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SUBLIMATION AND MELTING POINT DETERMINATION

Jiro A. Laxamana, John Patrick T. Lizarondo, Naim G. Macasalong, Don Gilson L. Maderaso, Xyza S. Malenab Group 4 2A-Medical Technology Organic Chemistry

ABSTRACT
The sample of Benzoic acid was purified through sublimation. This process occurs if the vapor pressure of a substance is greater than the atmospheric pressure. Since the vapor can solidify, vaporization-solidification cycle was used by the group as a purification process. The sublimate collected after solidification became colorless needle-like crystals. The melting point was determined through a set-up using an oil bath and a thermometer. The melting point of the sample, which was 122C, was close to the melting point of the standard, which was 124C.

INTRODUCTION

Sublimation is the process where some solids that can pass directly into the vapor phase without passing through the liquid phase. Since the vapor can solidify, the vaporizationsolidification process cycle can be used as a purification process. Sublimation, therefore, is a technique used to purify solid mixtures. The purities, however, can be done only if the impurities are non-volatile or have significantly lower vapor pressure than the pure compound. In this experiment sublimation was used as a purification process by the group. The melting point of the sample and the substance was determined by the group with the use of a set-up which is composed of a hot oil bath and a thermometer to measure the temperature of the substance when it begins to melt. The melting point of the sample compared to the standard is lower. The sample given was not that pure that is why the group needed to purify it through sublimation. The vapor collected was solidified and it turned into colorless needle-like crystals which were pulverized in order to be contained inside a capillary tube which would later be put in an oil bath to determine the melting point. In this experiment, the group should be able to attain the following objectives: (1) Purify benzoic acid by sublimation. (2) Determine and compare the melting point of the product with a standard. (3) Calculate the percentage recovery.

EXPERIMENTAL
A. Compounds Tested 5.0g Benzoic acid (impure) Benzoic acid (pure)

B. Procedure
1. Preparation of the capillary tube On one side of the capillary tube heat one end of the capillary tube using a Bunsen burner.

While heating one end of the capillary tube rotate it to make it even. Continue heating it until the other end of the capillary tube is totally closed. 2. Preparation of the hot oil bath set-up In a clean beaker put unused cooking oil about half-full. Place the beaker on top of a tripod with a wire-gauze and a Bunsen burner underneath it. Attach the thermometer in a clamp and submerge it with the capillary tubes in the oil bath. 3. Purification of the Benzoic acid Place 5.0g of impure benzoic acid in an evaporating dish. Cover the dish with a perforated filter paper. On top of the filter paper, an inverted pre-weighted watch glass should be placed. Heat the substance using a hot plate. 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. Stop heating and cool the set-up. Carefully invert the pre-weighted watch glass. Collect all the sublimate (including the crystals adhering to the perforated filter paper) in the pre-weighted watch glass and weigh. Calculate the percentage recovery. 4. Determining of Melting point For melting point determination, grind the sublimate into a fine powder. Press the open end of the capillary tube into the powder. 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. Attach the capillary tube to a thermometer with a piece of thread/rubber band. Align to the closed end of the capillary tube with the mercury bulb of the thermometer. Immerse the capillary tube in an oil bath and heat. Stir constantly. Take note of the temperature at which the sublimate starts to meld and when it is completely melted.

RESULTS AND DISCUSSION


After subjecting the substance to heating the vapor began to solidify and became crystalline in nature. The substance that was once amorphous when subjected to sublimation began to be a colorless needle-like crystal which was later on grinded to be able to allow it to be inserted to the capillary tubes. The 0.70g of the benzoic acid (sublimate) that was collected from the previous 5.0g of benzoic acid sample. The percentage recover of the benzoic acid in the substance is 14%. The grinded crystals were inserted to a capillary tube attached to the thermometer, which was later on subjected to a hot oil bath which was used to melt the substance together with the standard to be able to compare their melting points from each other. The standard began to melt at 124C and it became completely melted at 125C. The sample began to melt at 122C and it became completely melted at 123C. Therefore, one could conclude that the standard has a higher melting point compared to the sublimate which was acquired through sublimation.

Table 1. Data and results


Weight of Benzoic acid (impure) 5.00g

Weight of watch glass

4.15g

Weight of watch glass with the sublimate

4.85g

Weight of the sublimate

0.70g

Weight of the residue

4.31g

Percentage recovery

14%

Table 2. Melting points


Temperature 1 Sublimate 122C Temperature 2 123C

Standard

124C

125C

Figure 1. Purification of Benzoic acid through sublimation

Calculations: %recovery = = =

14%

REFERENCES
Pavia, D.L., Lampman, G.M. & Kriz, G.S. (2005). Introduction to organinc laboratory techniques: A small-scale approach (2nd ed.). Pacific Grove, CA: Thomson-Brook/Cole University of Colorado-Boulder, Department of Chemistry and Biochemistry. (2003). CU Boulder organic chemistry undergraduate courses lab techniques. Retrieved May 30,2007 from the University of Colorado website: http://orgchem.colorado.edu/hndbksupport/dist/h tml. University of Santo Tomas Department of Chemistry. (2006). Organic chemistry laboratory manual. Manila: Author.