Experiment 2

PURIFICATION AND MELTING POINT DETERMINATION

I. Objectives
1. To clarify the meaning of purity in the chemical sense.
2. To apply the methods of sublimation and recrystallization in the purification of a
solid
sample.
3. To recognize melting point as a physical property that can serve as an index of
purity.
4. To determine the melting point of a substance using a simple apparatus.
5. To compare the melting point of a pure versus an impure sample of a substance.
II. Materials
Naphthalene
95% ethanol
Sand
Benzoic Acid
Iron clamps
Cooking oil
Test tubes
Hot plate
Thermometer
Water bath
Capillary tubes
Petri dish
III. Procedure
A. Recrystallization of Naphthalene
1. Selection of a Solvent for Recrystallization
a. Using the tip of a spatula, place a small amount of the naphthalene into a test
tube
and add about 5 mL of water. If the sample is not completely soluble, gently heat
the test tube in a water bath.
b. If a solution is obtained in hot water, allow the solution to cool slowly at room
temperature.
c. Compare the size, color and crystal form of the resulting crystals with the
original solid material.
d. Repeat steps a-c using 95% ethanol.
2. Recrystallization
a. Weigh 0.5 g of naphthalene and place it in a test tube.
b. Add 7.5 mL of solvent into the test tube (15mL/gram of sample)
c. Heat the test tube in a hot water bath with stirring until all the solid dissolves.
d. If the solution is colored, swirl with a small pinch of activated carbon after the
solution
has cooled down to at least 5C below its boiling point.
e. Filter the hot mixture rapidly.
f. Allow the filtrate to cool to room temperature slowly. DO NOT AGITATE THE
MIXTURE.
g. After the mixture has cooled to room temperature, place the test tube in an icewater
bath, along with the test tube of pure solvent.
h. Filter the crystals in a fluted, pre-weighed filter paper.
i. Wash the crystals both in the test tube and in the filter paper with the cold
solvent.
j. Air dry the filter paper in a pre-weighed petri dish and weigh in a top-loading
balance
after all the solvent is removed and the filter paper and the petri dish is dry.
k. Determine the %recovery after recrystallization.
B. Sublimation of Benzoic Acid
1. Weigh about 0.1 g of crude benzoic acid in a 50-mL beaker.
2. Cover with filter paper and hold the filter paper in place with a rubber band.

3. Place the beaker in a sand bath such that about 1/3 of the beaker is immersed.
4. Heat the sand bath in a hot plate. Continue heating until needle-like crystals
deposit on
on the filter paper and at the sides of the beaker.
5. Carefully remove the filter paper and scrape the sublimate into a previously
weighed
vial. Report the weight and the %recovery of pure benzoic acid.
C. Sublimation of Caffeine
1. Weigh all the isolated caffeine left from Expt 1 in a weighing cup and transfer in
an
evaporating dish.
2. Prepare a simple heating set-up with Iron stand, iron ring, Bunsen burner and
wire
gauze and heat the weighed caffeine.
3. Cover the evaporating dish with a watch glass and wait until caffeine sublimes
from the
Evaporating dish into the watch glass.
4. Scrape all the sublimate into a previously weighed weighing cup.
5. Report the weight of the sublimate and the %recovery of pure caffeine.
D. Melting point determination of Benzoic Acid
1. Pulverize a small amount of recovered pure benzoic acid from Part B with the aid
of a
clean watch glass and a stirring rod.
2. Make a heap of the powder. Gently thrust the open end of a capillary tube (a
glass
capillary closed at one end) into this heap. Tap the capillary tube gently to cause
the
sample to collect at the bottom of the capillary tube. Repeat this step until a
sample
1-2 mm high has collected in the bottom of the tube.
3. Assemble the melting point determination set-up as shown in Figure 1.
4. Heat the oil with a moderate Bunsen flame. Allow the temperature to rise fairly
rapidly
to within 15 to 20 degrees below the expected melting point of the sample.
Then adjust
the flame size so that the temperature rises no more than 2-3 degrees per
minute just
before, during and just after the period in which the compound melts.
5. Record the range of temperature from the first visible evidence of liquid (the
sample
appears moist, or a tiny drop of liquid is observed) to the complete liquefaction
of the
sample.

IV. Questions (serves as points of discussion)

1. What is a crystal and what is meant by recrystallization?
2. What is a sublimate and what is meant by sublimation?
3. How does sublimation and recrystallization free a substance from impurities?
Explain how each step
In recrystallization contributes to the removal of impurities.
4. What must be considered in choosing a solvent for recrystallization?
5. What is melting point? Why can it be used as an index of purity?