University of Santo Tomas Faculty of Pharmacy Organic Chemistry Laboratory

Sublimation and Melting Point Determination

Manlutac, D.T.; Maravillas, M.S.; Miranda, M.H.; Navarro, M.J.; Panaligan A.C.

Abstract
The experiment performed was about Sublimation and Melting Point Determination, wherein the target chemical was Benzoic Acid. The experiment used five grams of impure benzoic acid, which was sublimed in a tarred watch glass by heating the evaporating dish with perforated filter paper. The sublimate was dried by evaporation in a fume hood and was later weighted for the percentage recovery. After which it was inserted in a capillary tube separated in the pure benzoic acid for melting point determination. The filled capillary tubes were immersed in oil bath whose temperature is measured. The temperatures in which the powders melted were recorded.

Introduction Sublimation is the process were solid substances can pass directly into their vapor phase without passing through the liquid phase. This process occurs when the vapor pressure of a substance is greater than the atmospheric pressure at melting point. Since vapor can solidify, sublimation is considered a purification process for solid mixtures. Sublimation is done by heating the mixture in a evaporating dish which is covered usually of a watch glass. Sometimes a perforated paper is placed to achieve a purer sublimate. The melting point of a solid is the temperature at which it changes from solid to liquid phase. The melting point of Benzoic Acid is 122 C. Melting point

determination is the technique wherein two substances, one is the control and the other is the test subject, are compared to know whether the test substance is already purified of impurities. The objective of this experiment is to: a.) purify the benzoic acid by sublimation; b.) determine the melting point of benzoic acid by comparing the melting point of the pure benzoic acid to the product acquired from sublimation; c.) and lastly to calculate the percentage recovery Experimental The experiment for sublimation requires the following: Bunsen burner, Tarred watch glass, evaporating dish, iron clamp and stand, perforated filter paper, iron ring and wire gauze.

The first step in sublimation is to place five grams of the impure benzoic acid in an evaporating dish. The evaporating dish is then covered with perforated filter paper and topped with the watch glass that is secured by a masking tape. A water moistened tissue paper is placed on top of the watch glass. The set-up is heated for 15 minutes or until the sample has completely vaporized. After heating, the set-up is cooled and inverted. Collect the sublimate in the watch glass and weigh. The percentage recovery is calculated using the formula:

wherein the sublimate and the benzoic acid start to melt and when they completely melt. Shown
Caution!
HOT OIL CAN CAUSE BURNS. USE A DRY BEAKER FOR THE OIL BATH.

figure one is the set-up for melting point determination

For the melting point determination, the materials to be used are: capillary tubes, rubber band, thermometer, and cooking oil. First and foremost close the ends of the capillary tubes, then grind the sublimate and insert the powders produced in a capillary tube; at least 3-5mm of the capillary tubes must be filled. Do the same procedure for the benzoic acid. Place the two capillary tubes in the thermometer by strapping them using the rubber bands. Immerse the tubes in an oil bath and heat. Stir the liquid constantly and take note of the temperature

Figure 1 Melting Point Determination Set-up

Results & Discussion The results of the experiment are divided into two parts, the sublimation and melting point determination results. The sublimate collected was weighed and the result was 4.5 grams of the initial 5 grams. Shown below is the calculation for the percentage recovery:

References The result of the computation showed that 90% of the impure benzoic acid was purified, and the remaining 10% were the impurities removed. The results for the melting point determination are tabulated in table 1.
Substance Sublimate Initial Melting Final Melting point point 120 135 123

[1] Bayquen, A.V., et.al. (2009). Laboratory Manual in Organic Chemistry. Manila: University of Santo Tomas pp. 37-39.

Benzoic Acid 117 (pure)

Table 1 Table for melting point determination

The results proved that there are still impurities in the sublimate because the range of the initial temperature from the final melting point which is 120-135 has a large range or difference unlike the pure benzoic acid which has a short range of 117-123. Do take note that the melting point of benzoic acid which is 122 C which was far from the final melting point of the sublimate. Below are the computations for the differences of the melting point:

Sublimate: 135-120= 15 Benzoic Acid: 123-117= 6