Experiment 10: Bomb Calorimetry

Equipment: Bomb calorimeter

Fuse Wire
Thermometer for Bomb Calorimeter
Pellet press

Consumables: Benzoic acid

Oxygen cylinder
Cashew (or M&M's)

Purpose: To calibrate a bomb calorimeter and then use the calibrated bomb calorimeter to determine
the calorie content of a cashew.

Background:

One of the most important types of reaction studied by means of calorimetry is combustion. We can
measure the amount of heat from a combustion reaction by measuring the effect the heat produced
from the reaction has on a container surrounding the reaction chamber filled with water. This apparatus
is called a bomb calorimeter, and is composed of an insulated container of water in which there is a
metal "bomb“ (reaction chamber), a stirrer and a thermometer (Fig I ). The bomb is a strong metal
container that can withstand the high pressures associated with the rapid combustion of a material and
transmit the heat to its surroundings very quickly. Inside the bomb is a sample holder, an electrical
ignition system to start the reaction and enough oxygen gas to achieve complete and rapid combustion.
Theory:

To calculate the heat of combustion, the sample is placed in the sample holder arid sufficient oxygen is
pumped into the chamber to allow for complete combustion. The reaction chamber is then immersed
in the water, and the initial temperature checked over a length of time to ensure that the temperature is
stable before beginning the combustion reaction. After the combustion reaction is performed, the final
temperature is recorded. The increase in temperature corresponds to the amount of heat generated
(evolved) by the combustion reaction.

To calculate the heat of combustion from the increase in temperature of the water, we need to first find
the relationship between the temperature changes we measure in the experiment and the heat produced
from a reaction. This is the heat capacity (Ccal) of the whole calorimeter, including the bomb, water,
stirrer, thermometer and calorimeter casing. The process of finding Ccal called calibration. We do
these by combusting a sample of benzoic acid which produces a known amount of heat and observing
the temperature change of the apparatus.

For example, it is known that the combustion of 1.000 g of benzoic acid (C7H6O2) will produce
-26.38kJ of heat. If we combust 1.000 g of benzoic acid in a bomb calorimeter, and observe a
temperature rise of 5.022 ° C, the heat capacity of the calorimeter would be given by

q evolved = -C calorimeter T

Which rearranges to give:

-q evolved = calorimeter
T

Plugging in the known heat of combustion for benzoic acid gives:

o
(-26• 38)kJ = C calorimeter = 5 .253 kJ/
5.022 ° C
This relationship means that for the apparatus in this example if we ever see a I °C temperature
increase when doing a reaction, the reaction produced 5.253 kJ of heat. If you observe a 2 °C
temperature increase in this apparatus, the reaction produced 10.56 kJ ( 2 x 5.253 kJ) etc.

The first part of the experiment is to come up with the relationship between heat and temperature change,
and then we will use this relationship to find the heat produced by the combustion of a cashew (calorie
content of a cashew).
Procedure:

Figure 2. Bomb calorimeter apparatus.

1. Fill the calorimeter water bucket with 2.00 Liters of distilled water. The amount of water must
be reproducible (so that the heat capacity of the calorimeter will be constant), but it is not
necessary that it be exactly 2.00 Liters. The initial temperature of the water should ideally be
1-2 °C below that of room temperature. PLACE the water bucket in the calorimeter.

2. Obtain (or make using a pellet press) a benzoic acid pellet. The pellet should weight close to,
but not over, 1 gram.
3. Weight the pellet, recording the exact weight in the data table. Be sure to treat the pellet very
gently as not to lose any of the benzoic acid.

4. Cut a 10.0 cm length of string. Tie the string around the benzoic acid tablet.

5. Then attach the string to the wire between the electrodes. If all is not perfect, the benzoic acid
will not ignite (read this as "you need to start over!"). It is okay if the tablet is hanging in the
air and not sitting in the bottom of the cup.

6. Seal the bomb by screwing the bottom part of the bomb onto the top part of the bomb while
the bomb is being held still. When properly closed, no threads on the cylinder should be
exposed. Hand tightening should be sufficient to secure a tight seal.

7. Pressurize the bomb to 30 atm with oxygen. (Caution! Do not exceed 35 atm).

8. Place the bomb into water bucket in the calorimeter, and CONNECT the electrodes to the
bomb and to the ignition unit. Check for gas bubbles coming from the bomb. If any are
observed, the bomb has a leak and will need to be reassembled.

9. Close the calorimeter with its lid. Connect the pulley, and start the motor to begin stirring.
CAREFULLY lower the thermometer into its slot.
 10. Take temperature readings every 30 seconds for 5 minutes. Record in the data table provided.
Then.... At the start of the 6th minute....

11. Ignite the bomb by pressing the ignition button and holding it down until the indicator light
goes out. This can take from 1- 4 seconds. NO MATIER WHAT, DO NOT HOLD THE
BUTTON DOWN FOR MORE THAN 4 SECONDS. The temperature should begin to rise
within 20 seconds after firing.

12. Continue to record the temperature every 30 seconds until the temperature reading stabilizes
and then begins to fall. Continue to record the temperature reading 3 minutes after the
maximum temperature is achieved

13. Stop the motor. CAREFULLY raise the thermometer and the stirrer and remove the bucket
and bomb.

14. Pour the water out and dry the bucket for the next run.

15. Release the pressurized gas slowly from the bomb and then open the bomb.

16. Carefully remove any unburned fuse wire, measure its weight and record that figure.

17. Repeat using a cashew instead of benzoic acid. Be sure to use the same amount of water in the
water bucket as last time.

Discussion

Based on result obtain from the experiment,

Bomb calorimeters are also commonly calibrate by combustion naphthalene. If a 2.00g sample of
naphthalene produce 7.81 °C temperature increase in calorimeter, what is Ccal of the calorimeter. The
heat of combustion of naphthalene is -43.6 kJ/g.

q evolved = -C calorimeter T

Which rearranges to give:

-q evolved = calorimeter
T

Plugging in the known heat of combustion for naphthalene gives:

(-43.6)kJ = C calorimeter = -5.5826 kJ/ ° C

7.81 ° C