Supporting Information

Evaluating the Heats of Combustion of Coals using Bomb Calorimetry in the General
Chemistry Laboratory

A.M. Ranjika P. Bopegedera

Department of Chemistry, The Evergreen State College, Olympia, WA 90505, USA
bopegedd@evergreen.edu

S1: Student Handout

Pre-laboratory assignment – Use your general chemistry textbook to review the components of
a bomb calorimeter. In your laboratory notebook, write down these important components. You
may also want to make a rough sketch of them. You have solved bomb calorimeter problems in
general chemistry. Do one such problem before coming to laboratory.

In the Laboratory:
Bomb calorimetry (constant volume calorimetry) is often used to determine the calorie content in
foods. In this experiment, we will use this technique to determine the heats of combustion of
various coal samples.

Work in groups of four. Your group will be assigned a bomb calorimeter. Do not mix any parts
of your bomb calorimeter with those of other groups for the duration of this laboratory. You will
be provided with the calorimeter constant (heat capacity of the bomb = Cbomb in kJ/°C)) for your
specific calorimeter. Please write this down in your laboratory notebook. The science technicians
obtained this value by calibrating the bomb calorimeter using benzoic acid standard.

Regarding balances: Please use the same analytical balance for all your mass measurements
throughout this experiment. The one exception is when you need to weigh 2000 g of water into
the water jacket of the calorimeter. This exceeds the weight limit of the analytical balance.
Please only use the top loading balance provided in the laboratory for this specific purpose.

Coal samples: You are provided with the following coal samples in the laboratory. You will
analyze TWO different samples (assigned to your group), but you will gather data from the
others, so you have data for all 5 samples (with multiple data sets per sample). The coal pellets
(combining the benzoic acid standard and coal) were prepared ahead of time for you by
laboratory staff. You will be given information on the preparation of these pellets. Please use
forceps to handle coal pellets.
 Sample ID Sample
DECS-9 Sub-bituminous B
DECS-11 Lignite A
DECS-21 Anthracite
DECS-22 High volatile A bituminous
DECS-37 High-volatile B bituminous

1. Measure out about 10 cm of the fuse wire provided for the bomb calorimeter and record the
exact weight of the wire. The heat evolved by the combustion of this wire is on the package.
Please record it. Bear in mind that when the contents of the bomb are combusted, heat is evolved
by the combustion of the coal sample and the wire.

2. Place 1.00 ml of distilled water into the bomb as directed in laboratory.

3. Weigh your sample pellet in the sample holder of the bomb calorimeter using an analytical
balance.

4. Connect the ignition wire to the sample as demonstrated in laboratory. See figure below.

5. After closing the bomb, charge it with ~30 atm of oxygen gas. Please ask help from the
laboratory staff for this step.

6. Place 2000. g of distilled water into the outer chamber of the bomb calorimeter as directed in
laboratory (use the top loading balance and record the exact weight of water). This water sample
absorbs some of the heat generated during the combustion.

7. Place the bomb in the calorimeter, connect the ignition wires, and ensuring the proper assembly,
seal the calorimeter. Insert the thermometer into the calorimeter.

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8. Set up the LabQuest and LoggerPro software to record the temperature for about 30 minutes at
15 data points per minute.

9. Start the stirrer. Begin recording time-temperate data using the software. After about 2 minutes,
and not sooner (you should see a steady temperature versus time graph by then), ignite the
sample inside the bomb. Stand back from the bomb calorimeter and observe the temperature/time
graph on the computer. Continue to stand back from the bomb until you observe a temperature
rise on the computer screen.

10. Upon ignition, temperature should first go up (this will take a little time so be patient) and then
taper off. IF the temperature does not rise, your sample did not ignite. You need to take the
calorimeter apart (consult the instructor about the protocol for doing this step) and re-start the
experiment.

11. You can stop data collection when the final temperature stays steady for about two minutes (and
not sooner). Then, export your data and save it as a Microsoft Excel file.

12. Disassemble the bomb calorimeter (consult the instructor about the protocol for doing this step)
and carefully remove any leftover, uncombusted wire. Measure the weight of this wire. Record
this in your laboratory notebook.

13. Clean the calorimeter thoroughly and repeat the above process with a different coal sample
(assigned to your group).

14. When you have completed the experiment with your two coal samples, please take apart the
calorimeter and clean it thoroughly. Leave all parts by the calorimeter and leave the station.

Post-Laboratory Assignment: Please show all work for your calculations.

