Experiment 9: Freezing Point Depression Safety Hazards

BC Chemistry 162 Laboratory Manual
Experiment 9: Freezing point depression

Safety hazards
Acetic acid causes severe eye and skin burns. It also causes Safety Hazards
severe digestive and respiratory tract burns. Keep goggles on
at all times. You may want to use gloves as well.
Some properties of solutions do not depend on the nature of the solute: they
only depend on the number of solute particles (ions or molecules) relative to Background
the number of solvent particles. We call these properties colligative
properties. In this experiment we will focus on one particular colligative
property, the freezing point depression.
It has been observed that the freezing point of a solution of a non-volatile

solute mixed with a solvent is lower than the freezing point of the pure
solvent. Quantitatively, for a non-volatile solute that is also not an
electrolyte, the lowering of the freezing point is described by the following
equation:
| ΔTf | = Kf x m
where | ΔTf | represents the lowering of the freezing point (Tf), m stands for
the molality of the solution (moles solute per kg solvent) and Kf is the molal
freezing point depression constant that depends only on the identity of the
solvent. When the solute is an electrolyte it is necessary to include the van’t
Hoff factor, i, in the equation (more about this later!).
Figure 1 represents a typical cooling curve of a pure substance (a solvent

without a solute added). It illustrates a very common phenomenon called Cooling curve
supercooling where the temperature of the solvent gets lower than its (pure substance)
actual freezing point. This can be avoided by careful stirring of the liquid.
Figure 1: Cooling curve for a pure substance
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Figure 2 illustrates a standard cooling curve for a solution. Besides the

phenomenon of supercooling, one notices that the freezing temperature
changes with time (see the slope of the line CB). A solution does not have a
sharply defined freezing point. This is because as the solvent freezes, solvent
molecules are removed from the liquid and deposited on the solid, changing
the concentration of solute in the liquid (the molality, m), which lowers the
freezing point even further. In general the freezing point is experimentally
determined by interpolation of the line AB to obtain the point C prior to
supercooling; this is the temperature at which the first crystals of solvent
would appear, if there was not any supercooling.
Cooling curve
(solution)
Figure 2: Cooling curve of a solution
For an electrolyte solution the change in the freezing temperature can be

expressed as
where i is the van’t Hoff factor and represents the number of ions that
would be produced after complete dissociation of the electrolyte in a very
dilute solution (ideal conditions).
In the following experiment, we will explore the freezing point depression of

solutions. In Part 1, we will obtain the cooling curve of a pure solvent, acetic
acid (HAc) and the equivalent curve after an unknown solute has been
added to the solvent. From the measurements of | ΔTf |, we will be able to
determine molality of the solution and consequently the molecular mass of
the unknown. In Part 2, we will calculate the van’t Hoff factor, i, for the
electrolyte CaCl2 by measuring | ΔTf |for two solutions with different values
of molality.
| ΔTf | = Kf x m x i
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Part 1. Freezing point depression of acetic acid
Procedure
Prepare the computer for data collection by opening experiment 15 in
LoggerPro from the folder Chemistry with Computers. The vertical axis of
the graph has a temperature scale from 0°C to 100°C. The horizontal axis has
time scaled form 0 to 10 minutes.
A. Freezing point determination of pure acetic acid (HAc)

1. Fill 2/3 of a 400 mL beaker with ice.
2. In the hood, using a 10 mL pipet, add 30 mL of HAc to a large test tube
and stopper it with a 2 hole stopper. Keep the stoppered tube in an upright
position at all times to avoid spilling any acetic acid.
3. Insert the temperature probe through the large hole of the stopper.
4. Insert the stirrer through the thin hole of the stopper. The paddle-like end
of the stirrer goes into the test tube to stir the sample.
5. Place the tube in the ice bath so that the level of the liquid in the test tube
is below the level of the ice and start collecting the data.
6. While the data is being collected stir the sample gently (you don’t want
to break the test tube!) with an up and down motion to avoid supercooling.
7. You can stop stirring once the sample starts freezing. (Think about it: how
would you know when that happens?)
8. Collect data for 8-10 minutes.
9. Determine the freezing point of HAc using the computer graph. Enlarge
the y-axis (cursor on y-axis; click on ~ symbol and drag) to better determine
the freezing temperature.
10. Remove the temperature probe.
11. Melt the HAc under the tap’s warm water. Do not remove the stopper!
You will add the unknown solute to this same HAc sample.
12. Optional: Repeat the experiment without stirring to observe the
supercooling of HAc.
B. Freezing point determination of a solution of HAc and an unknown

