LABORATORY REPORT

CHM476

(PHYSICAL CHEMISTRY)
NAME & STUDENT NO : NUR INSYIRAH SHAZRIN BINTI ABIDIN (2020960861)

PROGRAMME : AS222

GROUP : AS2221A1

EXPERIMENT : PHASE EQUILIBRIUM (FREEZING POINT DEPRESSION AND MOLAR MASS

DETERMINATION)

DATE OF EXPERIMENT : 30 APRIL 2020

DATE OF REPORT SUBMISSION : 4 JUNE 2020

NAME OF LECTURER : DR NORLIZA BINTI DZAKARIA

EXPERIMENT 5

TITLE: PHASE EQUILIBRIUM (FREEZING POINT DEPRESSION AND MOLAR

MASS DETERMINATION)

OBJECTIVES:

1. To determine freezing point depression of a solution and molar freezing point

constant of the solvent.
2. To obtain the molar mass of a solute.

INTRODUCTION

Colligative properties are the properties of a liquid that change when a solute is added.
Colligative properties include vapour pressure lowering, boiling point elevation, freezing
point depression and osmotic pressure (Colligative properties). One of these properties can be
used to obtain molecular weight of the solute.

A small amount of non-volatile solute is dissolved in a volatile solvent. The vapour pressure
of the solvent over the solution will be less than the vapour pressure of the pure solvent at the
same temperature. Therefore, the temperature at which the equilibrium vapour pressure
reaches atmospheric pressure is higher for the solution than for the pure solvent. As a result,
the boiling point of the solution, Tb, is higher than the boiling point of the pure solvent, Tbo.
The amount by which the boiling point of the solution exceeds the boiling point of the pure
liquid, ΔTb = Tb−Tbo, is called the boiling point elevation. Similarly, because of the reduction
in vapor pressure over the solution the freezing point of the solution, Tf, is lower than the
freezing point of the pure solvent, Tfo. The amount by which the freezing point of the solution
is decreased from that of the pure liquid, ΔTf=Tfo−Tf is called the freezing point depression.
Figure 1 below illustrates this behaviour for water (College, 2019).

Figure 1 (source: https://chem.libretexts.org/)

The changes in the freezing point, ∆Tb and the boiling point, ∆T are directly proportional to
molality, m, of the solute in solution. The proportionally is a constant, characteristic of the
actual solvent.

The equation describing the freezing point depression is

∆Tf = Kf m = │Tf solvent – Tf solution│ (1)

Where T, represents the freezing point and │Tf solvent – Tf solution│ represents the absolute
temperature difference in the freezing point change.

For boiling elevation, the equation is described as

∆Tb = Kb m = │Tb solvent – Tb solution│ (2)

And Tb represents the boiling point of the respective system.

Molality is defined as:

Molality, m = (3)

In this experiment, the freezing point of a pure solvent (naphthalene), a solution of a known
solute (1,4-dichlorobenzene, C6H4Cl2) dissolved in naphthalene, and an unknown solution of
p-nitrotoluene in naphthalene. The p-nitrotoluene is considered as an unknown solute because
the molar mass of p-nitrotoluene needs to be determined. Equations 1 and 3 are used to
calculate the freezing point lowering (difference), ∆Tf and Kf for the solvent, the moles of
solute dissolved in solution and from its measured mass, the molar mass of the solute.

The freezing points of the solvent and the solution are obtained from a cooling curve – a plot
of temperature versus time.
APPARATUS

1. Boiling tubes
2. Thermometer
3. Conical flask
4. Stopwatch
5. Weighing boat
6. Water bath
7. Analytical balance
8. Retort stand and clamp

MATERIALS

1. Naphthalene, C10H8
2. 1,4-dichlorobenzene, C6H4Cl2
3. p-nitrotoluene, C7H7NO2

PROCEDURE

A. Determination of freezing point of naphthalene

1. 5g of naphthalene was weighed to the nearest 0.01g and was added to a clean and
dry boiling tube.
2. The naphthalene was melted completely in the hot water bath. The rubber stopper
containing thermometer and copper wire was inserted into the boiling tube.
3. The tube was taken out from the water bath once the temperature of naphthalene
had reached 95°C.
4. A clamp was used to set the tube vertically in the conical flask. Once the
temperature of naphthalene had dropped to 90°C, the temperature was recorded
every 30 seconds to the nearest 0.1°C.
5. The temperature of naphthalene was recorded until the temperature had dropped
to about 60°C.
6. The frozen naphthalene was kept for Part B.
 B. Determination of K1 for naphthalene
1. 0.5g of 1,4-dichlorobenzene was weighed to the nearest 0.01g and was added to
the boiling tube containing the naphthalene
2. Steps (2) to steps (5) in Part A were repeated.
3. Once the mixture had solidified, the mixture was melted in the hot water bath and
the solution was discarded in the waste container.

