SCI 212 – Lab 3 – Sublimation and Boiling Point Determination of Benzoic Acid

OBJECTIVES:
• Purify benzoic acid by sublimation.
• Determine and compare the melting point of the product with a standard.
• Calculate the percentage recovery

BACKGROUND INFORMATION

The vapor pressure of a solid varies with its temperature. There are some solids that can pass directly
into the vapor phase without going through the liquid phase. Since the vapor can solidify, the vaporization-
solidification cycle can be used as a purification process. The purification can be done only if the impurities are
non-volatile or have significantly lower vapor pressure than the pure compound.

Non-polar substances are symmetrical compounds that have high melting points and high vapor
pressures. The ease by which a non-polar substance can break away from the solid state is determined by the
strength of intermolecular forces. Symmetrical compounds have a relatively even distribution of electron
density and a small dipole moment. A smaller dipole moment means a higher vapor pressure due to lower
electrostatic attractive forces in the crystal.

If the vapor pressure is greater than the atmospheric pressure at the melting point, the solid will sublime.
Sublimation is a technique used to purify solid mixtures. Melting point determination can be employed to
ascertain the identity and purity of an unknown compound.

MATERIALS NEEDED

Bunsen burner iron stand and clamp capillary tubes

beaker cork rubber band/thread
watch glass iron ring cooking oil (unused)
thermometer wire gauze benzoic acid

STEPS/PROCEDURE

1 Place 5 g of impure benzoic acid in an evaporating dish. Cover the dish with a perforated filter paper.
On top of the filter paper, place an inverted pre-weighed watch glass (meaning, you have to weigh the
watch glass before accomplishing the step 1). Seal all the openings with masking tape. Heat using a hot
plate.
2 Cool the center top of the watch glass with a tissue paper kept moist with water. Continue heating for
10-15 minutes until most of the sample has vaporized.
3 Stop heating and cool the set-up. Carefully invert the pre-weighed watch glass. Collect all the sublimate
(including the crystals adhering to the perforated filter paper) in the pre-weighed watch glass and weigh.
Calculate the percentage recovery.
4 For melting point determination, grind the sublimate into a fine powder. Seal one end of the capillary
tube using a bunsen burner. Press the open end of a capillary tube into the powder.
5 Drop the closed end of the capillary tube down through a glass tubing several times until it is well-
packed with 3-5 mm of the sublimate.
6 Attach the capillary tube to a thermometer with a piece of thread/rubber band or masking tape. Align the
closed end of the capillary tube with the mercury bulb of the thermometer.
7 Immerse the capillary tube in an oil bath and heat. Stir constantly. TAKE NOTE of the temperature at
which the sublimate starts to melt and when it is completely melted.
Answer the ff:

Pre-Lab Questions:

1 What is sublimation? What is melting point

2 In this experiment, why is it preferable to use an oil bath instead of a water bath?
3 Why is it necessary to grind the sample?
4 Why is it important to pack the sublimate uniformly?

Data Sheet

• Weight of the impure benzoic acid _______________________

• Weight of the watch glass + sublimate _______________________

• Weight of the watch glass (empty) _______________________

• Weight of the sublimate _______________________

• Percentage recovery _______________________

• Melting point of benzoic acid _______________________

Post-Lab Questions:

1 What are the limitations of sublimation as a purification method?

2 Give other methods of determining the melting point of a compound

Provide a report and documentation of this laboratory experiment (sample reference:

tinyurl.com/sci212-lab3)

Note: The submission of this output will be further announced in the online LMS