solute.
1. Add 1.5 mL of the unknown solute to the test tube containing the HAc
sample that you used determined the freezing point of pure HAc in
experiment A. Stir well. We will call this solution “solution #1”.
2. Insert the temperature probe.
3. Repeat steps 4-8.
4. Determine the freezing point of the solution using the computer graph. As
explained in the background section you will need to interpolate to
accurately determine the freezing temperature.
6. Melt the frozen solution under the tap’s warm water. Do not remove the
stopper! You will add more unknown solute to this same solution.
7. Add 1.5 more mL of the unknown to the same test tube. We will call this
solution “solution #2”.
8. Repeat steps 3-8 from experiment A.
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9. Determine the freezing point of the solution using the computer graph.
Again, as explained in the background section, you will need to interpolate to
accurately determine the freezing temperature.
11. Melt the frozen solution under the tap’s warm water.
12. Dispose of the sample in the provided chemical waste container. Do NOT
dispose of this sample anywhere else.
Data for Part 1

Prepare a data table to record the freezing points and composition (measured
volumes of solvent and/or solute) of each of three samples for which freezing points
were measured (pure acetic acid, solution #1, and solution #2).
Calculations for Part 1

The density of acetic acid is 1.049 g/mL and Kf (acetic acid) = 3.90 °C· kg/mol
The density of the unknown is 0.791 g/mL.
1. Calculate the masses of the solvent and/or solute present in each of the three
samples.
2. Calculate the freezing point depression (|ΔTf|) for the two solutions.
3. Calculate the experimental value of the molality (moles of solute per kg solvent)
of the two solutions based on the |ΔTf| for the two solutions.
4. Calculate the experimental value for the moles of solute present in each solution.
5. Calculate the molar mass (grams per mole) of the unknown solute.
6. Calculate the average molar mass of the unknown solute based on the values
obtained from the two solutions.
Part 2. Determination of the van’t Hoff factor, i, for CaCl2
Procedure
In this experiment you will use two different solutions of CaCl2 to determine
the van’t Hoff factor, i, using the known Kf value for water, 1.86 °C ·kg/mol.
a. Using a 10mL pipet, add 30 mL of 0.5 m CaCl2 solution to a large test tube
and stopper with a 2 hole stopper.
b. Insert the temperature probe through the large hole of the stopper.
c. Insert the metal stirrer through the thin hole of the stopper.
d. Place the tube in the rock-salt ice bath and start collecting the data.
e. While the data is being collected stir the sample gently with an up and
down motion to avoid supercooling.
f. You can stop stirring once the sample starts freezing.
g. Collect data for 8-10 minutes.
h. Determine the freezing point of the solution using the computer graph.
Enlarge the y-axis (cursor on y-axis; click on ~ symbol and drag) to better
determine the freezing temperature. As explained in the background section
Page 4 of 9
you will need to interpolate to accurately determine the freezing

temperature.
i. Remove the temperature probe.
j. Melt the sample under the tap’s warm water and dispose of it as indicated
by your instructor,
k. Repeat steps a-j with the 1 m solution.
Data for Part 2

Set up a data table to record the molality of each solution (read the concentration on
the bottle!) and the corresponding measured freezing point.
Calculations for Part 2

The Kf value for water is 1.86 °C ·kg/mol.
1. Calculate the freezing point depression, |ΔTf|, for each solution.

