Chem 31.

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EXPERIMENT 2
Recrystallization and Melting Point Determination

I.

Objectives
1. To clarify the meaning of purity in the chemical sense
2. To apply the method of 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 vs. impure sample of a
substance

II.

Procedure
A. Selection of a Solvent for Recrystallization
1. Using the tip of a spatula, place a small amount of the crude sample
into a test tube. Add about 5 mL of water.
2. If the sample is not completely soluble, gently heat the test tube in a
water bath.
3. If a solution is obtained in hot water, allow the solution to cool slowly at
room temperature.
4. Compare the size, color and crystal form of the resulting crystals with
the original solid material.
5. Repeat steps 1 5 using: a) 95% ethanol; and b) CCl4
B. Recrystallyzation
Note: Set aside a small portion of the crude sample and determine its
melting point (procedure C).
Prepare a hot filtration set up.
Weigh 0.5 g of sample and place in a test tube.
Add 7.5 mL solvent into the test tube (15 mL/gram of crude sample)
Heat the tube in a hot water bath with stirring until all the solid
dissolves.
5. If the solution is colored, swirl with a small pinch of activated carbon
after the solution has cooled down to at least 5 0C below its boiling
point.
6. Filter the hot mixture rapidly
7. Allow the filtrate to cool to room temperature slowly. DO NOT
AGITATE THE MIXTURE.
1.
2.
3.
4.

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8. After the mixture has cooled to room temperature, place the test tube
in an ice water bath, along with the test tube of pure solvent.
9. If crystals do not form, scratch the inside of the test tube with a stirring
rod.
10. Filter the crystals by suction
11. Wash the crystals with the cold solvent
12. Continue the suction until no more solvent passes through the filter
13. Determine the melting point of the recrystallized sample. Compare the
melting point range obtained with that of the crude sample.
14. Put the rest of the sample in a vial and label it properly. Submit to your
instructor.

C. Melting Point Determination

1. Pulverize a small amount of the sample with the aid of a clean
watchglass and stirring rod
2. Make a heap of the powder. Gently thrust the open end of a melting
point 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 the
figure.
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.
III.

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

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