CALORIMETRY (MICROSCALE)

(Temperature Change and Heats of Reaction)

I. Objectives
In this experiment you will determine the specific heat of a metal, the heat change and
acid/base stoichiometry which accompanies an acid-base neutralization using the Job's
method.
II. Introduction
Heat is a form of energy. Objects can emit or absorb heat: Red-hot charcoal emits heat
in the form of radiant energy; an ice pack absorbs heat when it is placed on a swollen
ankle. The emission or absorption of heat causes an object to change its temperature.
Experimentally, we can calculate the heat flow associated with a chemical reaction by
measuring the temperature change it produces. Calorimetry is a very simple technique
used to measure changes in temperature. At constant pressure the heat of reaction is the
enthalpy of reaction. An apparatus used to measure heat flow is a calorimeter. Ideally,
a calorimeter should not absorb any heat from the chemical reaction taking place in it and
should not transfer it to the surroundings. In reality, even the best calorimeter absorbs a
little bit of heat. Thus, the heat capacity of the calorimeter (or calorimeter constant) must
be determined.
Heat capacity: This is the amount of heat (q) required to increase the temperature of a
substance by 1 K (or C).
Molar heat capacity: This is the heat capacity of 1 mole of substance or just the amount
of heat (q) required to increase the temperature of 1 mole of substance by 1 K (or C).
Specific heat (S.H.) capacity or specific heat: This is the amount of heat (q) required to
increase the temperature of I g of substance by 1 K (or C) or just the heat capacity of 1
g of a substance. The specific heat of a substance can be determine experimentally by
measuring the temperature change, T, that a known mass, m, of the substance undergoes
when it gains or loses a specific quantity of heat.
q

(quantity of heat transfer)

Specific heat =

=
(grams of substance) x (temperature change)

mx

The quantity of heat gained or lost when a sample of any substance undergoes a
temperature change at constant pressure is given by
H = (S.H.)(m)(T)
where H is the heat gained or lost in joules, n is the mass in grams, S.H. is the specific
heat and T is the difference between the final and initial temperature of the sample. For
example, the S.H. of gold is 0.128 J/g C and the quantity of heat released when the
temperature of 1.50 x 102 g of gold changes from 73.8C to 54.6C is given by
H = (0.128 J/g C)(1.50 x 102 g)(54.6C - 73.8C) = - 3.69 x 102 J

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If a metal does not react with water, its specific heat can be determined by immersing a
weighed sample of the metal at a known temperature in a known volume of water at
another known temperature, and measuring the resultant final temperature of the metal
and water. The heat gained or lost by the metal is equal to the heat gained or lost by
water.
Heat gained (or lost) by the water = Heat gained (or lost)by the metal.
III. Experimental Procedure:
(USE THE SAME NUMBERED CALORIMETER ASSEMBLY FOR PARTS A,
B, C, D, AND E)
Part A Preparation of a Calorimeter Assembly (Figure 1)
1. Obtain a 2 x 2 x 4 in. Styrofoam block (this is your calorimeter) and a 13x100 mm
test tube (small test tube). Record the number. You will use the same calorimeter in
parts A, B, C, and D.
2. Loosely insert a rubber ring/stopper, fitted with a thermometer, in the test tube.
3. The ring-thermometer assembly (Figure 1) should be briefly removed when adding
chemicals to the tube and then quickly replaced.

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Thermometer

Ring
Stand

One-hole
Ruber Stopper

Clamp

Test Tube

Styrofoam Block

FIGURE 1
4. When the calorimeter is heated during each run, it cools slowly. To avoid the
accumulation of heat ("memory"), bring the calorimeter back to room temperature by
inserting a test tube containing tap water at room temperature in the calorimeter for 5
minutes after each run to dissipate the heat.
Part B Calibration of the Calorimeter
* YOU WILL USE PIPETS AND PIPET FILLERS/BULBS TO FILL THE
PIPETS. FILL THE PIPETS SLOWLY TO AVOID CONTAMINAING THE
PIPET FILLERS.
** AFTER YOU ARE DONE USING THE PIPETS, RINSE THEM TWICE
WITH DI WATER.
1. Pipet 2.00 mL ( 0.01 mL) of room-temperature water (tap water) into a 13 x 100
mm test tube and place it in the calorimeter. Insert the thermometer and record the
temperature ( 0.1 C) at 30-second intervals for 5 minutes.