2. Calculate the value of the van’t Hoff factor, i, for each solution.
3. Calculate an average value for i based on the two values for i.
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BC Chemistry 162 Laboratory Manual Name ___________________________________ Section _____
Report Sheets
Part 1
Record the following information to demonstrate your successful completion
of the experimental objectives for Part 1.
Volume of acetic acid
Volume of unknown solute in solution #1
Volume of unknown solute in solution #2
Freezing point of pure acetic acid
Freezing point of solution #1
Freezing point of solution #2
Average molar mass of the unknown solute
Part 2
Record the following information to demonstrate your successful completion
of the experimental objectives for Part 2.
Freezing point of ~0.5 m CaCl2 solution
Freezing point of ~1 m CaCl2 solution
Average value of van’t Hoff factor
Follow-up questions
1. Why is molality used instead of molarity in the context of colligative properties?
Page 7 of 9
2. Assume that in the acetic acid experiment you obtained the following values:
Tf (acetic acid) = 16.1°C Tf (with 3 mL of unknown) = 11.3°C
a. Calculate the molar mass of the unknown. Show your work.
b. Your instructor shows you that you made a mistake in the interpolation and that the correct
value is Tf (with 3 mL of unknown) = 11.0 °C. Calculate the new molar mass of the unknown and
compare this value with the molar mass determined based on Tf = 11.3 °C.
2. What do you think are the major sources of error in the determination of the molar mass of the
unknown?
3. What is the theoretical value of the van’t Hoff factor, i, for CaCl2? How does your experimental
value compare to the theoretical value? What does this suggest is happening at the molecular level
in the solution?
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BC Chemistry 162 Laboratory Manual Name ___________________________________ Section _____
Pre-lab assignment—To be completed BEFORE lab!

1. Define molality of a solution.
2. Calculate the molality of a solution prepared by dissolving 78.0 grams of butanone (C4H8O) in
800 mL of acetic acid. The density of acetic acid is 1.049 g/mL.
3. You dissolve 93.24 g of an unknown solute in 1000 g of water and obtain | ΔTf | = 2.34°C.
a. What is the molality of the solution if Kf is 1.86 °C ·kg/mol for water?
b. How many moles of solute are present in the solution?
c. What is the molar mass of the unknown solute?
Page 9 of 9

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BC Chemistry 162 Laboratory Manual

Experiment 9: Freezing point depression

It has been observed that the freezing point of a solution of a non-volatile

Figure 1 represents a typical cooling curve of a pure substance (a solvent

Figure 1: Cooling curve for a pure substance

Figure 2 illustrates a standard cooling curve for a solution. Besides the

Figure 2: Cooling curve of a solution

For an electrolyte solution the change in the freezing temperature can be

In the following experiment, we will explore the freezing point depression of

Part 1. Freezing point depression of acetic acid

A. Freezing point determination of pure acetic acid (HAc)

B. Freezing point determination of a solution of HAc and an unknown

Data for Part 1

Calculations for Part 1

The density of the unknown is 0.791 g/mL.

Part 2. Determination of the van’t Hoff factor, i, for CaCl2

you will need to interpolate to accurately determine the freezing

Data for Part 2

Calculations for Part 2

1. Calculate the freezing point depression, |ΔTf|, for each solution.

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Volume of acetic acid

Volume of unknown solute in solution #1

Volume of unknown solute in solution #2

Freezing point of pure acetic acid

Freezing point of solution #1

Freezing point of solution #2

Average molar mass of the unknown solute

Freezing point of ~0.5 m CaCl2 solution

Freezing point of ~1 m CaCl2 solution

Average value of van’t Hoff factor

a. Calculate the molar mass of the unknown. Show your work.

Pre-lab assignment—To be completed BEFORE lab!

b. How many moles of solute are present in the solution?

c. What is the molar mass of the unknown solute?

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