CLP 303: Chemical Engineering Laboratory - III

Semester IIA, 2020 - 2021

Experiment Name (as given in Bomb calorimeter (Exp 10)

handout)

Group day (Mon/Tue/Thu/Fri) Tuesday

Sub group-9
Subgroup Number

30/08/22(Tuesday)
Date/day of submission

Date/day of common doubt session

for the experiment 23/08/22

Sankalp Bhardwaj (2019CH10125)

Sunandita Borah(2019CH10137)
Names of group members Aryan (2019CH10078)

Gaurav Goel
Name of the lab instructor

Marks (to be filled by instructor / TA)

Objective:

The objective of this experiment as follows: -

❖ To understand the operation of a bomb calorimeter.

❖ To find the value of water equivalent of the calorimeter using benzoic acid.

❖ To determine the calorific value of wood dust.

Apparatus:
Bomb calorimeter, Pellet press, Thermometer, Nichrome wire, Thread, Pipette

Chemicals:
Benzoic acid, Wood dust, Distilled water

Experimental Setup:

Fig1: Experimental Setup

Bomb: The bomb's body is a cylindrical container with a 303 ml capacity. The walls can
readily withstand both the extraordinary pressures of 300 atmospheres and the usual
working pressure of 30 atmospheres. There are two connections on the lid. These
terminals are connected by two metallic rods, one of which has a ring and a tiny hook
for holding the sample crucible and the other of which has a groove. A ring to push a
fuse wire linked to it is also supplied on each rod. Additionally, the upper portion of the
lid has a little hook for raising it and a Schrader valve for adding oxygen to the bomb.
Additionally, a pressure gauge is included for measuring the oxygen pressure.

Water Jacket: To reduce radioactive losses, it is composed of copper and has a thick
layer of chromium plating on the outside. A rod to support the stirrer unit, a threaded
adapter to hold the rod for the Beckman thermometer, and a tiny pipe to deliver water
are all attached to the top of the jacket. The thermometer used to gauge the
temperature inside the jacket is likewise supported by this pipe.

Offset Stirrer: It comprises of a fan-driven stirrer that runs continuously at 800 rpm. In
order to prevent radioactive heating, the motor unit was kept at a suitable distance from
the vessel.
Gas release valve: It is used to collect gases after use and to release the pressure of
the bomb's gases. It is attached to the Schrader valve that is built into the bomb's lid. To
let extra oxygen gas out of the tube, turn the knob down in a clockwise direction.
Pellet press: The punch and die on the pellet press have a diameter of around 12 mm.
Before burning, powdered samples are formed into pellets. This slows down the burning
process and has the effect of keeping the particles inside the capsule, decreasing the
likelihood of incomplete combustion. Additionally, handling pellets is simpler than
handling loose samples. The pellets shouldn't be very hard because doing so increases
the likelihood that they would burst when ignited, which would result in insufficient
combustion.
Crucible: Stainless Steel crucible, holding the sample.
Ignition wire: Nichrome fuse wire is used to start the sample's burning. The electrodes
are connected to one 10-cm-long piece of fuse wire. When working with pelleted samples,
bend the wire such that the loop presses firmly enough on the edge of the pellet to retain
it to the side of the capsule.

Procedure:

1. Pelletize samples of one gram of wood dust and one gram of benzoic acid. Place
the pellet in the crucible after weighing it, and then use a pipette to add 2.0 ml of
distilled water to the bomb.
 2. Stretch a section of the firing wire over the bomb's electrodes. Place the crucible
in place and arrange the loose ends of the thread so that they are in touch with the
material. Tie a length of sewing cotton measuring about 10 cm around the wire.

3. With care to avoid disturbing the sample, pipette 2ml of distilled water into the
bomb, then cover it with the lid.

4. Connect a copper tubing to the high-pressure valve's outlet and place it in the
oxygen cylinder's outlet. Lightly tighten the union nut. Make the connections as
light as possible by connecting the copper tube to the pressure gauge, the filling
tube to the bomb valve, and the pressure gauge to the filling tube. Open the
cylinder's filling connections control valve gradually. Close the control valve for the
collection of gases after monitoring the gauge and allowing the pressure to
increase until the appropriate level is attained (about 30 atmospheres).

5. Submerge the bomb's nut to a depth of at least two millimetres in the water jacket
after adding 2 litres of distilled water, leaving the terminals protruding. Cover the
equipment.

6. Start the stirring mechanism, which must be maintained running continuously at a

steady speed during the experiment. Adjust the stirrer. Position the thermometer
and covers.

7. As soon as the temperature reaches a steady value, continue gathering

thermometric measurements from the automated system, which samples the
temperature every 5 seconds.

8. Open the valve to relieve pressure after removing the bomb from the calorimeter.

9. By observing that there is no sooty deposit within the bomb, you may confirm that
the combustion has finished.

Theory And Derivation:

The heat produced when material burns in a sealed chamber (referred to as a "Bomb") in
an atmosphere of pure oxygen gas is measured with a bomb calorimeter. Initial burning
of the sample takes place in the bomb while it is being flushed with pure oxygen. A fuse
wire is used to electrically ignite the sample. The temperature of the calorimeter assembly
rises while the sample burns, reflecting the heat generated by the exothermic combustion
reaction. Knowing the water equivalent of the calorimeter assembly and the temperature
increase allows one to calculate the heat of combustion of the sample because, barring
the loss of heat, the amount of heat produced by burning the sample must be equal to
the amount of heat absorbed by the calorimeter assembly.