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2. Obtain 400-500 mL of 45-50 C tap water in a 600 mL beaker. Pipet 2.00 mL of this
hot water into a second test tube and place it in the hot-water bath for several minutes.
Record the temperature of the hot water.
3. Tilt the calorimeter slightly and quickly pour the hot water from the test tube into the
room-temperature water. Swirl the mixture and record the time of addition.
4. Insert the room-temperature thermometer immediately. Continue to record time and
temperature data for another 5 minutes.
5. Discard the contents, bring the calorimeter back to room temperature (Part A, step
4), Repeat Part B, steps 1 4.
Part C Heat of Dissolution of Mg(s) with HCl(aq)
Mg(s) + 2HCl(aq) MgCl2 (aq) + H2(g)
1. Pipet 2.00 mL of 1.00 M HCl into the test tube and place it in the calorimeter. Insert
the thermometer and record the initial temperature at 30-second intervals for 5 minutes.
2. Weigh 8 - 10 mg ( 1 mg) of Mg, on a tarred weighing paper.
3. Using a long stem funnel add the Mg to the HCl solution in the calorimeter. Make
sure the bottom of the funnel stem doesn't touch the HCl solution. Swirl cover and
note the time of addition.
4. Measure and record the temperature at 30-second interval for 5 minutes.
5. Discard the contents in your waste beaker, bring the calorimeter back to room
temperature (Part A, step 4), Repeat Part C, steps 1 4.
Part D Specific Heat of a Metal (OPTIONAL)
1. Pipet 2.00 mL of room temperature deionized water into the test tube and place it in
the calorimeter. Insert the thermometer and record the initial temperature a 30-second
interval for 5 minutes.
2. Using an analytical balance ( 0.0001 g), weigh a weighing paper and record.
3. Place a sample of your assigned unknown metal on it, reweigh and record (You can
tare the weighing paper if you like).
4. Immerse the metal in a beaker of boiling water. Wait about 1 minute, the temperature
of the metal will become the same as the temperature of the water. Measure the
temperature of the water.

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5. Hold the tip of a pair of crucible tongs in the boiling water for about 1 minute. Lift the
metal from the boiling water and quickly transfer it to the water in the calorimeter.
Measure and record the temperature at 30-second interval for 5 minutes.
6. Rinse the metal with d.i. water. Bring the calorimeter back to room temperature.
Repeat Part C.
7. Return the metal to its original container.

SECOND PERIOD
Part E Job's Law Neutralization of HCl with NaOH
HCl(aq) + NaOH(aq) NaCl(aq) + H2O(l)
=================================================================
TABLE 1
__________________________________________________________________________
Run Number
1
2
3
4
5
__________________________________________________________________________
Volume of HCl, mL
0.50 1.00 2.00 3.00 3.50
Volume of NaOH, mL

3.50

3.00

2.00

1.00

0.50

* The total volume is the same (4.00 mL) in each run.

=================================================================
1. In Run # 1, pipet 0.50 mL of 1.00 M HCl into the test tube and place it in the
calorimeter. Insert the thermometer and record the initial temperature at 30-second
intervals for 5 minutes.
2. Pipet 3.50 mL of 1.00 M NaOH into a 10 mL beaker and pour it all at once into the
HCl test tube. Immediately inert the thermometer. Swirl, note the time of addition,
and
observe and record the temperature at 30-second intervals for 5 minutes.
3. Collect the solution in waste flask. Bring the calorimeter back to room temperature
(Part A, step 4).
4. Repeat the procedure for runs 2, 3, 4, and 5 using the quantities shown in Table 1.
5. Clean up and return the equipment.

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IV. Data Treatment

Graphs: Plot the data (FIGURE 2) of Parts B, C, and D on 3 separate graph papers (use
EXCEL), using the temperature as the vertical axis. On each graph, draw a vertical line at
the time of addition, and extend the nearly straight portion of the curve to intersect this line.
Determine Tf (shown in the graph), the hottest "final" temperature that would have been
observed had an instantaneous reaction taken place. The quantity T is the difference
between Tf and Ti.

