Sublimation

Objectives
This experiment will introduce the students to a separation technique involving sublimation. Specifically,
they will learn to

1. determine which mixtures can be separated through sublimation;

2. build a sublimation setup; and
3. purify a mixture through sublimation
Overview
Before most solid organic compounds evaporate, they melt, a process that usually requires a reasonably high
temperature. However, some substances exhibit appreciable vapor pressure below their melting points. These
substances change directly from the solid phase to the gas phase without forming an intermediate liquid
phase by a process called sublimation or volatilization. The process of sublimation seems somewhatunusual
in that, unlike normal phase changes from solid to liquid to gas, no liquid phase forms between the solid and
gas phases.

In the laboratory, sublimation is used as a purification method for an organic compound (1) if it can vaporize
without melting, (2) if it is stable enough to vaporize without decomposition, (3) if the vapor can be
condensed back to the solid, and (4) if the impurities present do not also sublime. Many organic compounds
that do not sublime at atmospheric pressure sublime appreciably at reduced pressure, thus enabling their
purification by sublimation. For certain substances, sublimation at ambient atmospheric pressure can be
performed by converting the solid into its gaseous phase by heating in a sublimation chamber (sublimator)
or beaker. A cold finger is set over the sublimation chamber; it can be any cold surface that enables collection
of the deposited vapor. When the vapor comes into contact with the cold finger, the temperature lowers
allowing it to return to solid phase (deposition).

This experiment will be divided into two parts wherein the first involves purification of samples of
naphthalene, camphor, and phthalic acid anhydride and the second is separation of iodine from a mixture. It
will also provide a modified sublimation setup if a sublimator apparatus is not available. Practice caution as
heat sources, vacuum pumps, delicate glassware, and harmful reagents are used. The rate of recovery in
purification or separation is expressed in percentage of the ratio of the mass of the sublimate to the
mass of the crude sample .
Procedure
Using a sublimator apparatus
Mount the sublimator on an iron stand. In separate containers, prepare crude samples of naphthalene,
camphor, and phthalic acid anhydride (a). Record the mass of each sample that will be introduced into the
sublimator. The amount of the crude solid should be enough that it does not touch the cold finger and the
purified solid depositing on the cold finger grows down and touches the crude solid. Put the crude solid into
the bottom of the sublimator (b) and afterwards insert the cold finger into the sublimator (c), keeping in mind
proper jointing and greasing.

Connect the cold finger inlet to the tap by attaching a hose; attach a hose to the outlet and lead it to the sink
or back to the reservoir. Connect the sublimator to a vacuum pump. Slowly start the cooling circuit and the
vacuum pump, in that order. Next, slowly begin heating the bottom of the sublimator using a heat gun or any
other heat source (c). Vapors will start forming and eventually crystals, called a sublimate, deposit on the
cold finger (d). Until no more solids deposit on the cold finger, turn off the heat and let the sublimator cool.
Disconnect the cold finger from the cooling circuit and slowly release the pressure of the vacuum pump lest
a sudden inrush of air might blow off the sublimates. Carefully remove the cold finger without the sublimate
touching the walls of the sublimator, avoid excessive agitation or shaking the cold finger. Properly scrape
off the sublimate onto a pre-weighed watch glass or weighing boat. Record the mass of the sublimate and
determine the rate of recovery. Clean the sublimator and cold finger and start the process for the next crude
substance.

Using a petri dish

Prepare a clean and dry petri dish and separately weigh the base and the lid. Weigh about 1 gram of dry crude
naphthalene and place on the base of the dish and cover with the lid. Make sure the crude sample doesnot
touch the lid. Place a wire gauze atop a hotplate and place the covered dish with the crude sample. Set the
temperature to the appropriate range, depending on its sublimation point. Place a beaker filled with ice-water
bath atop the lid of the petri dish. Sublimates will deposit inside the lid; monitor the sublimation as the sample
may char during the process. Continue the sublimation until no more solids deposit inside the lidor no more
solid remains at the base. Remove the dish from the heat but keep the beaker atop the lid. Do notremove the
lid as the harmful fumes may escape. Let the sublimate cool. Carefully remove the lid and turn it over to
keep the sublimates from falling. Next, weigh the lid containing the sublimates and determine the mass of
the sublimate and the rate of recovery. Prepare two more dishes and start sublimation for camphor and
phthalic acid anhydride.

Separation of iodine
Prepare a mixture of 0.5 gram of iodine and 0.5 gram of salt and place in either setup (sublimator or petri
dish) for separation, whichever is available. Start the sublimation process, identify the sublimate and the
residue, and determine the recovered mass and rate of recovery.
 CHY 42.1
Sublimation

Name Date
Section Schedule
Group members Score

Data Sheet
1. Purification of naphthalene, camphor, and phthalic anhydride
a. Naphthalene
Crude Sublimate
Mass of container, g
Mass of container with sample, g
Mass of sample, g
Rate of recovery, %
b. Camphor
Crude Sublimate
Mass of container, g
Mass of container with sample, g
Mass of sample, g
Rate of recovery, %
c. Phthalic Anhydride
Crude Sublimate
Mass of container, g
Mass of container with sample, g
Mass of sample, g
Rate of recovery, %
2. Separation of iodine
Crude Sublimate
Mass of container, g
Mass of container with sample, g
Mass of sample, g
Identity of sublimate
Identity of residue
Rate of recovery, %
Observation upon heating the iodine-salt mixture
Exercises
1. Discuss the process of sublimation.

2. Which type of mixtures or samples can be separated or purified through sublimation?

3. Draw the structures of naphthalene, camphor, and phthalic anhydride.

Naphthalene Camphor Phthalic anhydride

4. The sublimation of naphthalene was performed in a purification experiment. At the beginning of the
technique, 6.9 g of impure naphthalene was obtained. After the purification technique was
completed, 4.7 g of pure naphthalene was recovered. Calculate the percent of naphthalene that was
recovered.

5. The phase diagram of a substance is shown below whose phase depends upon pressure and
temperature .
Pressure

a. Determine the range of temperatures that allows

purification by sublimation at a specific Solid
Liquid
pressure. Complete the table below.

Pressure Temperature range

p3

p2 Gas

p1
b. Is it possible to conduct sublimation at p3?
T1 T2 T3 Temperature
Explain your answer.