1. Define an “isolated system”? Can the bomb calorimeter be treated as a nearly isolated
system? Why or why not?
2. What components make up the “system” in this experiment? What components make up the
“surroundings”?
3. What components absorb thermal energy? What components give off thermal energy?
4. Write a statement showing the law of conservation of energy for the components in the
system and the surroundings.

Determination of the heats of combustion of coal samples –

5. For one of the coal samples you worked with in the laboratory, plot a thermogram
(temperature versus time graph). Attach the thermogram to your laboratory notebook.
6. Determine the average initial temperature and the average final temperature for the two coal
samples you analyzed in the laboratory. Input this data into the class spreadsheet.
7. Calculate the heat absorbed/emitted by each of the components of the system.
8. Use this to determine the heat of combustion of each coal sample.
9. Calculate the heat of combustion for each coal sample in kJ/g and then in BTU/lb (note: BTU
stands for British thermal units. 1 British thermal unit = 1.05505585 kJ)

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10. Analyze the class dataset using Microsoft Excel (use the formula feature wherever possible)
11. Where appropriate, calculate the average and the standard deviation for the heats of
combustion of coals.
12. Based on the analysis, which coal sample is most effective in heating a home and why?
13. Save your spreadsheet electronically for evaluation. Please do not print the spreadsheet.

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 Evaluating the Heats of Combustion of Coals using Bomb Calorimetry in the General
Chemistry Laboratory
A.M. Ranjika P. Bopegedera
Department of Chemistry, The Evergreen State College, Olympia, WA 90505
bopegedd@evergreen.edu

S2: Notes for Instructors

Purchasing coal samples:

 Five different coal samples were purchased for this experiment from the Pennsylvania State
University Coal Bank. DECS samples [50 g (3 oz.) at 60 mesh (0.25 mm)] were purchased and
used without further processing. The cost was about $60 per bag. After opening the bags, they
were re-sealed in an argon environment and stored in the refrigerator. Samples have been used
over multiple years without observable degradation. Please use the following URL to access the
Pennsylvania State University Coal Bank. https://www.energy.psu.edu/services/introduction-
department-energy-coal-sample-bank-and-database

Notes on preparing coal pellets for bomb calorimetry:

1. First, grind up benzoic acid standard (CAS number 65-85-0, purchased from Sigma-Aldrich in
tablet form especially for bomb calorimetry) with a mortar/pestle. A large ceramic mortar is
needed. This takes some effort and the benzoic acid powder is tough on lungs. Wearing goggles,
a mask, and working inside a hood is recommended when grinding these tablets. Make sure that
the acid is well powdered before weighing. The powdered acid is hygroscopic.

2. Using an analytical balance, weigh the coal sample (approximately 1.3 g) into a clean, dry,
container that has a lid. Record the exact weight. Then add enough benzoic acid powder to the
container until the total weight is about 5.5- 6 g. Record the exact weight. Provide these two
weights to students. The goal is for the benzoic acid: coal ratio to be about 75%:25%. Otherwise,
the coal may not combust in the bomb calorimeter.

3. Close the lid and mix thoroughly by shaking the container until the mixture is homogenized. Use
this mixture to make a pellet using the pellet press. The weight of each pellet should be around 1
g (check this with a top loading balance). Students will weigh the pellet using an analytical
balance in the laboratory.

4. Do not store the prepared pellets in a desiccator because they tend to fall apart as they dry.
Instead, store pellets in small, covered scintillation vials (airtight containers- see figure below). A
small amount of moisture might help hold the pellets together a little better. It is best if the
pellets are made the day before the lab.

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 Notes on operating the bomb calorimeter:
Instructors and laboratory staff must read the instruction manual that accompanies the bomb
calorimeter and follow their guidelines carefully. The following precautions (summarized from
the instruction manual) are particularly important.

1. Do not use too much sample. This experiment used about 0.8 g of benzoic acid and about 0.2
g of coal in each sample pellet. It is advised that the mass of the pellet does not exceed about
1.1 g.
2. Do not overfill the bomb with oxygen gas. We used ~30 atm of oxygen. The maximum
prescribed in the manual is 35 atm.
3. Keep all parts of the bomb in good working order. If gas bubbles are visible when the bomb
is submerged in the water jacket, there is an obvious leak, and the bomb should not be fired.
4. Stand away from the bomb calorimeter for 30 seconds after it is fired.
5. Do not use lubricants on valves or fittings in contact with high pressure oxygen.