Tf

Draw this Line

T
Cooling off
TEMP
Ti

Time of Addition
TIME
FIGURE 2

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A graph (FIGURE 3) is then made of T (y axis) versus volume of acid and base added (x
axis). The maximum T of the Job's Plot corresponds to the reaction stoichiometry of HCl
and NaOH.

0.0

1.0

2.0
Volume of Acid Added, mL

3.0

4.0

4.0

3.0

2.0

1.0

0.0

Volume of Base Added, mL

FIGURE 3

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V. Calculations
For all runs, determine T for each reaction. For water the specific heat is 4.184 J/g C
and the density is 1.00 g/mL. For the solutions used in this experiment it is assume that
the specific heat is 4.184 J/g C and the density is 1.00 g/mL. This is a reasonable
assumption.
Part B: Heat Capacity (J/C) of the calorimeter
Tf is determined from the T(C) vs. time (seconds) graph
Th is the temperature of hot water and Ti is the initial temperature of the calorimeter
and cold water.
a. Heat lost by the hot water = (M hot water)(4.184 J/g C)(Tf Th)
* Grams of cold water = (1.00 g/mL)(mL of cold water)
b. Heat gained by cold water = (M cold water)(4.184 J/g C)(Tf Ti)
* Grams of hot water = (1.00 g/mL)(mL of hot water)
c. Heat gained by the calorimeter = X(Tf Ti)
X = heat capacity of the calorimeter (the amount of heat needed to change the
temperature of the calorimeter by 1.00 C or 1.00 K.)
According to the First Law of Thermodynamics, heat lost = heat gained, then;
Heat lost by the hot water = (Heat gained by cold water + Heat gained by the
calorimeter) so,
(M hot water)(4.184 J/g C)(Tf Th) = [(M cold water)(4.184 J/g C)(Tf Ti) +
X(Tf Ti)]
Part C: Heat of Dissolution of Mg(s) with HCl(aq)
Mg(s) + 2HCl(aq) MgCl2 (aq) + H2(g)
Using X from Part B, and Tf from each graph.
a. Heat gained by the calorimeter = X(Tf Ti)
b. Heat gained by the HCl solution = (g HCl solution) )(4.184 J/g C)(Tf Ti)
* Grams of HCl solution = (1.00 g/mL)(mL of HCl solution)
* Since the amount of Mg is very small, its mass can be ignore.
c. Heat of reaction produced by the reaction of Mg with HCl (aq) is
Y = (a + b). Since this reaction is exothermic the sign is negative.
Calculate the Heat of reaction of Mg with HCl (aq).
d. Calculate the Heat of reaction of 1 mole Mg with HCl (aq), H/mole Mg.

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Part D: Specific Heat of a Metal (OPTIONAL)

a. Heat gained by the calorimeter = X(Tf Ti)
b. Heat gained by cold water = (g cold water)(4.184 J/g C)(Tf Ti)
c. Heat lost by the metal = (g metal)(S.H metal)(Thot metal Tf)
Since heat lost = heat gained, a + b = c
d. Calculate the specific heat of the metal
Part E: Molar Heat of Neutralization of HCl with NaOH
HCl(aq) + NaOH(aq) NaCl(aq) + H2O(l)
The maximum temperature change will occur when the reactants are in the stoichiometric
ratio. Use the point of intersection of the two lines (Job's Plot) to find the maximum T
and its corresponding stoichiometric ratio. Use this T to calculate the H of this
neutralization. Since the concentrations and volumes of the acid and base are known, the
number of moles of each can be calculated and the stoichiometric ratio can be determined.
a. Heat gained by the calorimeter solution = (g HCl + g NaOH)(4.184 J/gC)( Tf Ti)
* Grams of HCl solution = (1.00 g/mL)(mL of HCl solution)
* Grams of NaOH solution = (1.00 g/mL)(mL of NaOH solution)
b. Heat gained by the calorimeter = X(Tf Ti))
c. Total # joules produced by the neutralization = (heat gained by the calorimeter
solution + heat gained by the calorimeter)
d. Calculate the molar heat of neutralization (H/mol HCl)