C. Determination of freezing point of p-nitrotoluene

1. 5g of naphthalene was weighed to the nearest 0.01g and was added to a clean and
dry boiling tube.
2. 1g of p-nitrotoluene was weighed to the nearest 0.01g and was added to
naphthalene in the tube.
3. Steps (2) to (5) in Part A were repeated.
4. Once the mixture had solidified, melted it the hot water bath and the solution was
discarded in the waste container.

RESULT

A. Determination of Freezing Point of Naphthalene

1. Mass of naphthalene (g): 5.0169
2. Freezing point of naphthalene from cooling curve (°C): 80.0

B. Determination of Kf of Naphthalene
1. Mass of 1,4-dichlorobenzene (g): 0.5157
2. Freezing point of solution from cooling curve (°C): 75.0

C. Determination of Freezing Point p-nitrotoluene solution

1. Mass of naphthalene (g): 5.0393
2. Mass of p-nitrotoluene (g): 1.0136
3. Freezing point of solution from cooling curve (°C): 68.0
 Naphthalene Naphthalene + 1,4- Naphthalene + p-nitrotoluene
dichlorobenzene
Initial 90 Initial 85 Initial 85
temperature temperature temperature
(°C) (°C) (°C)
Time (sec) Temp (°C) Time (sec) Temp (°C) Time (sec) Temp (°C)

30 84.0 30 80.0 30 76.0

60 82.0 60 79.0 60 70.0

90 80.5 90 78.5 90 69.0

120 80.5 120 76.0 120 68.5

150 80.0 150 75.5 150 68.0

180 80.0 180 75.0 180 68.0

210 80.0 210 75.0 210 68.0

240 80.0 240 75.0 240 68.0

270 79.5 270 74.5 270 67.0

300 78.5 300 74.0 300 64.0

330 78.0 330 73.0 330 63.5

360 73.0 360 68.0 360 63.5

390 68.0 390 66.0 390 63.0

420 65.5 420 64.0 420 62.5

450 62.5 450 63.0 450 62.5

480 61.5 480 62.5 480 61.0

510 60.0 510 60.0 510 60.0

(a) Graph of temperature of naphthalene against time in minutes
(b) Graph of temperature of naphthalene – 1,4-dichlorobenzene against time in minutes
(c) Graph of temperature of naphthalene – p-nitrotoluene against time in minutes
DISCUSSION

In this experiment, there are three part, Part A, Part B and Part C were conducted to
determine the freezing point of naphthalene, Kf of naphthalene and freezing point of p-
nitrotoluene respectively.

Firstly, in Part A, 5.0169g of solid naphthalene was melted inside the boiling tube
using hot water bath. After the temperature of melted naphthalene reached 95.0°C, the tube
was taken out from the water bath and started to record the temperature at every 30 seconds
when the temperature has dropped to 90.0°C, which was recorded as initial temperature. The
temperature reading was stopped recording as the temperature has reached 60.0°C. At this
temperature range, the naphthalene has frozen. The temperature reading that has been
recorded was tabulated in form of a cooling curve graph. The cooling curve graph of pure
naphthalene was constructed where the temperature of naphthalene against the time in
minutes.