Notes on calibrating the bomb calorimeter:

Use only a standard benzoic acid pellet to calibrate the bomb calorimeter. Use the analytical
balance only for weighing.
1. Measure out about 10 cm of the wire provided for the bomb calorimeter and record the exact
weight of the wire. Record the heat evolved by the combustion of this wire (provided on the
package).
2. Place 1.00 ml of distilled water into the bomb.
3. Handle the benzoic acid standard only with forceps and when not in use, store them in a
desiccator.
4. Weigh one benzoic acid pellet in the sample holder of the bomb calorimeter using an analytical
balance (weigh the empty holder first, then weigh the holder with the pellet).
5. Place the weighed pellet in the sample holder in the bomb. Set up the fuse.
6. After closing up the bomb, charge it with ~30 atm of oxygen gas.
7. Place 2000.0g (record the exact weight using a top loading balance) of distilled water into the
water jacket of the calorimeter. Place the water jacket in the calorimeter followed by the bomb.
Seal the calorimeter.
8. Set up the LoggerPro software to record the temperature for about 30 minutes.
9. Start collecting time-temperature data using the software. After about 2 minutes, ignite the fuse
inside the bomb.
10. Upon ignition, temperature should first go up and then taper off. IF the temperature does not rise,
your fuse did not ignite. You need to take the bomb apart and re-do the experiment.

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11. The temperature inside the calorimeter will eventually taper off to a constant value. After this
happens, record data for another 2 minutes and stop data collection. Export the data into a
Microsoft Excel spreadsheet.
12. Disassemble the bomb calorimeter and remove any leftover wire and measure the weight of the
unburned wire carefully and record it.
13. Use this data to determine the calorimeter constant for your calorimeter.
14. Repeat the experiment 2 more times to ensure precision.

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 Evaluating the Heats of Combustion of Coals using Bomb Calorimetry in the General
Chemistry Laboratory
A. M. Ranjika P. Bopegedera
Department of Chemistry, The Evergreen State College, Olympia, WA 90505
bopegedd@evergreen.edu

S3: Sample Dataset and Analysis

Data Collected for an anthracite coal sample

Mass of coal used to make pellet mixture (g) 1.32859
Mass of pellet mixture (benzoic acid + coal) (g) 5.52347
Mass of benzoic acid used to make pellet mixture (g) 4.19488
Mass of the pellet (g) 1.03865
Mass of water in calorimeter bucket (g) 2000.00
Initial mass of fuse wire (g) 0.01607
Final mass of fuse wire (g) 0.00510
Average initial temperature in the calorimeter (°C) 18.80
Average final temperature in the calorimeter (°C) 21.60

Thermogram produced for this sample:

22
21.5
21
20.5
temperature (C)

20
19.5
19
18.5
18
17.5
0 2 4 6 8 10 12 14 16
time (minutes)

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Analysis of data:

constants and conversion factors used in calculations

Heat capacity of calorimeter (Ccalorimter) (kJ/°C) 1.933
Enthalpy of combustion of benzoic acid (HBA) (kJ/mol) -3226.9
heat of combustion of wire (cal/g) -1400
-1
Specific heat capacity of water (J g °C ) -1 4.184
-1
gas constant (R ) (kJ K mol )-1 8.314 x 10-3
molar mass of benzoic acid (g/mol) 122.12
1 cal = 4.184 J
1 BTU = 1.0550559 kJ
1 lb = 453.592 g

Calculations:

final temperature (K) = final temperature in °C +273.15 = 21.60 + 273.15 = 294.75 K

mass of wire combusted (g) = initial mass of wire-final mass of wire = (0.01607-0.00510) g =
0.01097 g
fraction of benzoic acid in pellet = mass of benzoic acid used to make pellet mixture/mass of
pellet mixture
= 4.19488 g / 5.52347 g = 0.75946
fraction of coal in pellet = mass of coal used to make pellet mixture/mass of pellet mixture
= 1.32859 g / 5.52347 g = 0.24054
mass of benzoic acid in the pellet = mBA = fraction of benzoic acid in pellet x mass of pellet
= 0.75946 x 1.03865 g = 0.78881 g
mass of coal in the pellet = fraction of coal in pellet x mass of pellet = 0.24054 x 1.03865 g
= 0.24984 g
temperature change = T = final temperature - initial temperature = (21.60-18.80) °C = 2.80 °C
heat absorbed by calorimeter = qcalorimeter = Ccalorimeter x T = 1.933 kJ/ °C x 2.80 °C
= 5.412 kJ

heat absorbed by water =qwater = mass of water x specific heat capacity of water x T =
2000.00 g x 4.184 J g-1 °C-1 x 2.80 °C = 2.343 x104 J = 2.343 x 101 kJ

heat given off by wire = qwire = heat of combustion of wire x mass of wire combusted
=  1400 cal/g x 0.01097 g = 1.5358 x 101 cal =  1.5358 x 101 cal x ( 4.184 J/cal)
=  6.426 x 101 J =  6.426 x 10-2 kJ

moles of benzoic acid in pellet = mass of benzoic acid in pellet / molar mass of benzoic acid
= 0.78881 g /(122.12 g/mol) = 6.4593 x 10-3 mol

