GENERAL CHEMISTRY LAB MANUAL

FORMULA MASS OF A SOLID

REAGENTS
Cyclohexane
Unknown solute
CAUTIONS
Be careful while working with cyclohexane and dispose the waste of cyclohexane and
cyclohexane solution in the “Waste Liquids” container.
PURPOSE
 To determine the formula mass (molecular weight) of a nonvolatile, non-electrolyte
solute by observing the difference between the freezing points of a solvent and a
solution.

INTRODUCTION AND THEORY

The addition of a nonvolatile solute to a solvent produces characteristic changes in several

physical properties of the solvent. It lowers the vapour pressure of the solvent, it increases the
boiling point of the solvent, it decreases the freezing point of the solvent, and it creates an
osmotic pressure for the solvent. These physical properties are called colligative properties
because these changes depend only upon the number of solute particles dissolved in the
solvent, not the kind of solute particles.

For example, one mole of glucose or urea (neither dissociate) lower the freezing point of one
kilogram of water by 1.86 ºC; whereas one mole of sodium chloride (it dissociates in solution,
NaCl (aq) → Na+(aq) + Cl– (aq)) lowers the freezing point of one kilogram of water by nearly
twice that amount (≈3.72 ºC) because it provides twice as many moles of solute particles per
mole of solute as do glucose or urea. When salt is used to freeze ice cream the salt-ice-water
mixture used as a low temperature bath is at a lower temperature than an ice-water mixture
alone. Antifreeze (ethylene glycol) added to the cooling system of the automobile reduces the
probability of freeze-up in the winter and boiling in the summer because the antifreeze-water
solution has a lower freezing point and a higher boiling point than pure water.

These changes in the properties pure water, when it dissolves a non-volatile solute, are
illustrated by the phase diagram in Figure 1, a plot of vapour pressure as a function of
temperature. The solid lines refer to the equilibrium conditions between the respective phases
for pure water; the second line represent the same conditions for an aqueous solution.

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Figure 1. Phase diagram for water and an aqueous solution

When the vapour pressure of water is 760 torr, it boils at 100 ºC. When a non-volatile solute
is dissolved in water to form a solution, solute molecules occupy a part of the surface area.
This, inhibits movement of some water molecules into the vapour state causing a vapour
pressure lowering of the water (Figure 1), lower than 760 torr. Since the vapour pressure is
less than 760 torr, the solution (more specifically, the water in the solution) no longer boils at
100 ºC. For the solution to boil its vapour pressure must be increased to 760 torr; this is done
by increasing the temperature above 100 ºC. This is the boiling point elevation (Figure 1) of
the water due to the presence of the solute.

A solute added to water also affects its freezing point. The normal freezing point of water is 0
ºC, but in the presence of a solute, the temperature must be lowered (the energy of the water
molecules must be lowered to increase the magnitude of the intermolecular forces, so that the
water molecules "stick") below 0 ºC before freezing occurs; this is the freezing point
depression of the water due to the solute.

The changes in the freezing point, ΔTf, and the boiling point, ΔTb, are directly proportional to
the molality of the solute in solution. The proportionality is a constant, characteristic of the
actual solvent. For water the freezing point constant, Kf, is 1.86 ºC• kg/mol and the boiling
point constant, Kb, is 0.512 ºC• kg/mol.

ΔTf = | tf, solvent – tf, solution | = Kf m (1)

ΔTb = | tb, solvent – tb, solution | = Kb m (2)

tf represents the freezing point and tb represents the boiling point of the system.
| tf, solvent – tf, solution | represents the absolute temperature difference in the freezing point
change.

(3)
Kf and Kb values for various solvents are listed in Table 1.

In this experiment the formula mass of a solid solute is determined, using cyclohexane as a
solvent, by measuring the freezing point difference between pure cyclohexane and the
solute/cyclohexane solution. From the Kf (Table 1) and equations 1 and 3, you can calculate
the moles of solute dissolved and from the measured mass, calculate formula mass of the
solute.

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The freezing points of the cyclohexane and the cyclohexane solution are obtained from a
cooling curve-a plot of temperature vs. time (Figure 2). The cooling curve for pure
cyclohexane reaches a plateau at its freezing point. The cooling curve for the solution does
not reach a plateau, but continues to decrease slowly as the cyclohexane freezes. Its freezing
point is determined at the intersection of two straight lines drawn through the data points
above and below the freezing point (Figure 2).

Table 1. Molal Freezing Point and Boiling Point Constants for a Number of Solvents
Substance Freezing Kf Boiling Kb
Point (ºC) (ºC•kg /mol) Point (ºC) (ºC•kg /mol)
H2O 0.0 1.86 100.0 0.512
Cyclohexane - 20.0 80.7 2.69
Naphthalene 80.2 6.9 - -
Camphor 179 39.7 - -
Acetic acid 17 3.90 118.2 2.93
t-butanol 25.5 9.1 - -

Figure 2. Cooling curves for a pure solvent and a solution

TECHNIQUES
Review the techniques that are used for this experiment from the laboratory guideline.

