. Belo
[2]
 of moisture present initially. The remaining sample
was subsequently heated for 7 minutes. After
heating, the sample was cooled, again, inside the
desiccator, and weighed. Further reducing the loss of
weight from the amount of moisture determines the
volatile matter. Lastly, the remaining sample was
heated until ignition, cooled, and weighed.

2.3.2 Bomb Calorimetry and Heat of Combustion

After all the necessary equipment has been properly

Figure 1. Heating of the coal sample using the Meker
burner.
In experiment 9B, a Parr bomb calorimeter system
was used to ignite the sample, thus allowing the
determination of the heat evolved by the sample.
Figure 2 shows the apparatus, with the necessary
equipment to fully operate the calorimeter. This
setup involved the use of a pail, jacket, cover,
electric stirrer, thermometer, ignition unit, oxygen
filling device, pellet press and fuse wire.
checked and calibrated, a 1.0 gram sample of pellet
was put inside the dish of the bomb cover. A 10 mm
fuse wire was placed onto the terminals of the bomb
cover, and a part of it touching the pellet. 1.0 mL of
water was placed inside the stainless-steel container;
then, was tightly closed and screwed. 10 atm oxygen
was flushed twice inside the bomb, until 25 atm was
reached. The bomb was put inside the tank and was
filled with 2000 mL of water using the graduated
cylinder or beaker available. All wires and tubes, for
the bomb and igniter, and stirrer were connected
prior the ignition. Similarly, the thermometer was
properly adjusted, so that it would immerse in the
water, while having the lens adjusted at the correct
position to perceive the temperature. After setting up
the apparatus, the stirrer was turned on, and
temperature readings was conducted every 30
seconds, until the temperature stabilized. Upon
stabilization, the apparatus was ignited, and
temperature reading was recorded every 15 seconds,
until it stabilized. Afterwards, the setup was
disassembled. The pellet was weighed, while the
length of the remaining fuse wire was measured
using a ruler.

Figure 2. Bomb calorimetry apparatus and equipment

used.
III. RESULTS & DISCUSSION

2.3 Experimental Procedure

3.1 Analysis and Heating Value of Solid Fuels

2.3.1 Analysis and Heating Value of Solid Fuels

The proximate analysis of activated carbon weighing
1.10 g described the composition of the solid fuel to be
The solid fuel sample was weighed using the Mettler
made primarily of volatile matter, followed by fixed
balance. The sample was then heated for
carbon, moisture, and ash, accordingly. The proximate
approximately one minute. It was then cooled inside
analysis is shown in Table 1.
the desiccator and weighed afterwards. The
calculated loss in weight corresponded to the amount
Cruz, Dela Cruz, Francisco(your last names only) Dr. Lawrence P. Belo
[3]
 Table 1. Proximate analysis of 1.0 g activated carbon.
Component Mass (g) % (w/w)
Moisture 0.20 18.18
Volatile matter 0.42 38.18
Fixed carbon 0.36 32.73
Ash 0.12 10.90
Total 1.00 100
From the table, the combustible matter in the solid
fuel is determined to be 70.91%, or the sum of the
percent composition of volatile matter and fixed carbon.
These components provide an approximate on the
heating value of a solid fuel, as it follows from their
capability to combust and therefore give off heat. On the
other hand, moisture and ash are found to comprise
29.09% in the sample. These are components of the solid
fuel which do not contribute to its heating value but
rather lower it, as the vaporization process is
endothermic, describing that the moisture content will
utilize heat simply to vaporize the liquid, and that ash is
incombustible and therefore has no capacity to provide or
use up heat. However, the data remains inadequate in
evaluating the definitive heating value or the calorific
value of the coal sample, as the precise chemical
composition of the volatile matter namely free carbon,
net hydrogen, combined water (oxygen in coal not
present in moisture however treated as though it is
combined with hydrogen), nitrogen, and sulfur must be
known completely, alongside the other known
components from the proximate analysis such as the
moisture, ash, and fixed carbon [5]. Nonetheless, the data
from the proximate analysis is adequate to determine that
the activated carbon analyzed may be used as a solid fuel
for, considering its high composition of combustible
matter and fixed carbon.
3.2 Bomb Calorimetry and Heat of Combustion
The equilibrium temperature of the setup was
recorded at 25.08oC after 300 s. As the sample was
ignited, the initial temperature for the rise period was
recorded at 25.1oC, and the final temperature after 750 s,
taken as the end of the post-period, was 27.52oC. From
these data, it can be observed that the temperature rise is
not significant, which can be expected for a small scale
setup. However, it is important to note that the
thermometer used had fine graduations that allowed for a
more precise recording of temperatures of up to four
Cruz, Dela Cruz, Francisco(your last names only)
[4]
significant figures. Fig. 2 below shows the thermogram
plotted from the temperature data recorded over time.
f(x) =0
28.00
27.50
f(x) = 0 x + 27.09
27.00 26.53
Temperature (oC)
26.50
26.00
25.50
25.00
24.50
24.00
23.50
300 350 400 450 500 550 600 650 700 750 800
Time (s)
Pre-period Linear (Pre-period)
Figure 3. Thermogram for combustion of benzoic acid with
∆Te determined using the 63% rise method
From the graph, the effective temperature change was
determined to be ∆Te=1.43oC by taking the 63% of the
temperature difference at the middle of the rise period,
considered at 465 s, using the linear fitted line equations
for the pre-period and post-period data. The raw data and
data for calculations are listed in Appendix A of this
paper.
Using the effective change in temperature, the heat
capacity of the calorimeter can be determined according
to Eq. 4. Denoted by E , the energy equivalent of the
calorimeter, is given byQ b which refers to the heat of
combustion of the benzoic acid in J/g, m b is the mass of
the benzoic acid sample in grams, C f is the correction
factor determined by the type of wire used equal to
9.62964 J/cm, and ∆ T e is the effective temperature rise
for the reaction in oC.
Q b m b +C f
E= (4)
∆Tc
It can also be observed that Eq. 4 is another form of
an energy balance between the heat absorbed by the
calorimeter expressed by E ∆ T c , and the heat evolved
from the burning of the benzoic acid sample and the fuse
wire, represented by (Q b m b+C f ). No amount of work is
considered as the reaction takes place in constant
Dr. Lawrence P. Belo
volume.
With this, the balanced chemical equation for the
reaction is shown in Eq. 1 with a heat of combustion
∆ H c value of -3227 kJ/mol [5].
inside the tank increased slowly and minutely. It was
observed that the thermometer used was appropriate
and that a less accurate thermometer would not be
able to show the rise in temperature (Soriano).
IV. SUMMARY AND CONCLUSION

