Chapter # 3

Experimental setup

CALORIMETRY :
Calorimetry is derived from Latin word “calor”
meaning heat and the Greek word “metry” meaning
to measure. So it is science of measuring the amount
of heat. On this basis we can define the term
calorimetry as
“It is the measurement of the amount of heat
evolved or absorbed in a chemical reaction, in
changing of state, or in the formation of a solution.”
CALORIMETER:
A calorimeter is a devise used to measure heat
of reaction. A calorimeter may be operated under
constant pressure or constant volume.

BOMB CALORIMETER:
DESCRIPTION OF APPARATUS:
• CALORIMETER BOMB:

General design:

Bomb is made of stainless steel. It shall be so constructed that it

does not leak, and can be easily drained. All parts enclosing the gas
space shall be constructed of materials which are not affected
sufficiently by the combustion process or products so as to
introduce measurable heat input or alteration of the end products.
The electrodes shall be made of heat and corrosion resistance
material, e.g. platinum or its alloy, suitable steels or nickel chrome,
and so placed when the oil cup is in position its base shall be not
less than 89 mm from the underside of the bomb lid. The closure of
the bomb should be preferably self sealing.

Materials:

Bomb bodies and heads shall be machined from solid or

hollow forgings, bar, seamless tube or pipe, complying with the
appropriate British Standards. Welding or brazing of major
components is prohibited. Closure sings may be made of any
suitable material chosen to minimize any tendency towards galling
or seizing of screw threads. Gaskets may be made of any suitable
material.

• CALORIMETER VESSEL:

Calorimeter metal vessel polished on the outside, preferably

slightly higher than the bomb and preferably of such cross
sectional area that 2 liters of water will just cover the bomb.
• STIRRER:

Stirrer is mechanical device for stirring the

water in the calorimeter vessel at a uniform rate.
The stirring shall be throughout, but not so rapid
as to cause appreciable heating of water.
Continuous stirring of water in the calorimeter
vessel of the isothermal apparatus for 10
minutes after the thermal equilibrium has been
established shall not cause the increase the
temperature of more than 0.01 oC. With the
adiabatic apparatus continuous stirring of the
water in the calorimeter vessel for 10 minutes
after thermal equilibrium has been established
shall not cause an increase in temperature of
more than 0.002 oC. The portion of the stirrer
immersed in the calorimeter vessel shall be
connected to the outside portion with material of
low conductivity.

• WATER JACKET:
Water jacket is a double walled metal vessel
containing water, fitted with a lid and leaving an
air gap around the calorimeter vessel. The
isothermal jacket shall be arranged so as to
remain at a uniform temperature.
Adiabatic calorimeter shall be capable of
circulating water continuously through both
jacket and lid. The system shall be fitted with
heating and cooling devices such that the
 temperature of the jacket water is automatically
and rapidly adjusted to within 0.1 oC of that of
the water in the calorimeter vessel with
sensitivity sufficiently good to satisfy the
requirements.

• IGNITION CIRCUIT:
The electrical supply used in firing the
charge may be AC or DC. The emf shall be kept
at the minimum need for instantaneous fusion of
the ignition wire. The switch controlling shall not
remain closed for more than 2 sec, and shall be
of a type that remains open except when held in
the closed position by the operator. An ammeter
may be used to indicate when the wire has
fused.

• THERMOMETER:
A 6oC range BS calorimeter thermometer or
a platinum resistance thermometer of equal
accuracy shall be used for determining the rise
in temperature of the calorimeter water.

• OXYGEN CHARGING EQUIPMENT:

Oxygen charging equipment is to be robust,
having a range approximately equal to twice the
normal charging pressure used in the bomb. The
gauge front and back shall be of safety type. An
arrangement of two gauges separated by a
reducing valve may be employed. Pressure
 gauges shall be checked frequently for
accurately.

• IGNITION WIRE:
Ignition wire of platinum or nickel-chrome
may be used. Calculate the heat release from his
source by allowing 335 cal/g for nickel-chrome
wire and 100 cal/g for platinum wire.

• MATERIAL:
OXYGEN:
Oxygen is under pressure in cylinders, free from
combustible material.