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JOURNAL OF

CHEMICALEDUCATION Laboratory Experiment

Cryoscopic Method of Molecular Mass


Determination
John Francis Egenias, Alyssa May Frias, Krizzi Eve Garcia, Arnold John Granda

1 CHEM 1, BS Chemistry, Chemistry Department, College of Science


University of Santo Tomas
España Blvd, Sampaloc, Manila, 1008 Metro Manila

__________________________________________________________________
ABSTRACT: Colligative properties are properties of solutions that depend on the concentration of
solute particles present and not on its nature. These properties are significant to many natural phenomena
and practical applications including antifreeze in cars, making ice cream and desalinating water. The
experiment aims to determine the molecular mass of the assigned solid by measuring the lowering it causes
on the freezing point of the solvent. It utilizes the freezing point depression property of solutions. The
determination of the molecular mass of the solute is done by the cryoscopic method where freezing point of
the solvent, naphthalene, is identified first in order to determine the freezing point depression used in
calculating for the molecular mass. As solute was added to the solvent, the resulting temperature of the
solutions were lower as compared with the pure solvent. The molecular mass was calculated using the
formula for the freezing point depression and was found to be 45.5 g/mol. The computed mass was a lot
lower as compared with the true value. However, it can be concluded that colligative properties can be used
in determining a solid’s molecular mass.
KEYWORDS: Cryoscopic constant, Colligative properties, Molality, Freezing point depression

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INTRODUCTION

Certain important properties of solutions depend on the concentration or quantity of solute


particles in solution while being independent on the nature of the solute. These properties that
characterizes solutions are called colligative properties (Chang & Overby, 2011). The four properties of
solutions are vapor pressure lowering, boiling point elevation, freezing point depression and osmotic
pressure. For an instance, when a particular nonvolatile solute is added to a solvent, the vapor pressure of
the liquid is decreased. The decline in vapor pressure is an example of vapor pressure lowering caused by
the presence of solute. The stability of the solvent in the liquid state tends to lower the tendency of the
particles to escape to the gas phase (Brown, et al., 2018). Many important practical applications of
colligative properties help us in our daily lives especially freezing point depression and osmotic pressure.
The use of antifreeze in the radiator of automobiles demonstrates freezing point depression as well as

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boiling point elevation. During winter, it prevents the liquid in the radiator from freezing whereas during
summer, it prevents the liquid from boiling (Malik, 2017).
Another application of colligative properties is in the determination of a substance’s molecular
mass. The cryoscopic method is an approach utilized to determine a molecular mass of a solute by
dissolving it and measuring the freezing point depression of the solution (Merriam-Webster’s Collegiate
Dictionary, 1999). This method utilizes the cryoscopic constant, which expresses the freezing point
depression by the addition of a solute (Croatian-English Chemistry Dictionary & Glossary, 2018). The
objective of the experiment is to determine the molecular mass of a solid by determining first the freezing
point depression of the solvent, naphthalene. The calculation for the molecular mass is possible with the
formula: ∆ Tf =Kfm where the freezing point depression is related with the cryoscopic constant and
molality. Since molality is the moles of solute per kilogram of solvent, the molar mass of the solid can be
readily calculated.

STUDENT LEARNING GOALS


This laboratory experiment aims the students to determine the molecular mass of the assigned
substance by identifying the lowering effect on the freezing point of the solvent which is naphthalene. The
students must be able 1) to determine the freezing point of naphthalene from its cooling curve 2) to
determine the cryoscopic constant of naphthalene and 3) to determine the molecular mass of the assigned
solid from the lowering it causes on the freezing point of the solvent, naphthalene.

EXPERIMENTAL SECTION
Determination of Freezing Point of Naphthalene
For the determination of the freezing point of the solvent which is naphthalene, a 200 mL of tap
water was placed in a 250 mL beaker and was heated to boiling using a hot plate. Using an analytical
balance, 1.0 g of solid naphthalene was weighed to the nearest 0.1 g using an aluminum foil. The foil will
help avoid errors in transferring the solid into the test tube. The test tube was then left undisturbed in
boiling water until the solid turns into liquid. A thermometer was inserted into the test tube and was
immersed into the melt to measure its corresponding temperature. Then a cotton plug was used to cover
the test tube to prevent the escape of obnoxious odor.

