Experiment N0.

4
HEAT OF COMBUSTION
Dellosa Joash Kurt 9/08/16
Group 1 9/08/16

I. Objectives
To determine the heat of combustion of an unknown sample
II. Theory
Enthalpies of combustion can be determined reliably using bomb calorimeters. Bomb
calorimetry is used to measure the heat that a reaction absorbs or releases, and is practically used
to measure the calorie content of food. A bomb calorimeter is a type of constant-volume
calorimeter used to measure a particular reaction's heat of combustion. For instance, if we were
interested in determining the heat content of a sushi roll, for example, we would be looking to
find out the number of calories it contains. In order to do this, we would place the sushi roll in a
container referred to as the "bomb", seal it, and then immerse it in the water inside the
calorimeter. Then, we would evacuate all the air out of the bomb before pumping in
pure oxygen gas (O2). After the oxygen is added, a fuse would ignite the sample causing it to
combust, thereby yielding carbon dioxide, gaseous water, and heat. As such, bomb calorimeters
are built to withstand the large pressures produced from the gaseous products in these
combustion reactions.[1] Once the sample is completely combusted, the heat released in the
reaction transfers to the water and the calorimeter. The temperature change of the water is
measured with a thermometer. The total heat given off in the reaction will be equal to the heat
gained by the water and the calorimeter. The change in temperature increased could be measured
during the combustion using the formula: qv= CvΔT. The heat capacity constant must be
obtained first by using the standard benzoic acid which is used widely and normally combusted
in nearly identical bomb calorimeters that’s why it’s the substance used.[2] When something is
burning in the calorimeter, there are several side reactions that happen therefore generating
additional heat. Since we only want to get the heat generated by the sample, the equation which
𝐶 𝛥𝑇−𝐸 −𝐸
is qv= CvΔT will be changed to 𝑞 = 𝑣 𝑚𝑁 𝐹 , where EN is for the correction of heat released
from nitrogen, EF for the fuse wire.
III. Procedures
 Read the operating manual about the bomb calorimeter
 Study the instructions
 Learn the manipulation of the equipment
 Run 2 tests, one for 1.0 g of benzoic acid and an unknown sample
 Weigh out 1.0 g portions of benzoic acid and an unknown sample provided by the
instructor using a top loading balance.
 Form the solids into pellets using a pellet press, place each in labelled weighing bottle
and weigh as accurately as possible in the analytical balance.
 Cut a piece of fuse wire using the measuring device provided in its holder.
 Sand lightly the bomb terminals to ensure a good electrical contact with the fuse wire
then thread the wire to the holes of the terminals following the instructions provided in
the manual
 Place the sample holder in position and place the weighted sample pellet.
 Check that the O-ring located in the groove of the lower lid of the bomb is properly
positioned. Assemble the bomb.
 Fill the bomb with oxygen following the instructions provided in the manual
 Fill the calorimeter bucket with exactly 2000 g of water.
 Place the bomb in the bucket. If bubbles rise, remove the bomb and depressurize it.
Adjust or replace the sealing ring and reassemble
 Switch the calorimeter on.
 Open the calorimeter lid and position the calorimeter bucket on the 3 lugs on the base of
the outer jacket assembly
 Insert the banana plugs into the sockets in the bomb making sure of proper contact of the
electrodes and the bomb firing socket.
 Press start and the calorimeter asks for necessary data like sample id, date and others. It
will automatically start and beep once the bomb fires.
 A value of heat will be displayed. Remove the bomb from the assembly and release
oxygen.
 Wash the inside of the bomb including the capsule with distilled water.
 Titrate the washings with the standard NaoH solution.
 Measure the length of the unburned fuse wire.
 Clean and dry the bomb and repeat procedure using the unknown sample.

IV. Abstract
The objective of the experiment is to determine the heat of combustion of the unknown
sample using the heat capacity of Benzoic acid as a standard at constant volume. The experiment
will use the parr adiabatic bomb calorimeter which reliably could get the enthalpy of
combustion. The instructions on how to operate the calorimeter should be read thoroughly to
prevent any accident and to generate accurate results. Once the sample is completely burned,
there is a need to titrate the washings since inside the bomb, the heat of combustion of the
sample is also accompanied by the heat of combustion of the acid formed and also the heat
generated by the fuse wire used. The results show that as more amount of sample is tested, a
higher rise in temperature will occur showing that the heat of combustion is an extensive
property. Once the experiment is done, the heat of combustion could be calculated by deducting
the amount of heat generated by the acid and the heat generated by the fuse wire to the enthalpy
of combustion of sample divided by the mass.

V. Data and Results

Benzoic Acid Unknown Sample
Mass sample, g 0.9969 0.5525
Temperature rise, °c 2.73338 1.50492
Molarity NaOH, M 0.0725 0.0725
Volume NaOH used, mL 8.967 5.87068
Length of fuse wire, cm 10 10
EN, cal 8.967 5.87068
EFe, cal 18.7 19
Cv, cal/°c 0.27046 0.27046
ΔH, cal/g -27.01147 -44.27812