Analysis of Heating Value of Solid Fuels

15
C 6 H 5 C OOH (s) + O → 7 C O 2(g )+ 3 H 2 O(l)(1) The experiment gives the students an understanding
2 2(g )
of the proximate analysis of coal. Constituents of the
proximate analysis are mostly based on their boiling
In terms of mass, ∆Hc is equal to 26,424.83 J/g. Using
point since constituents leave after heating or igniting the
this value, the bomb calorimeter setup is found to have
sample after a couple of minutes or reaching a certain
an energy equivalent of 18,515.94 J/oC. This value refers
temperature. Moisture leaves first since it has a lower
to the heat capacity of the bomb cell.
boiling point than the other constituents, while ash
remains since the elements or compounds in it have
Lastly, individual observations from the experiment
higher boiling points than the other constituents. It is
are as follows:
very much recommended to place the sample in a
(1) It was challenging to take note of the temperatures
desiccator to prevent the sample from being
every fifteen seconds. The reader needs to carefully
contaminated by the moisture in the environment.
monitor the rise in the calibration to avoid errors
The proximate analysis obtained 0.20 g moisture,
(Cellona).
0.42 g volatile matter, and 0.12 g ash. Addition of these
(2) For the first part of the experiment, the sample must
three combustion products gives a total of 0.74 g carbon,
be completely cooled down to attain accurate weight
which has a 32.73% difference from the solid fuel initial
measurements. For the second, the initial readings
weight of 1.10 g. This difference can be attributed to the
from the bomb calorimeter were relatively small,
weighing of the crucibles without letting them cool down
which looked like that the combustion was not
completely. Had they been cooled sufficiently, the weight
complete. Upon consulting, though, the value was
of moisture, volatile matter, and ash would have
known to be correct. Similarly, the temperature was
increased; hence, the sum would be closer to 1.10 g.
increasing at a fast rate, making it difficult to
Thus, it is recommended to allot enough time to cool the
determine the reading (Dar).
samples after ignition. 
(3) In the first part, a large part of the coal sample is
composed of fixed carbon. However, there are also
Bomb Calorimetry and Heat of Combustion
carbon in the volatile matter, so the percentage of
The bomb calorimeter can be used to determine the
actual carbon is higher than the percentage of fixed
identity of an unknown sample through the sample’s heat
carbon. For the second part, the bomb calorimeter
of combustion value. If the sample and wire is placed
system is an example of an ideal system to burn
properly, the sample is completely burned. Also, it
fuels since it contains more oxygen than what is
considers correction factors like the heat produced by the
needed (Javier).
burnt wire and the unburnt sample.
(4) In the bomb calorimetry experiment, initially, the
However, the accuracy of the bomb calorimeter in the
ignition of the sample seemed unsuccessful from
laboratory was not tested, since only the first half of the
observing that the temperature data was only
experiment was done. It is recommended to follow the
increasing very gradually at very small increments.
laboratory manual and do the second half of the
However, upon opening the calorimeter at the end of
experiment, which is to determine the heat of combustion
the experiment, the sample was gone and completely
of another sample based on the heat capacity of the bomb
combusted. The thermogram plotted also illustrated
calorimeter using benzoic acid and compare it to the
that the temperature rise after the ignition period was
theoretical data. The second half of the experiment will
significant (Lopez).
show how big the deviation of the experimental data to
(5) After igniting the bomb calorimeter, the temperature
the theoretical data. Also, the difficult part of using bomb
Cruz, Dela Cruz, Francisco(your last names only) Dr. Lawrence P. Belo
[5]
calorimeter is the determination of effective temperature
change since personal bias like determining the points to
consider during the reaction and the estimation in the
points in the graph.
For the bomb calorimetry and heat of combustion, the
obtained heat capacity of the calorimeter was 18,515.94
J/oC.
V. ANSWERS TO GUIDE QUESTIONS
1. What does bituminous coal refer to?
Bituminous coal or soft coal is the most
abundant form of coal. It is something that is
widely used in the steam generation in electric
power plants and industrial boiler plants. It is
called bituminous because it contains a tar-like
substance called bitumen.
2. What are the constituents of coal?
Coal is a carbon-rich material. It does not only
contain organic matter, but it also has small
amounts of inorganic constituents. It is not a
homogeneous substance. Thus, it does not have
a fixed chemical formula. The main constituents
of coal are carbon, oxygen, and hydrogen.
However, there are also other constituents such
as ash, sulfur, and the undesirable chlorine and
REFERENCES
[1] LBYCHED manual [PDF Document]
[2] Principles of combustion, solid fuels [PDF Document]
[3] Available online at
https://chem.libretexts.org/Textbook_Maps/Physical_and_Theoretical_Chemistry_Textbook_Maps/Supplemental_
Modules_(Physical_and_Theoretical_Chemistry)/Thermodynamics/Calorimetry/Constant_Volume_Calorimetry
[4] 374Calorimetry-Callis16 [PDF Document]
[5] Himmelblau, D. M., and Riggs, J. B. Basic principles and calculations in chemical engineering. 7th ed. New Jersey,
Prentice Hall, 2004. 
Cruz, Dela Cruz, Francisco(your last names only)
[6]
sodium.
3. What are the important by-products from
distillation or carbonization of bituminous coal?
Coal derivatives are the important by-products
from the distillation of carbonization of
bituminous coal. When distilled, the remaining
material is called coke, while the gases that are
formed are further processed to become
ammonia, coal gas, and coal tar. Ammonia is
useful as a fertilizer in the agricultural sector.
Coal gas, having many combustible substances,
makes it a suitable fuel for substances that have
high calorific values. Coal tar is useful for both
medical and industrial applications.
4. What are the different types of coal?
The most useful and widely used application for
classifying coal is according to their ranks. The
highest rank is anthracite, a hard, brittle, and
black lustrous coal. It contains a high percentage
of carbon matter and low percentage of volatile
substances. Bituminous coal is next in rank and
is the most abundant type of coal. Lignite coal is
the lowest type of coal and has the least
concentration of carbon.
Dr. Lawrence P. Belo
APPENDICES

