EXPERIMENT 2

Sublimation and Recrystallization

OBJECTIVES
 To perform sublimation on air fresheners.
 To extract paracetamol from tablets and purify it by recrystallization.

DISCUSSION

Impurities are commonly present in most substances upon synthesis and

analyses, thus, purification processes are employed. For solid substances,
sublimation and recrystallization processes are the useful techniques.

Sublimation is the process whereby a solid evaporates from a warm

surface and condenses on a cold surface. When the amount of material
to be purified is less than 100 mg, sublimation is the method of choice for
purifying a solid. Some solids sublime at atmospheric pressure but for
substances with lower vapor pressures, sublimation can take place if
vacuum is applied.

Crystallization is accomplished by dissolving the material to be purified in

an appropriate hot solvent. As the solvent cools, the solution gets
saturated with the material which crystallizes. As the material crystallizes,
foreign materials are excluded from the developing crystal lattice such
that the crystal form is a pure substance. The crystals are then removed
from the solvent by filtration. The surface of the crystals is washed using
the cold solvent. In crystallizing natural products, decolorization is
necessary to remove pigments. Finally, the crystals are dried.

MATERIALS

Bring the following materials

 Air freshener (e.g. albatross); gel-type fresheners will not work
 Moth balls (naphthalene)
 (2) Analgesic tablets containing only paracetamol as active
ingredient (different brands for each group)
 Small piece of cotton

Experiment 2  Sublimation and Recrystallization

 Borrow the following materials
 spatula
 water bath
 (2) 250 mL beakers
 Hot plate
 (2) 50 mL beakers
 stirring rod
 a piece of boiling chip
 iron ring + iron stand
 top loading balance
 funnel
 graduated cylinder
 watch glass
 mortar and pestle
 (2) filter paper
 Thermometer
 Clay triangle

REAGENTS

Substance Description
 acetone Liquid
 activated carbon powder

SAFETY PRECAUTIONS
 Thoroughly clean your work area before and after
experimentation.
 Acetone is flammable. Do not heat it directly.
 Avoid inhaling the vapors of the air fresheners and naphthalene.
 Wear your lab coat, safety goggles, safety masks and lab gloves.
 Be careful handling heating equipment and hot glasswares.

PROCEDURE

A. SUBLIMATION

1. Place a few lumps of air freshener weighing about 2 grams in a 250

mL beaker. Measure the exact weight using a top loading balance.

2. Cover the beaker with a watch glass. Place ice over the watch
glass. You can also use aluminum foil to cover the beaker.

3. Place the set-up on a warm water bath at 50 C. You can replace

the ice during the process. Avoid inhaling the vapors. Continue
heating until sublimation is complete. Remove the set-up from the
heat source and let it cool.

Experiment 2  Sublimation and Recrystallization

 4. Scrape the deposited solids from the watch glass and walls of the
beaker. Obtain the exact weight of material.

5. Calculate the percent recovery

weight of purified material

percent recovery = x100
initial weight

6. Repeat the procedure using mothballs (naphthalene). This time

use a water bath at 75 C.

B. RECRYSTALLIZATION

1. Using a mortar and pestle, crush two paracetamol tablets of the

same brand. Transfer to a 50-mL beaker and measure the exact
weight using a top-loading balance.

2. To the paracetamol sample, add 20 mL acetone, and a boiling chip.

3. Partially fill a water bath with water, place on a hot plate and heat
the water to 40 C. Using a thick cloth to protect your hands,
remove the water bath from the hot plate. Place the beaker
containing the sample in this hot water bath for about a minute.

4. Filter the undissolved material (fillers and binders) using a funnel

and filter paper. Evaporate the solvent from filtrate using a warm
water bath (at a temperature not more than 40 C). You can
facilitate the evaporation process by drying it against an electric
fan. The solid that will remain is crude or impure paracetamol.

5. Place 10 mL water to the solid and dissolve by heating in a water

bath. If the previous filtration did not remove the colorants, add a
pea-sized amount of activated carbon to the mixture.

6. Using a thick cloth to protect your hands, filter the hot solution
through a very small cotton in a warm funnel. You can warm the
funnel by pouring hot water first.

7. Cool the fitrate in an ice bath. Filter the crystals and dry by
pressing with filter papers. Obtain the exact weight of the dry
paracetamol. Calculate the percent recovery.

Experiment 2  Sublimation and Recrystallization

 DISPOSAL AND CLEAN-UP:
All aqueous solutions can be discarded into the sink. Flush with generous
amounts of tap water. Place solids and paper into the solid wastes
container.

Experiment 2  Sublimation and Recrystallization

 NAME: ____________________________

GROUP: _________RATING:____________

LAB REPORT FOR DATE PERFORMED: __________________

EXPERIMENT 2 DATE SUBMITTED: ___________________

________________________________________________________________________

Sublimation and Recrystallization

RESULTS AND OBSERVATIONS

A. SUBLIMATION

Sample Percent recovery (%)

p-dichlorobenzene (air freshener)
Naphthalene (moth balls)

B. RECRYSTALLIZATION

Paracetamol brand
Weight used (mg)
Weight of paracetamol per tablet on the
label (mg)
Weight of recrystallized paracetamol (mg)
Weight of recrystallized paracetamol per
tablet (mg)
= Weight of recrystallized paracetamol
(mg)/2
Percent recovery

CALCULATIONS

Experiment 2  Sublimation and Recrystallization

LAB REPORT FOR EXPERIMENT 2 (continued) NAME:

POST-LAB QUESTIONS

1. State the characteristics of a good recrystalization solvent.

2. Why is a solution cooled to effect recrystallization?

SUMMARY AND CONCLUSIONS

Experiment 2  Sublimation and Recrystallization