EXPERIMENTAL PROCEDURE

Obtain about 15 ml of cyclohexane. You’ll use this throughout the experiment. Your
laboratory instructor will issue to you about 1 gram of unknown solute. Record the unknown
number on the Report Sheet.

A. Freezing Point of Cyclohexane ( Solvent)

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1. Construction of Apparatus. Assemble the apparatus shown in Figure 3. Use a 600-ml

beaker as an outside, insulating beaker. You may want to place paper between the 600-ml
beaker and the 400-ml beaker to better insulate the ice-water bath. Place about 300 ml of an
ice-water slurry into the 400-ml beaker.

Obtain a thermometer clamp, mount it to the right stand, and position the thermometer into
the test tube. Insert a wire stirrer into the test tube.

Figure 3. Freezing point apparatus

2. Preparation of Cyclohexane. Weigh (±0.01 g) your clean, dry 200 mm-test tube in a 250-
ml beaker. Add approximately 10 g of cyclohexane to the test tube and reweigh. Record these
two masses on the Report Sheet. Place the test tube and cyclohexane in the ice-water bath
(Figure 3). Secure the test tube with a utility clamp. Insert the thermometer and wire stirrer
into the test tube. Make sure the thermometer extends down into the cyclohexane.

3. Data for the Freezing Point of Cyclohexane. While stir,ing with the wire stirrer, record
the temperature (± 0.1 Cº) readings at timed intervals (30 or 60 seconds) on the Report Sheet.
The temperature remains virtually constant at the freezing point until the solidification is
complete. Continue recording until the temperature begins to drop again.

4. Plot the Data. On linear graph paper, plot the temperature (ºC, vertical axis) vs. time (sec,
horizontal axis) to obtain the cooling curve for cyclohexane. Have your instructor approve
your graph.

B. Freezing Point of Cyclohexane + Unknown Solute

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Three freezing point trials for the solution are to be completed. Successive amounts of
unknown sample are added to the cyclohexane in Parts B.4 and B.5.

1. Mass of Solid Solute. Dry the outside of the test tube containing the cyclohexane and
reweigh (±0.01 g). Weigh approximately 0.1 to 0.3 g of unknown solute (ask your instructor
for the approximate mass to use) on weighing paper. Quantitatively transfer the unknown
solid solute to the cyclohexane in the 200-mm test tube.1
2. Data for the Freezing Point of Solution. Determine the freez,ing point of this solution in
the same way as that of the solvent (Part A.3). When the solution nears the freez,ing point of
the pure cyclohexane, record the temperature at more frequent time intervals (≈ 15 seconds).
A break in the curve occurs as the freezing begis, although it may not be as sharp at that for
the pure cyclohexane.
3. Plot the Data on the Same Graph. Plot the temperature vs. time data on the same graph
as that for the pure cyclohexane (Part A.4). Draw straight lines through the data points above
and below the freezing point, the intersection of the two straight lines is the freezing point of
the solution.
4. Repeat with Additional Solute. Remove the test tube/solution from the ice-water bath.
Add an additional 0.1 to 0.2 g of unknown solid solute, using the same procedure as in Part
B.1. Repeat the freezing point determination and plot the temperature vs. time data on, again,
the same graph (Parts B.2 and B.3).
5. Again, Repeat with Additional Solute. Repeat Part B.4 with a n additional 0.1 to 0.2 g of
unknown solid solute, using the same procedure as in Part B.1. Repeat the freezing point
determination and again plot the temperature vs. time data on the same graph (Parts B.2 and
B.3). You now should have four plots on the same graph.
6. Instructor’s Approval. Have your instructor approve the three temperature vs. time graphs
that have been added to your first temperature vs. time graph for the pure cyclohexane.

DISPOSAL INFORMATION: Dispose of the waste cyclohexane and cyclohexane solution in

the "Waste Liquids (Cyclohexane)" container.

1
In the transfer be certain that none of the solid solute adheres to the test tube wall. If some does, roll the test
tube until the solute dissolves.

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PRE-EXPERIMENT ASSIGNMENT

FORMULA MASS OF A SOLID

1. Students prepared two cyclohexane solutions having the same mass of solute. Student 1
used 13 g of cyclohexane and Student 2 used 10 g. Which student will observe the larger
freezing point change? Explain.

2. A 0.433 g sample of non-volatile solid solute dissolves in 15.6 g of cyclohexane. The

change in the freezing point is 3.62 C. What is the formula mass of the solute?