VI. Discussion of Results

The data shows a difference between the temperature rise of the unknown sample and
Benzoic acid. This shows that as more amount of sample was burned, the more the temperature
rises if you compare the mass between the unknown sample and Benzoic acid. The unknown
sample has less mass compared to benzoic acid and showed a less change in temperature rise
compared to benzoic acid. The volume of NaOH used in Benzoic acid is more than the volume
of the NaOH used for the unknown. This showed that more heat was generated by the acids
within the bomb or the nitrogen that reacted with water to form nitric acid in the combustion of
Benzoic acid than in the combustion of the unknown sample. The more acid formed by the
combustion of Benzoic acid shows a less heat of combustion of Benzoic acid. Now when looking
at the combustion of the unknown sample, it shows a higher heat of combustion with a lower
acid formed since the volume of NaOH used is less than the volume used in the Benzoic acid.
The burnt fuse wire was almost the same on the two samples and shows somehow that it was
almost completely burned. Since what is happening in the bomb cannot be seen, the relationship
of the burned fuse wire with the purity of the sample cannot be established. It does not show how
pure the substance was just by looking at the burned fuse wire. Now since the wire was burned,
and there are some NaOH used when the washings were titrated, it confirms that there are some
nitrogen present in the system and it reacted to water to form acid as predicted by the theory. So
there is a proper correction for the heat generated by the acid. The heat of combustion of the
unknown sample is greater than that of Benzoic acid since the mass of the unknown sample is
less than that of Benzoic acid. One possible source of error will be on the titration of the
washings since the moles of acid that have reacted with the base is important to get the amount
of acid that has generated heat in the bomb calorimeter. This is crucial since this is the only part
where human error could occur given that the experiment uses a Parr adiabatic bomb calorimeter
where much of the work will be done by the machine and the task left is to get the change in
temperature and calculate the heat of combustion.
VII. Conclusion
The experiment was able to determine the heat of combustion of the unknown sample. It
shows that the heat of combustion of a sample inside a bomb calorimeter should be corrected
since there are some other heat generated which is of the fuse wire and the nitrogen present in the
system that formed acids. Since the temperature rise depends on the amount of sample, the heat
of combustion is an extensive property.

VIII. Appendices

Boundless. “Constant-Volume Calorimetry.” Boundless Chemistry. Boundless, 26 May. 2016.

[1]

Retrieved 06 Sep. 2016 from https://www.boundless.com/chemistry/textbooks/boundless-

chemistry-textbook/thermochemistry-6/calorimetry-60/constant-volume-calorimetry-283-1830/
[2]
Hawtin P. (n.d.). Retrieved September 06, 2016, from
http://www.nature.com/nature/journal/v210/n5034/abs/210411a0.html

Sample Cal’n:

Molarity NaOH: (gKHP/Μu) ÷ L = (0.8020/204.22) ÷ (53/1000) = 0.074097 M

Volume NaOH used: M1/V1 = M2/V2 = 0.074097/6 = 0.0725/V2

V2 = 5.87068 mL

EN = V0.0725M = 5.87068 cal

EFe = 2.3 cal/cm (total length- unburnt) = 2.3(10-1.739130) = 19 cal

0.9969 1 𝑐𝑎𝑙
Cv = n(Cpm-R) = (146.8 – 8.314)( )(4.184 𝑗) = 0.27046 cal/°c
122

ΔH = ( CvdT - EN - EFe ) ÷ m = ( (0.27046×1.50492) - 5.87068 - 19 ) ÷ 0.5525 = -44.27812 cal/g

 MSDS
Benzoic Acid
Physical state and appearance: Solid.
Molecular Weight: 122.12 g/mole
Color: Not available.
pH (1% soln/water): 3 [Acidic.]
Boiling Point: 249.2°C (480.6°F)
Melting Point: 122.4°C (252.3°F)
Potential Acute Health Effects: Hazardous in case of skin contact (irritant), of eye contact
(irritant), of ingestion, of inhalation. Slightly hazardous in case of skin contact (permeator). The
substance is toxic to lungs, the nervous system, mucous membranes. Repeated or prolonged
exposure to the substance can produce target organs damage.
Eye Contact: Check for and remove any contact lenses. In case of contact, immediately flush
eyes with plenty of water for at least 15 minutes. Cold water may be used. WARM water MUST
be used. Get medical attention.
Skin Contact: In case of contact, immediately flush skin with plenty of water. Cover the irritated
skin with an emollient. Remove contaminated clothing and shoes. Wash clothing before reuse.
Thoroughly clean shoes before reuse. Get medical attention.
Serious Skin Contact: Wash with a disinfectant soap and cover the contaminated skin with an
anti-bacterial cream. Seek immediate medical attention. Inhalation: If inhaled, remove to fresh
air. If not breathing, give artificial respiration. If breathing is difficult, give oxygen. Get medical
attention

Sodium Hydroxide

Physical state: solid

Form: Pellets
Color: White
Odor: Odorless
pH: 13 (5,0 g/l,)
Melting Point: 323 °C
Boiling Point: 1.388 °C
Physical Hazards: Corrosive to metals
Health Hazards: Skin corrosion, Serious eye damage
Inhalation: In case of inhalation of spray mist: Move person into fresh air and keep at rest.
Consult a physician for specific advice.
Eye contact: If in eyes, hold eyes open, flood with water for at least 15 minutes and see a doctor.
Call a physician or poison control center immediately.
Skin Contact: Wash skin thoroughly with soap and water. Immediately flush with plenty of water
for at least 15 minutes while removing contaminated clothing and shoes. Call a physician or
poison control center immediately. Wash contaminated clothing before reuse. Destroy or
thoroughly clean contaminated shoes.
Ingestion: Promptly get affected person to drink large volumes of water to dilute the swallowed
chemical. Get medical attention immediately.