Balanced reaction for the combustion of 1 mol of benzoic acid:

C6H5COOH (s) + 7.5 O2 (g)  7 CO2 (g) + 3 H2O (l)
Enthalpy of combustion of benzoic acid = HBA =  3226.9 kJ/mol of benzoic acid

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Relationship between the change in internal energy (U) and the change in enthalpy of
combustion (H): H = U + nRT where n is the change in the number of gaseous moles
in the combustion reaction for benzoic acid, R is the universal gas constant and T is the final
temperature in the calorimeter in Kelvin

For one mole of benzoic acid:

n = 7 mol -7.5 mol =  0.5 mol
T = 294.75 K
R = 8.314 x 10-3 kJ K-1 mol-1
HBA =  3226.9 kJ/mol of BA where BA = benzoic acid

HBA = UBA + nRT

UBA = HBA - nRT
UBA =  3226.9 kJ  ( 0.5 mol x 8.314 x 10-3 kJ K-1 mol-1 x 294.75 K)
=  3225.67 kJ/mole of BA

Amount of heat released by the combustion of benzoic acid in the pellet = qBA
=  3225.67 kJ/mol BA x moles of benzoic acid in pellet

=  3225.67 kJ/mol BA x 6.4593 x 10-3 mol BA

=  2.0836 x 101 kJ

Since the calorimeter is a thermally isolated system:

qcalorimeter + qwater + qwire + qBA + qcoal in pellet = 0 where qcoal in pellet is the heat of combustion
of coal in the pellet

5.412 kJ + 2.343 x 101 kJ + ( 6.426 x 10-2 kJ) + ( 2.0836 x 101 kJ) + qcoal in pellet = 0

qcoal in pellet =  7.942 kJ (extensive property)

qcoal per gram of coal combusted =  7.942 kJ/mass of coal in pellet =  7.942 kJ/0.24984 g
=  31.79 kJ/g (intensive property)

 31.79 kJ 1 BTU 453.592 g

qcoal in BTU/lb = g 𝑥 1.0550559 kJ 𝑥 1 lb
=  1.367 x104 BTU/lb (intensive property)

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 Evaluating the Heats of Combustion of Coals using Bomb Calorimetry in the General Chemistry
Laboratory
A. M. Ranjika P. Bopegedera
S4: Laboratory Notebook Grading Rubric

Description Points
Earned
Pre-Lab (10 points)
 Correct answers to all questions
 Submitted on time
Complete Heading (5 points)
 date, lab partners’ full names, title for experiment
Observations & Data (15 points):
All necessary information recorded, correct units & proper significant figures used, qualitative
observations made, block diagram of experimental set up where appropriate, tabulated data when
possible, used complete sentences, electronic data file saved
Data Analysis (50 points):
 Definition of an isolated system.
 Can the bomb calorimeter be treated as a nearly isolated system?
 Components of the system
 Components of the surroundings
 Components that absorb/give off thermal energy
 Law of conservation of energy

FOR YOUR ASSIGNED COAL SAMPLES:

 Thermogram plotted for one sample and attached to laboratory notebook
 Average initial and final temperatures determined
 Heat absorbed calculated for each component of the system in notebook
 Heat emitted calculated for each component of the system in notebook
 Heat of combustion calculated for each coal sample in notebook
 Heat of combustion calculated in kJ/g and BTU/lb in notebook
 All calculations include formulas, used correct units & proper significant figures, all work
shown, use of tables whenever possible, used complete sentences

FOR THE CLASS DATASET:

 Formula feature in Excel used in all calculations, correct units & proper significant figures
displayed on spreadsheet
 Where possible calculated the average and the standard deviation of heats of combustion
 Spreadsheet saved electronically for evaluation
Discussion (15 points):
 Answered the question - which coal sample is most effective in heating a home
 Used qualitative and quantitative data to support conclusions
 Results are described and discussed (are the results consistent with your expectations? if
not why?), errors are identified and sources of error discussed
Overall (5 points) - Notes taken during lab lecture, report is organized, neat & easy to read,
citations used where needed
Negative Points
Late to lab (-10 points)
Late lab report (-10 points)
Disruptive behavior in lab (-15 points)
Loose pages in notebook (-5 points)
Total Points Earned (out of possible 100)

Comments:

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