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Figure 1. Melting the solid by immersing the test tube in boiling water
After the solid completely melted, the hot test tube was transferred into an air bath and was allowed to
cool while stirred gently. Stirring will make the particles interact with each other more, so the
measurement of temperature will be of the solution. The melted solid will solidify once again when
cooled thus, the solid’s freezing point will then be determined. The temperature was then recorded from
the thermometer readings for 5 minutes in 10-second intervals.

Determination of the Cryoscopic Constant of Naphthalene


The cryoscopic constant of naphthalene was determined by preparing a mixture of naphthalene
and acetanilide. The cryoscopic constant which will be identified through the solution’s freezing point
depression will be needed to compute for the molecular mass of the solid. A 1.0g of naphthalene and .01 g
of acetanilide was weighed to the nearest 0.01 g and was mixed thoroughly in a test tube. The mixing of
the mixture is essential in order to properly measure the freezing point of the solution and not of the
denser liquid. Afterwards, the procedure for Part A was then repeated. The formula for the cryoscopic
constant is:
T f −T f '
Kf =
m
 Tf - freezing point of naphthalene
 Tf’ – freezing point of solution with acetanilide
 m – molality

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Figure 2. Weighing of the acetanilide solid


Determination of Molecular Mass of Unknown Solid
A mixture of an assigned solid and naphthalene was prepared. A 1.0 g of naphthalene and .01 g of
acetanilide was weighed to the nearest 0.01 g and was mixed thoroughly in a test tube. The procedure for
Part A was also repeated. The freezing point depression caused by the addition of solute was then
measured using the thermometer readings. The formula used for the molecular mass is:
T f −T f ( {kg} rsub {naphthalene} )
K (g ) ;Kf – obtained cryoscopic constant in Part B
molecular mass= f ¿unkown

HAZARDS
Naphthalene and a similar substance, paradichlorobenzene are considered to be carcinogens.
These substances can be harmful to the body when exposed and can cause various effects like irritation,
vision damage, headache, fatigue, confusion, tremor, nausea and vomiting. Both substances are also
combustible solids. The vapor released when heated is flammable, thus poses a dangerous fire hazard. On
the other hand, acetanilide, can be hazardous when inhaled, ingested or in contact with the eyes. Correct
handling with wearing of proper personal protective equipment is essential in managing these substances.
Proper disposal with melted solids must be followed accordingly.

RESULTS AND DISCUSSION


The purpose of this laboratory experiment was to determine the assigned solid’s molecular mass
using the concept of freezing point depression. Since freezing point depression can be related to molality,
moles of a particular substance can be determined. Relationships from colligative properties and the
number of moles can give a substance’s molecular mass.

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(A) (B)
Mass of naphthalene – 1.0003g
Mass of naphthalene – 1.0003g
Mass of acetanilide - 0.1023g
Time (mins) Temperature (
Time (mins) Temperature (
℃¿ ℃¿
0 94.2
0 94.2
1 79.1
1 79.1
2 74.5
2 74.5
3 68.9
3 68.9

(C)
Mass of naphthalene – 1.0072g
Mass of solid - 0.1036g
Time (mins) Temperature (
℃¿
0 87.4
1 72.7
2 68.1
3 64.9

Figure 3. (A) Recorded time and temperature for the cooling of naphthalene, (B) for the
naphthalene-acetanilide solution, (C) for naphthalene-solid solution
The determination of the freezing point of pure naphthalene in the first part of the experiment was
necessary in order to have a basis when temperatures are compared in the latter part of the experiment. It
is essential to determine how much lowering in the temperature occurred. From the graphical presentation
of the temperature vs. time (cooling curve), the point where the sudden drop of temperature landed before
it slowly decreases continuously is the recorded freezing point. The melted naphthalene solid which was
cooled in an air bath recorded 80 degrees Celsius as the freezing point. After three minutes and a half, the
temperature reached by the solidification of naphthalene was 67 degrees Celsius.