A. Raw Data

Table 2. Analysis and heating value of solid fuels.

    Mass (g)
A. Determination of Moisture
Crucible 44.57
Crucible and Solid Fuel 45.67
Solid Fuel 1.10
After drying 45.47
Weight of Moisture 0.20
B. Volatile Matter
Crucible with Dehydrated Sample 45.47
After 7 mins. of Ignition 45.05
Volatile Matter 0.42
C. Determination of Ash
Crucible with Ignited Sample 45.05
After 15 mins. of ignition 44.69
  Fixed Carbon 0.36
Ash 0.12

Table 3. Bomb calorimetry and heat of combustion.

Mass (g)
Benzoic acid 1.00
Remaining weight 0.05
Length (mm)
Wire 10.00
Remaining wire 5.50

Table 4. Temperature over time after ignition.

Time
Temperature (oC) Time (s) Temperature (oC)
(s)
0 25.08 315 26.82
60 25.08 330 27.00
120 25.08 345 27.08
180 25.08 360 27.14
195 25.10 375 27.20
210 25.28 390 27.28
225 25.46 405 27.32
240 25.68 420 27.36
255 26.00 435 27.38
270 26.28 450 27.42
285 26.46 465 27.44
300 26.66 480 27.46
Cruz, Dela Cruz, Francisco(your last names only) Dr. Lawrence P. Belo
[7]
 Time
Temperature (oC)
(s)
495 27.46
510 27.48
525 27.48
540 27.49
555 27.50
570 27.50
585 27.52
600 27.52
615 27.52

B. Sample Calculations

 Conversion of pressure in kp/cm2 to kPa at 5 min

kp
P ( kPa )= P
( cm2 )( 0.0981
1
kp
MPa 1000 kPa

)( 1 MPa )
cm2

C. Photos

Figure 4. Recording the temperature over time in the bomb calorimetry experiment.

Cruz, Dela Cruz, Francisco(your last names only) Dr. Lawrence P. Belo
[8]