If W represents the calorimeter assembly's water equivalent in calories per degree C;

ΔT = Increase in temperature, measured in degrees Celsius by a sensitive thermometer;
ΔH stands for the sample's heat of combustion in grammes of calories (calorific value)
M is the sample's burned mass in grams.
So,

W ΔT = ΔH M.
ΔH can be determined easily as W,ΔT and M are known. In this experiment, we use a
sample of benzoic acid to determine the calorimeter's first water equivalent (known
calorific value). Additionally, this is utilised to calculate the calorific value of wood dust.
CALCULATIONS:

ʃ(m Cp dT) = Q (heat generated)

m Cp(T final – T initial) = Q

Q = ΔH*M

M: Mass of fuel sample in grams

ΔH: Heat of combustion of standard benzoic acid in calories per gram

m*C : Heat capacity of water represented as water equivalent (W) in calories per degree
p

centigrade

Replacing above values results in the following formula :

Where:

W- Energy equivalent of calorimeter in calories per degree centigrade;

ΔH- Heat of combustion of standard benzoic acid in calories per gram:

M- Mass of standard benzoic acid sample in grams;

ΔT - Corrected temperature rise in degrees centigrade;

E1- Correction for heat of formation of nitric acid in calories; and

E2- Correction for heat of combustion of firing wire, in calories

Water equivalent calculation of a 0.955 gram benzoic acid sample: (6319 Cal/gram)
produced a net corrected temperature rise of 2.609°𝐶. The acid titration required 2.8 ml
of .1 N standard alkali and 7.5 cm 18.4 mg of Nichrome wire and 8 cm (5 mg) of cotton
thread were consumed in the firing.
Substituting in the standardization equation:
H = 6319 cal/gram.
M= 0.955 gram.
E1 = (2.8 ml) x (1.43 cal/ml) = 4.0 cal.
E2 = (18.4 mg) x (0.335 cal/mg) + (5 mg) X (4.180 cal/mg) = 6.0 + 20.9 = 27.1 cal.
ΔT = 2.609 °𝐶
W = ((6319 x 0.955) +4 +27.1)/ 2.609 = 2325 cal/°C
NOTE: Calorific value of nichrome wire of 36 SWG (diameter 0.0913 cm) is 0.82cam/cm.
For calculating the calorific value of wood dust, We take W= 2422 cal/°C, and E1+ E2=
108cal.
RESULTS:

 The theoretical value of water equivalent of benzoic acid is 2352 cal/celsius and the
experimental value comes out to be 2509 cal/celsius.

 The calorific value of the wood dust sample is 4918.64 cal/g

 The calorific value of the black wood dust sample is 4203.16 cal/g

DISCUSSION:

 The water equivalent is the weight which has the same heat capacity as that of the
entire system (Calorimeter vessel containing a specified weight of water;
calorimeter bomb charged with oxygen, fuel and water; thermometer and stirrer).

 Since the specific heat of the water is 1 cal/g℃ in the range 10 to 40 the water
equivalent is approximately equal to the heat required to affect unit temperature
rise in the system under the condition of a calorimeter determination.
  The effective heat capacity has a temperature dependence since the specific heats
of the constituent parts of the system vary with temperature. 25 has been chosen
as the reference temperature because of its use in thermochemical calculations
and because the specific heat of the water in the range 25 to 40 is constant.

Precautions:

 We should not use too much sample. The impact of combustible charges that
release more than 10,000 calories cannot be anticipated to be tolerated by the
bomb. As a result, the total weight of flammable material is often limited to 1.10
gram or less. If an accidental excess of oxygen is introduced, do not ignite the
bomb and do not charge with more oxygen than is necessary.

 Maintain constant good condition for all the bomb's components, notably the
insulated electrode assembly. If the bomb is submerged in water and gas bubbles
are flowing from it, do not launch the bomb.

 After firing, step back at least 15 feet from the calorimeter, and most all, stay away
from its top. The power of the explosion, if the bomb were to detonate, would
probably be directed upward.

 When evaluating novel materials that burn quickly or have explosive properties,
proceed with caution and utilise just a small portion of the permitted maximum
sample.

CAUSES OF POOR COMBUSTION: An incomplete combustion in the oxygen bomb is

nearly always due to one or more of the following causes:

 Excessively, rapid admission of gas to the bomb during charging, causing part of
the samples to be blown out of the cup.
 Loose or powdery condition of the sample in the cup prior to ignition causing
ejection due to violence of combustion.
 The use of a sample containing coarse particle which cannot burn readily with coat,
such particle are usually too large to pass through 60 mesh screen.
 The use of a sample in the form of pellet which has been made too hard, causing
the fuse to and the ejection of fragment during heating.
 Use of an ignition current too low to ignite the charge or too high, causing the fuse
to break before combustion is well under way.
  Insertion of the fuse wire loop below the surface of a loose sample- Best results
are obtained by barely touching the surface of the sample or even hanging the wire
slightly above the surface.
 Use of not enough oxygen to burn the charge completely or conversely, the use of
a very high initial gas pressure which may retard development of the required
turbulence during combustion.

Scope for further Improvement:

 We should take care of the above points to avoid poor combustion.

 Many in-between time readings are not taken, which may be causing the
estimation error; thus, increasing the number of measurements at different times
or reducing the time gap between the measurements would give an accurate
estimation of the Temperature Gradient.