3. What is the actual boiling point of the solution in Question 2?

4. Are the unknowns in this experiment expected to be polar or nonpolar solutes? Explain.

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5. Cyclohexane and the cyclohexane solution may ‘undercool’ at their freezing points.
a. Define undercoling (supercooling).

b. How can undercooling be avoided (or minimized)?

Report Sheet

FORMULA MASS OF A SOLID

Student’s Name: Date:

Laboratory Section: Assistant’s name and signature:

A. Freezing Point Of Cyclohexane (Solvent)

1. Mass of test tube + cyclohexane (g)

2. Mass of test tube (g)
3. Mass of cyclohexane (g)
4. Freezing point, from cooling curve (ºC)
5. Instructor’s Approval of graph

A. Freezing Point Of Cyclohexane + Unknown Solute

Unknown Solute No.

Trial 1 Trial 2 Trial 3

(Parts B1,B3) (Parts B.4) (Parts B.5)
1. Mass of test tube + cyclohexane (g)
2. Mass of cyclohexane (g)
3. Mass of solute (g)
4. Freezing point, cooling curve (ºC)
5. Instructor’s Approval of graph

Calculations
1. Kf for cyclohexane 20.0 ºC • kg /mol
2. Freezing point change, ΔTf (ºC)
3. Mass of solute in solution, total (g)

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4. Mass of cyclohexane in solution (kg)

*
5. Moles of solute (mol)
6. Formula mass of solute
7. Average formula mass of solute

A. Cyclohexane B. Cyclohexane + Unknown Solute

Trial 1 Trial 2 Trial 3
Temp. Time Time Temp Time Temp Time Temp

Continue recording data on your own paper and submit it with the report sheet.

*
Show work for this calculation.

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QUESTIONS
1. If the freezing point of the solution is erroneously read 0.2 ºC lower than it should be,
will the calculated formula mass of the solute be too high or too low? Explain.

2. How will the freezing point change in this experiment be affected by

a.The presence of a volatile solute? Explain.
b. Two solutes that react according to the equation A +B → C? Explain.

3. If a thermometer is miscalibrated to read 0.5 ºC higher that the actual temperature over its
entire scale, will the reported formula mass of the solute be too high or too low?

4. If some solute adheres to the test tube wall in Part B.1, will the freezing point change be
greater than or less than it should be? Explain.

5. If the cyclohexane is initially, but unknowingly, contaminated with a non-reactive, non-

volatile solute, how (if at all) does this affect the reported formula mass of the solute? Why?

6. Explain why the freezing point of a pure solvent remains constant whereas the freezing
point of a solution continues to decrease with time (Figure 2).

Report Sheet

FORMULA MASS OF A SOLID

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Student’s Name: Date:

Laboratory Section: Assistant’s name and signature:

A. Freezing Point Of Cyclohexane (Solvent)

1. Mass of test tube + cyclohexane (g)

2. Mass of test tube (g)
3. Mass of cyclohexane (g)
4. Freezing point, from cooling curve (ºC)
5. Instructor’s Approval of graph

A. Freezing Point Of Cyclohexane + Unknown Solute

Unknown Solute No.

Trial 1 Trial 2 Trial 3

(Parts B1,B3) (Parts B.4) (Parts B.5)
1. Mass of test tube + cyclohexane (g)
2. Mass of cyclohexane (g)
3. Mass of solute (g)
4. Freezing point, cooling curve (ºC)
5. Instructor’s Approval of graph

Calculations
1. Kf for cyclohexane 20.0 ºC • kg /mol
2. Freezing point change, ΔTf (ºC)
3. Mass of solute in solution, total (g)
4. Mass of cyclohexane in solution (kg)
*
5. Moles of solute (mol)
6. Formula mass of solute
7. Average formula mass of solute

*
Show work for this calculation.

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QUESTIONS
3. If the freezing point of the solution is erroneously read 0.2 ºC lower than it should be,
will the calculated formula mass of the solute be too high or too low? Explain.

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4. How will the freezing point change in this experiment be affected by

a.The presence of a volatile solute? Explain.
b. Two solutes that react according to the equation A +B → C? Explain.

3. If a thermometer is miscalibrated to read 0.5 ºC higher that the actual temperature over its
entire scale, will the reported formula mass of the solute be too high or too low?

4. If some solute adheres to the test tube wall in Part B.1, will the freezing point change be
greater than or less than it should be? Explain.

5. If the cyclohexane is initially, but unknowingly, contaminated with a non-reactive, non-

volatile solute, how (if at all) does this affect the reported formula mass of the solute? Why?

6. Explain why the freezing point of a pure solvent remains constant whereas the freezing
point of a solution continues to decrease with time (Figure 2).

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