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VI. Lab Report

*In this lab report you will submit a total of 9 graphs of Temperature (C) vs. time
(seconds) and a graph of T (C) vs. either volume of HCl or NaOH (Jobs' Plot)

Name _________________________________

Part B: Heat Capacity of the Calorimeter (SHOW ALL YOUR CALCULATIONS)

Make a graph of temperature vs. time for each of your two runs.
Determine the minimum Ti and maximum Tf from the graph and calculate T.
Calculations

First Run

Second Run

Ti (Initial temperature
of water in calorimeter)

_____________

_______________

Th (Initial temperature
of hot water)

_____________

_______________

Tf (Final temperature
from graph)

_____________

_______________

Tf Th (T)

_____________

_______________

Tf Ti (T)

_____________

_______________

Heat released from hot water

_____________

Heat absorbed by cold water _____________

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_______________

_______________

Heat Capacity of
Calorimeter, X

Average Heat Capacity

_____________

_______________

________________

Sample calculation of X:

Part C: Heat of Dissolution (reaction) of Mg in HCl(aq)

(SHOW ALL YOUR CALCULATIONS)
Make a graph of temperature vs. time for each of your two runs.
Determine the maximum Tf. from the graph and calculate T.
Calculations
Ti (Initial temperature
of HCl(aq) in calorimeter)

First Run

Second Run

_____________

_______________

Tf (Final temperature
from graph)

_____________

_______________

Tf Ti (T)

_____________

_______________

Heat absorbed by
the solution

_____________

_______________

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Heat absorbed by the

Calorimeter

_____________

_______________

Heat of reaction of
Mg with HCl(aq)

_____________

_______________

Average heat of reaction of Mg with HCl(aq)

________________

Average heat of reaction per mole of Mg (H/molMg)

________________

Part D: Specific Heat of an unknown metal (SHOW ALL YOUR CALCULATIONS)

Make a graph of temperature vs. time for each of your two runs.
Determine the maximum Tf. from the graph and calculate T.
Unknown Number_______
First Run

Second Run

Mass of paper with metal

_____________

_______________

Mass of paper

_____________

_______________

Mass of metal

_____________

_______________

Tf (Final temperature
from graph)

_____________

_______________

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Tf Ti (T)

_____________

_______________

Volume of water

_____________

_______________

Calculated Specific Heat

_____________

_______________

Average Specific Heat

__________________

Sample calculation of Specific Heat:

Part E: Molar Heat of Neutralization (SHOW ALL YOUR CALCULATIONS)

1. Make a graph of temperature vs. time for each of your five runs. Determine the
maximum Tf. from the graph and calculate T for each run.
2. Make a graph of T vs. volume of HCl or NaOH used.
3. Use the maximum value of T (from Jobs Plot) to calculate the H of neutralization of
this reaction.
4. Determine the mole stoichiometry from the maximum T of the Job's Plot using the
corresponding volumes of the HCl(aq) and NaOH(aq) at this maximum T.

First Run
Tf Ti (T)

_____________

Second Run

_______________

Fourth Run
Tf Ti (T)

Third Run

_______________

Fifth Run

_______________

_______________

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Calculate the heat absorbed by

the HCl(aq)/NaOH(aq) solution

Calculate the heat absorbed

by the calorimeter

__________________

____________________

Calculate the heat of neutralization of HCl(aq) with NaOH(aq):

____________________

Calculate the molar (H) heat of neutralization per mole of HCl:

____________________

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Calculate the stoichiometry ratio for the HCl(aq) with NaOH(aq) neutralization reaction
using the volume of HCl at the maximum H:

____________________

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VII. Post Lab Problems:

1. Why is the total volume of HCl and NaOH the same for each run in Part E?

2. Use H formation values from your text book to calculate the H neutralization for the
following reaction:
H2SO4(aq) + 2NaOH(aq) H2O(l) + Na2SO4(s)

3. When 630. mg of a compund are dissolved in 6.00 mL water inside a calorimeter the
temperature increased from 19.0 C to 23.0 C. If the total number of Joules produced by
this reaction was 202 Joules calculate the heat capacity of this calorimeter.
Specific heat capacity of water = 4.184 J/gC
Density of water = 1.00 g/mL

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