BOMB CALORIMETER

A bomb calorimeter is a constant volume

calorimeter (constant volume is isochoric). So the
heat measured by such an instrument is equivalent to
the change in internal energy or ΔUΔU. The heat can
be determined from the temperature change, ΔTΔT,
and the heat capacity of the calorimeter, CcalCcal.
For a bomb calorimeter, the heat capacity is usually
quite large due to all the water and the hardware
(stirring paddles, blades, the stainless steel "bomb"
holding the reactants, the wiring, the walls of the
calorimeter, etc...). This value is CcalCcal. It is used
to find qvqv of the system:

A bomb calorimeter is a type of constant-

volume calorimeter used in measuring the
heat of combustion of a particular reaction.
Bomb calorimeters have to withstand the large
pressure within the calorimeter as the reaction
is being measured. Electrical energy is used to
ignite the fuel; as the fuel is burning, it will
heat up the surrounding air, which expands
and escapes through a tube that leads the air
out of the calorimeter. When the air is
escaping through the copper tube it will also heat up the water outside the tube. The
change in temperature of the water allows for calculating calorie content of the fuel
(Polik, 1997).

PARTS OF BOMB CALORIMETER

In the oxygen bomb calorimeter there are three main parts:
 A bomb, which houses the sample and oxygen for the combustion reaction.
 The steel bucket, which holds a measured amount of water, thermometer and the
bomb.
 The outer jacket, which thermally insulates the entire apparatus.

PROCEDURE
The apparatus must be calibrated first. By measuring the temperature rise from
the combustion of a known substance, one can determine the heat capacity of the
apparatus. The combustion of benzoic acid (26435 J/g or 6318 cal/g C6H6O2) is
usually used.
Preparation of the sample:
Benzoic acid is a powder and needs to be compressed into pellets. A
pellet is made from approximately 0.8 to 0.9 g of benzoic acid. Any
powdered sample in a bomb calorimeter must be formed into tightly-
packed pellets so that the entire sample will combust. The picture
below shows how to fill the pellet press mold with the powdered
sample:

After filling the pellet press mold with the powdered sample,
position the mold in the press and put pressure on the powder by
firmly pressing the handle down in a smooth stroke: Preparation of
the bomb: Place the bomb head on its stand. Using steel wool, polish
the two electrode terminals and the bomb head. Weigh the pellet to
0.1 mg. Cut a piece of Fe ignition wire ~12 cm in length. Weigh the
wire to 0.1 mg. Attach the wire. Put the solid pellet in the ignition
cup and wrap the wire around the ends of the electrode terminals.
Bend the wire so that it is in good contact with the pellet but does
not touch the ignition cup anywhere. Sealing of the bomb apparatus:
Taking care to maintain the setup of the bomb head intact (you want
to keep the wire connected to the electrodes and in contact with the
sample), gently place it in the body of the bomb and screw the head
into place. Check for electrical continuity by connecting an ohmmeter
across the external terminals on the bomb. If the resistance is low,
there is good connection between the fuse wire and the terminals. If
the resistance is infinite, the wire is not making good contact with
the electrodes and the bomb must be opened and the wiring checked
before continuing. Close the outlet valve on top of the bomb. Do not
over tighten. With the valves on the oxygen tank closed, attach the
inlet tube from the tank to the bomb. Slowly let 20 atm of oxygen
into the bomb by opening the valve on the oxygen tank. Then close the
tank valve. Bleed the gas out of the bomb by slowly opening the
outlet valve on the bomb head until you no longer hear a hissing
sound. Repeat this fill-and empty cycle two more times at least. This
ensures that there is pure oxygen in the bomb. Slowly let 25 atm of
oxygen into the bomb. Do not empty the gas from the bomb this time.
Below is a picture of how to connect the bomb to the O2 gas tank.
Place the bucket into the insulating jacket and be sure that it sits
flat. Measure 2 L of water with a volumetric flask and place it into
holding bucket. Make sure that the temperature of this water is near
the lower end of the temperature range visible on the thermometer
that is inserted into the calorimeter. Attach the lead wires to the
bomb while holding the bomb above the water. Gently lower the bomb
into the bucket and be sure that it sits flat. Put the lid into place
and clamp the lid down until snug. Do not over tighten the c-clamps
or you could crack the cover. Lower the thermometer into the
calorimeter. Use care as these thermometers are very fragile and very
expensive. Attach the rubber belt to the stirring motor. Below is a
picture of how the apparatus is assembled. Combustion of the sample:
Now you are ready to fire the charge and start taking time and
temperature readings. Before you fire the charge, make sure the timer
is on zero and that you can see the thermometer easily. Record the
temperature every 15 seconds for about three minutes prior to firing
the charge. Firing the charge: One person should push both the
ignition button and the timer button at the same time. Hold the
ignition button down for 2 to 5 seconds. Do not hold it down more
than 5 seconds. Keep your eye on the light as you push the button. It
should turn on briefly. The temperature will probably need about 20
seconds after ignition to begin rising. You should see a steady
increase in temperature for the first few minutes and then it may
slowly decrease. In a group: one person can read time, one reads
temperature, and one records the data. Continue to take readings for
two to three minutes after you have three consecutive temperature
readings within +/− 0.05 °C. When the run is complete, turn off the
stirring motor, lift and move the cover. Lift the metal bucket out of
the calorimeter, and remove the bomb from the bucket. Carefully dry
the bomb, and gently open the gas outlet valve to relieve the inside
pressure. Once the pressure has decreased (no more hissing), remove
the top of the bomb. Check the inside walls of the bomb for beads of
water or soot. These are signs of complete combustion. If there is
any unburned wire sitting inside the combustion cup or on the two
electrodes, remove it with tweezers and weigh it. Determine the
amount of unburned iron wire. The unburned wire will decrease the
actual amount of heat of combustion by 5858 J/g not burned. Be sure
not to mistake round balls of iron oxides for the unburned wire.
Remove these from the bomb and sample holder.
RERERENCES:

Polik, W. (1997). Bomb Calorimetery. Retrieved

from http://www.chem.hope.edu/~polik/Chem345-2000/bombcalorimetry.htm