SUBLIMATION AND MELTING POINT DETERMINATION Meah G. Pacheco, Paola Louise R. Palma, Fleur Jeizl P.

Perez, Maria Godesa F. Refuerzo and Michelle Nhat Ly T. Reyes Group 6 2F-Pharmacy Organic Chemistry Laboratory ABSTRACT
The experiment was conducted by sublimation and melting point determination or analysis using pure and impure benzoic acid. The set-up consists of two major steps subliming the impure benzoic acid and comparing the melting point of both pure and the extracted impure benzoic acid in a melting point set-up by using cooking oil as the medium of heat transfer. With this experiment, the melting point differences of pure and impure crystals of benzoic acid were actuated, having 2C difference in melting point. The lone powdered impure benzoic acid reacted with the heat on the hot plate, as it sublimated on top of the filter paper covered with moistened watch glass, weighing 2 grams of sublimate produced, were also observed, as well as the changes in impure benzoic acid before and after sublimating when it comes to its physical appearance, which could be noted as film-like colorless strips of crystals. The percentage of recovery for the sublimate was also computed, having 40% of impure benzoic acid redeemed in the sublimation process.

INTRODUCTION
Sublimation is the process of vaporizing a solid substance and condensing the vapors to again form the solid directly, without passing through an intermediate liquid state. There are very few substances which vaporize without melting, but in all cases of sublimation, the change from the vapor to the solid state, is direct, and without any formation of liquid.[3] Melting point is the temperature at which the solid and liquid forms of a pure substance can exist in equilibrium. As heat is applied to a solid, its temperature will increase until the melting point is reached. More heat then will convert the solid into a liquid with no temperature change. [2] The objective of the experiment is to discern the process of sublimation and recrystallizing the substrate. Difference between physical property differences are also distinguished between phases. Another objective is to measure the melting points of a substrate according to its purity, and to identify its differences with each other. B. Procedure 1. Benzoic Acid Sublimation and Recrystallization

EXPERIMENTAL
A. Compound tested and samples used Benzoic acid The substrate used was benzoic acid, also known as carboxybenzene, an aromatic carboxylic acid. It is also known in the industry as a food preservative and can undergo reactions such as sulfonation, nitration and halogenation.[1] In this experiment, sublimation and melting properties of benzoic acid was inspected. Three kinds or forms of benzoic acid were used in the process, namely impure benzoic acid, the sublimate of the impure benzoic acid, and the pure benzoic acid. Figure 1. Sublimation set-up All the necessary apparatus were prepared. The triturated impure benzoic acid was placed in a weighted evaporating dish, weighted again, and was sealed with perforated filter paper. A watch glass was placed on top for trapping of gas, and was covered with a cloth or tissue kept damp with water on top for condensation purposes. The set-up was heated on top of a hot plate for 10 to 15 minutes until most of the sample has vaporized. The set-up was allowed to let stand to

cool its surface, weighted for the last time, and was then again triturated for easy fixation in the capillary tube.

Figure 2. Recovered sublimate of impure benzoic acid 2. Benzoic Acid Melting Point Analysis After the set-up of the sublimation and recrystallization, capillary tubes were prepared and heated to close one of its ends. Both pure and impure powders of benzoic acid were separately placed in capillary tubes, and tying it on both sides of a thermometer. Clamps and stands were placed accordingly, holding the thermometer upright. For heating purposes, cooking oil was poured in a beaker, making it the medium for heat transfer since cooking oil can tolerate more heat in boiling than water. Bunsen burner was the source of heat in the set-up, to control the flame produced. The thermometer, along with the capillary tubes was immersed in the cooking oil being heated on the Bunsen burner. To maximize heating, a circular copper stirrer was used. The initial melting temperature was marked by the time the substrate becomes translucent. On the final temperature of each sample, a clear liquid should be obtained to be completely melted.

Figure 3. Melting point set-up

RESULTS AND DISCUSSION

1. Recovery of recrystallized benzoic acid The sublimate was instantaneously condensed because of the tissue that was kept damp with water on top of the watch glass covering. The sublimate came back to its original crystal form which resembles thin, elongated plastic strips. In this part of the experiment conducted, the benzoic acid, which is a solid, went through a direct transition to a gaseous state. By skipping the transition of the solid melting to liquid, a certain amount of substance can be recovered in condensing crystals. From the data gathered, the watch glass alone weighted 101 grams and 5 grams of impure benzoic acid was required. At the end

of the heating, only 103 grams, sublimate and watch glass together, was obtained. Table 1. Weight of sublimate before and after processing. Weight of watchglass with sublimate 106 103 Weight of sublimate 5 2

REFERENCES
[1] Dadachanji, D. Chemical Properties of Benzoic Acid. Demand Media.

http://classroom.synonym.com/chemical-propertiesbenzoic-acid-2721.html
[2] Encyclopdia Britannica. Melting Point. http://global.britannica.com/EBchecked/topic/37 4185/melting-point [3] Lenntech Water Treatment Soultions Sublimation. http://www.lenntech.com/chemistry/sublimation. htm#ixzz2ZxyeioWC

Before After Computation:

Weight of sublimate weight of impure benzoic acid x 100 = percentage of recovery 2 grams 5 grams x 100 = 40 40% %

The total weight of the substance recovered was divided to the total weight of the sample that was sublimated. 1. Differentiation of substrates using melting point Table 2. Melting point measurements.

[4] McGregor, M. The University of Rhode Island Chemistry Department. Using Melting Point to Determine Purity of Crystalline Solids. http://www.chm.uri.edu/mmcgregor/chm228/use _of_melting_point_apparatus.pdf

Initial Final

Sublimate 114C 116C

Pure 116C 118C

In the melting point set-up, the initial temperature was 66C. The sublimate started melting at 114C, having a translucent appearance, and became completely melted by 116C; while the pure benzoic acid started melting at 116C and appeared as clear liquid at 118C. Both samples have 2C intervals for the start and end of their melting. In the experiment, different melting points were the result because of the chemicals purity.[4] Because the impurity causes defects in the crystalline lattice, it is easier to overcome the intermolecular interactions between the molecules.