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SUBLIMATION AND MELTING POINT DETERMINATION

Lorraine M. Ramos, Sharmaine Michelle M. Reyes, Rhone Arevyn E. Roque Joseph T. Sabido and Jan Armelynn S. Santos Group 7 2A Medical Technology Organic Chemistry Laboratory

ABSTRACT
The experiment is to understand the process of sublimation as a technique used to purify solid mixtures by which a substance undergoes conversion from the solid phase to the gas phase, without going through an intermediate liquid phase and the used of melting point determination to ascertain the identity and purity of an unknown compound. Heated using a hot plate was a 5g of impure benzoic acid that was placed in an evaporating dish covered with a perforated filter paper and inverted pre-weighted watch glass. The center top of the watch glass was cooled by placing a tissue paper kept moist with water; this took 10-15 minutes until most of the sample had vaporized. The sublimate was collected and weighed from the pre-weighed watch glass; through which the percentage recovery was calculated. The sublimate was grinded into a fine powder and the open end of a capillary tube was pressed to it for melting point determination. The closed end of the capillary tube was dropped down through glass tubing several times until it was packed with 3-5 mm of the sublimate. This was attached to a thermometer together with another capillary tube with pure benzoic acid tied using a copper wire and was immersed in an oil bath and heated. The pure benzoic acid was recorded to have 124C and the purified sublimate have 125C which was computed to have only 1C difference stating the impurities of the sublimate. Therefore, there is less impurity.

INTRODUCTION
Benzoic acid, C6H5COOH, is a crystalline organic compound with a white color and the simplest aromatic carboxylic acid. It has slight solubility in water and soluble in ethanol. Its melting point is at 122C and boiling point at 249 C. It has a specific gravity of 1.321. It can be acquired naturally from many plants and resins and is converted to its salts and esters for the use of preservative applications in foods, drugs and personal products. [1] The compound must be subjected to the process of sublimation by which it undergoes conversion from the solid phase to the gas phase, without going through an intermediate liquid phase. This process occurs if the vapor pressure of a substance is greater than the atmospheric pressure at the melting point. [2] The vapor on cooling, gives crystals of the pure solid compound. The crystalline material obtained is called sublimate. [3] Sublimation is a technique used by chemists to purify compounds. The solid volatilizes and condenses as a purified compound on a cooled surface, leaving the non-volatile impurities behind. [2] The sublimate is then subjected to melting point determination, which can be defined as the temperature range at which a crystalline solid changes into a liquid. To obtain the melting point of a compound, a small sample is slowly heated. The sample is carefully observed in a small tube usually and the temperature at which liquid is first observed is noted. When the entire solid has liquefied, this temperature is noted as well. In most instances a sample will melt over a small range of temperature. Thus the temperature at which the liquid is first observed until the solid is

totally liquefied is referred to as the melting point range. Consequently, the melting point range of a compound can be an indication of purity. [4] The experiment is inclined to attain the following objectives: (1) to purify the benzoic acid using the process of sublimation, (2) to determine and compare the melting point of the product with a standard and (3) to calculate the percentage recovery. [5]

EXPERIMENTAL
A. Samples used Impure benzoic acid Amount: 5g B. Procedure 1. Sublimation The setup for the experiment was made by placing 5g of impure benzoic acid in an evaporating dish covered with a perforated filtered paper. An inverted pre-weighed watch glass with a tissue paper that was kept moist was placed on the top of the filter paper. The heating process was used to start the sublimation process for 10-15 minutes until most of the sample was vaporized. As seen in Figure 1.

Figure 1. Sublimation Set-up

2. Percentage Recovery The sublimate was then collected from the preweighed watch glass and perforated filter paper and weighed. The calculation of percentage recovery was then made. 3. Melting Point Determination A fine powder was made by grinding the sublimate, and was pressed to be inserted into the capillary tube. The glass tubing was used to provide a capillary tube well-packed with 3-5 mm of the sublimate. The capillary tube was attached into a thermometer with a copper wire. The process of melting point determination was made by immersing and heating the capillary tube in an oil bath. The temperature at which the sublimate starts to melt and when it is completely melted were recorded. See Figure 2.

