JOURNAL OF

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

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ABSTRACT: The separation of mixtures of substances into their components is called

chromatography. An example of this are pens with different inks of different colors where the variation
of the bonding properties of each molecule of the ink is utilized through the process of paper
chromatography. Qualitative and quantitative analysis are done on organic and inorganic samples by the
process of chromatography. Chromatography uses two types of substances; first is the mobile phase,
where a liquid or a gas transports the solution being tested with the other substances like water and rubbing
alcohol; second is the stationary phase where the solid and liquid which the tested substance is carried
like filter paper and a paper towel. In other words, solvent is the mobile phase while paper which is placed
in the solvent is stationary phase. Through this experiment, students can learn how to separate the
different components of a mixture. This allows the students to see the different components of the mixture
as they undergo separation.
KEYWORDS: Cryoscopic constant, Colligative properties, Molality, Freezing point depression

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INTRODUCTION
Certain important properties of solutions state tends to lower the tendency of the particles
depend on the concentration of solute particles in to escape to the gas phase (Brown, et al., 2018).
solution and not upon the nature of the solute.
Colligative properties describe these
The cryoscopic method is a technique
characteristics of solution (Chang & Overby,
used to determine a molecular mass of a solute by
2011). The four properties are vapor pressure
dissolving it and measuring the freezing point
lowering, boiling point elevation, freezing point
depression of the solution (Merriam-Webster’s
depression and osmotic pressure. When a
Dictionary, n.d.). This method utilizes the
particular nonvolatile solute is added to a solvent,
cryoscopic constant, which expresses the freezing
the vapor pressure of the liquid is decreased. The
point depression by the addition of a solute
decrease in vapor pressure is an example of vapor
(Croatian-English Chemistry Dictionary &
pressure lowering caused by the presence of
Glossary, 2018). The objective of the experiment
solute. The stability of the solvent in the liquid

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STUDENT LEARNING GOALS
This laboratory experiment aims the
students to determine the molecular mass of the
assigned substance by the lowering it causes 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 weight of the assigned unknown solid
from the lowering it causes on the freezing point
of the solvent, naphthalene.
EXPERIMENTAL SECTION
Determination of Freezing Point of
Napthalene
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 and was
transferred into a test tube. The test tube was then
heated in boiling water until the solid melts. A
thermometer was inserted into the test tube and
was immersed in the melt. Then a cotton plug was
used to cover the test tube to prevent the escape
of obnoxious odor. After the solid completely
melted, the hot test tube was transferred into an
air bath and was allowed to cool while stirred
gently. 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 is 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.
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.

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 and considered as 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. The determination of the freezing point of pure naphthalene

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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. 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
Cooling Curve of Pure Naphthalene melted
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

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.
Temperature (degrees
Celsius)

Time (secs)

Graph 1. Cooling Curve of Naphthalene

The second part of the experiment included the determination of the cryoscopic constant of
naphthalene. The cryoscopic constant expresses the freezing point depression of a solvent with an added
solute. It is significant in calculating an unknown molar mass by relating the cryoscopic constant with the
molality of the mixture. The added solute on the solvent was acetanilide, the freezing point of the solution

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was recorded at 77 degrees Celsius. This decrease of freezing point is called the freezing point depression.
The added solute on the naphthalene required more energy to be removed from the because its disorder
state made it harder to create an ordered state that in the pure solvent. The calculated cryoscopic constant
was 3.98 degrees 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.
Temperature (degrees

Cooling Curve of Naphthalene and the Assigned

Solid Solution
Celsius)

100
90
80
70
60
50
40
30
20
Time (secs)
10
0 The
third 0 10 20 30 40 50 60 70 80 90 100 110 120 130 140 150 160 170
part of the
experiment
entails the determination of the molecular mass of the assigned solid. 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 Acetanilide

Solution
100
90
80
70
60
50
40
30
20
10
0
0 10 20 30 40 50 60 70 80 90 100 110 120 130 140 150 160 170 180 190
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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.
∆𝑇𝑓 = 𝐾𝑓𝑚
Since molality is equal to moles of solute over kilogram of solvent,
𝑔 𝑢𝑛𝑘𝑜𝑤𝑛

𝑇𝑓 − 𝑇𝑓 ′ = 𝐾𝑓( 𝑘𝑔𝑚𝑚 𝑢𝑛𝑘𝑛𝑜𝑤𝑛

𝑛𝑎𝑝ℎ𝑡ℎ𝑎𝑙𝑒𝑛𝑒
)

The calculated molecular mass of the solid was 45.5 g/mol.

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 determined,
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:
ALYSSA MAY FRIAS
Email: alyssamay.frias.sci@ust.edu.ph
Contact number: 09161374788

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

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2) Brown A. (2013, Aug 26). Paper Chromatography. Retrieved September 29, 2018 from
https://www.amybrownscience.com/2012/01/paper-chromatography.html.

3) Coppens T. (2016, June 15). What Is Paper Chromatography and How Does it Work?. Retrieved
September 28, 2018 from https://owlcation.com/stem/What-is-Paper-Chromatography-and-How-
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4) Goldwhite H. (2017, October). Experiments in General Chemistry. 4th edition revised.

5) Harper College. (n.d.). Retention factors. Retrieved September 29, 2018 from
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