Cooling Curve of Pure Naphthalene


100
90
80
70
60
50
40
30
20
10
0
0 10 20 30 40 50 60 70 80 90 100 110 120 130 140 150 160 170 180 190 200

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Temperature ( ℃ )

Cooling Curve of Naphthalene and Acetanilide Solution


Time (secs)
100
90 Graph 1. Cooling Curve of Naphthalene
80
The second part of the experiment included the determination of the cryoscopic constant of
naphthalene. 70The cryoscopic constant indicates the freezing point depression of a solvent with an added
60
solute. It is significant in calculating an unknown molar mass by relating the cryoscopic constant with the
molality of the 50 mixture. The added solute on the solvent was acetanilide, the freezing point of the solution
was recorded40at 77 degrees Celsius. This decrease of freezing point is called the freezing point depression.
The added solute30 on the naphthalene required more energy to be removed from the because its disorder
state made it 20harder to create an ordered state that in the pure solvent. The calculated cryoscopic constant
was 3.98 degrees10 Celsius per molal while the freezing point depression was 3.00 degrees Celsius. After
three minutes, the recorded temperature of the solution was 68.1 degrees Celsius.
0
0 10 20 30 40 50 60 70 80 90 100 110 120 130 140 150 160 170180 190

Temperature ( ℃ )

Time (secs)

Graph 2. Cooling Curve of Naphthalene and Acetanilide Solution

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The third part of the experiment entails the determination of the molecular mass of the assigned
solid. The graph below show the solute added to the naphthalene recorded a freezing point of 71 degrees
Celsius which was a lot lower as compared with the previously recorded temperatures. After almost 3
minutes, the recorded temperature of the solution was 64.4 degrees Celsius.

Cooling Curve of Naphthalene and the Assigned Solid Solution


100
90
80
70
60
50
40
30
20
10
0
0 10 20 30 40 50 60 70 80 90 100 110 120 130 140 150 160 170

Temperature ( ℃ )

Time (secs)

Graph 3. Cooling Curve of Naphthalene and p-dichlorobenzene solution

Using the cryoscopic constant calculated from the previous part, the molecular mass of the solid
was determined. The formula for the change in freezing point was used in computing of the mass.
∆ T f =K f m

Since molality is equal to moles of solute over kilogram of solvent,

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3.98 ℃/m(0.1036 g)
m olecular mass=
80 ℃−71 ℃(1.0072 x 10−3 kg)
The calculated molecular mass of the solid was 45.5 g/mol which was lower compared with p-
dichlorobenzene’s true molecular mass which is 146.99 g/mol. Errors done in the laboratory have
influenced the substance’s change in molecular mass.

CONCLUSIONS
The cryoscopic method of determining the molecular mass of a solid demonstrates the
significance of solutions’ colligative properties particularly the freezing point depression. From the
obtained change in temperature, the molecular mass of the substance was calculated. The added solutes in
the solvent caused the lowering of the freezing point of the solutions as compared with the pure solvent.
This is due to the particles of the solute interfering with the solvent’s ordered state thus, requiring a lower
temperature for solidification to occur.
The objectives of the experiment were achieved with the determination of the theoretical
molecular mass of the assigned solid which was p-dichlorobenzene. The experiment’s percent error was
relatively high. The calculated molecular mass was much smaller as compared with the true value. Errors
committed have affected the resulting values. Some of these could be the incorrect freezing points
measured, improper transferring of the weighed solids from the foil to the test tube, and letting particles
stick to the thermometer thus changing molality.

AUTHOR INFORMATION
Corresponding Author:
KRIZZI EVE D. GARCIA
Email: krizzieve.garcia.sci@ust.edu.ph
Contact number: 09294864335

ACKNOWLEDGMENTS
The authors would like to acknowledge the assistance of Assoc. Prof. Joyce T. Tan, M.Sc. and Prof. Jose
H. Bergantin, Jr., Ph.D. of the Chemistry Department at University of Santo Tomas, College of Science.

REFERENCES
1) Brown, T. L., LeMay, H. E., Bursten, B. E., Murphy, C. J., Woodward, P. M., & Stoltzfus, M. W.
(2018). Chemistry: The Central Science (14th ed.). United Kingdom: Pearson

2) Generalic, Eni. (n.d.). "Cryoscopic constant." Croatian-English Chemistry Dictionary &


Glossary. Retrieved November 11, 2018 from https://glossary.periodni.com.

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3) Malik, M. (2017, December 03). What are some unique and useful applications of colligative
properties?. [Online forum comment]. Retrieved from https://quora/What-are-some-unique-and-
useful-applications-of-colligative-properties

4) Merriam-Webster’s collegiate dictionary (10th ed.). (1999). Springfield, MA: Merriam-Webster


Incorporated.