Table 1. Data Experiment

Obtained

from

Sublimation 5.0906 g 4.6283 g 4.2643 g 0.3640 g 7.15 %

Impure Benzoic Acid Watch Glass + Sublimate Watch Glass (empty) Sublimate Percentage Recovery

The aforementioned experiment proves that sublimation is a phase transition that occurs at temperatures and pressures below what is called the "triple point" of the substance. The process is an endothermic changethat is, a change in which heat is absorbed by the system. The enthalpy of sublimation can be calculated as the enthalpy of fusion plus the enthalpy of vaporization.

Figure 3. An example of a phased diagram Furthermore, the process of sublimation based on the group observation is proven to occur if the vapor pressure of a substance is greater than the atmospheric pressure at the melting point. The vapor pressure increases by heating the evaporating dish, and then the compound starts to evaporate. It passes through the perforated filter paper and will be trapped on the inverted watch glass. The role of the moist tissue paper is to provide cool environment to be able to resolidify the vapour, thus, crystal formation has occurred as the purified compound. The overall vaporizations solidification cycle can be used as purification method. The impurities are the solids left behind in the evaporating dish. The purification, however, can be done only if the impurities are non-volatile or have significantly lower vapor pressure than the pure compound. Benzoic acid is a non-polar substance. Non-polar substances are symmetrical compounds having high melting points and high vapor pressure. Its high vapor pressure is due to its smaller dipole moment because of lower electrostatic attractive forces.

Figure 2. Melting point determination setup

RESULTS AND DISCUSSION


Table 1 shows the results obtained from the process of sublimation. The percentage recovery was acquired by dividing the weight of the sublimate acid by the weight of the impure benzoic acid. The answer is then multiplied by 100.

Table 2 shows the results obtained from the process of melting point determination. Table 2. Data Obtained for Melting Point Determination Experiment Sublimate Pure 125C 124C = 1C 124C 124C = 0 C

In this part of the experiment, melting point determination can be employed to ascertain the identity and purity of an unknown compound. Based on the observation of the group, the pure/standard benzoic acid completely melted at 124C while the purified sublimate melted at 125C. A 1C difference in melting point of the standard or the pure compound and then the purified compound should be expected. However, when impurities are present, the difference in melting point can be expected to be greater than 1C because impurities lower the melting point of a compound. The difference in melting point can also be an effect of the air pockets in the capillary tube. This is because the air pockets prevent the compound from uniform heating thus increasing its melting point. Therefore, the result of the melting point determination of the purified sublimate and pure/standard compound was acceptable to have less impurity because it was recorded to have a difference of 1C.

REFERENCES
[1] Industrial Chemistry. Benzoic Acid. http://chemicalland21.com/industrialchem/organi c/benzoic%20acid.htm 8/7/11. [2] New World Encyclopedia. Sublimation. http://www.newworldencyclopedia.org/entry/Sub limation_%28chemistry%29 8/7/11. [3] TutorVista. Sublimation. http://www.tutorvista.com/content/chemistry/ch emistry-iii/organic-compounds/sublimation.php 8/7/11. [4] Paar, L. et al. (2008). Organic Chemistry Laboratory Experiments for Organic Chemistry Laboratory. http://webcache.googleusercontent.com/search? q=cache:2LqimCkaFBYJ:cns.uni.edu/~manfredi/8 60-121/ORG%2520LAB%2520MAN%2520S08. pdf+sublimation+formal+report&hl=tl&gl=ph 8/7/11. [5] Bayquen, A. et al (2007). Laboratory Manual in Organic Chemistry. Quezon City: C&E Publishing, Inc.