In Part B, 0.5157g of 1,4-dichlorobenzene which known as solute was added into the
frozen naphthalene which was from Part A. The freezing point of solution from cooling curve
was 80.0°C. This step was used to determine the freezing point depression constant, Kf of
naphthalene. The calculation is as shown below;

∆Tf = │T°f - T°f│

∆Tf = │80.0 – 75.0│ = 5.0°C

Mol C6H4Cl2 = 0.5157g / 147.00gmol-1 = 3.51 x 10-3mol = 0.00351 mol

Molality, m =

Molality, m = = 0.6996 mol/kg

∆Tf = (Kf) (m)

(5.0°C) = Kf (0.6996 mol/kg)

Kf = 7.15°Ckg/mol
 In Part C, the mass of naphthalene used was 5.0393g and the mass of p-nitrotoluene
used was 1.0136g. The freezing point depression of naphthalene – p-nitrotoluene was used to
determine the molar mass of p-nitrotoluene. The calculation is shown below:-

∆Tf = │T°f - T°f│

∆Tf = │80.0 – 68.0│ = 12.0°C

∆Tf = (Kf) (m)

(12.0°C) = (7.15°Ckg/mol) (m)

Molality, m = 1.68mol/kg

Molality, m =

⁄
1.68mol/kg =

Molar mass = 119.67g/mol

The actual value of freezing point depression constant of pure naphthalene is

6.94°Ckg/mol and the experimental value obtained was 7.15°Ckg/mol. Thus, the percentage
error was calculated was 3.023%.

% error =

% error =

= 3.023%

The molar mass of p-nitrotoluene obtained from this experiment was 119.67 g/mol
meanwhile the actual value of molar mass of p-nitrotoluene was 137.14 g/mol. Thus, the
percentage error obtained was

% error =

% error =

= 12.74%
 According to the percentage error calculated, there are some factors that led to obtain
a different value. Firstly, the source of error might be due to human error while conducting
the experiment. The eyes were not perpendicular to the scale of thermometer caused the
misread the temperature. Other than that, the weighing scale might show limitation that
caused the measurement of naphthalene, 1,4-dichlorobenzene and p-nitrotoluene not accurate.
These errors caused in obtaining almost similar or completely different value than the actual
value.

QUESTIONS

1. Supercooling happens when a solution momentarily drops below its freezing point,
and then warms up again before solidification. What event is likely to give rise to
supercooling?
Water presence in cloud in high altitude has low temperature than its freezing point
but the water droplets do not crystallize.

2. A 0.5g sample of a non-volatile solute dissolves in 10.0g of acetic acid. The freezing
point of the solution is 15.9°C. (K1 of acetic acid is 3.9°Ckgmol-1 and freezing point is
17°C)
a) What is the molality of the solute in the solution?
∆Tf = Kf m
17°C = 3.9°Ckgmol-1 (m)

m=

m = 4.36 kg/mol-1

b) Calculate the molar mass of the solute.

Molality, m =

⁄
4.36 kg/mol =

= (4.36 kg/mol) (0.01 kg)

Molar mass =

Molar mass of the solute = 11.47 g/mol

 c) The same mass of solute is dissolved in 10g of t-butanol instead of acetic acid.
What is the expected freezing point change of the solution?
(K1 of t-butanol is 9.1°C kgmol-1 and freezing point is 25.5°C)

Molality = = 4.36 mol/kg

∆Tf = Kf m
= (9.1°C kgmol-1) (4.36mol/kg)
= 39.7°C
40.0°C

CONCLUSION

In this experiment, the freezing point depression of naphthalene – p-nitrotoluene solution

obtained was 12.0°C. The freezing point of the solution obtained from the cooling curve
graph was 68.0°C. By obtaining the freezing point depression, the molar mass of p-
nitrotoluene can be determined by using this formula, ∆Tf = (Kf) (m). The freezing point
depression constant, Kf has been determined by using the freezing point depression of
naphthalene – dichlorobenzene. The Kf calculated was 7.15°Ckg/mol. Therefore, the molar
mass of p-nitrotoluene obtained was 119.67g/mol.

REFERENCES

College, S.M. (2019, June 6). Determination of the molar mass by freezing point depression
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hem_12_Experiments/10%3A_Determination_of_the_Molar_Mass_by_Freezing_Poi
nt_Depression_(Experiment)

Census data revisited. (n.d). Colligative properties. Retrieved May 7, 2020 from
https://www.chem.fsu.edu/chemlab/chm1046course/colligative.html

Shaharudin, M.D. & Kantasamy, N. (2019). Introduction to physical chemistry (pp. 37-42).
UiTM Printing Centre, Shah Alam.

Judge, M. (2018, April 27). Reason for error in a chemistry experiment. Retrieved May
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experiment-8641378.html