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SUBLIMATION AND MELTING POINT DETERMINATION

Carina Lyn D. Batol, Karen Rachel Joyce A. Birol, Alfonso Pio P. Calimag, Justin L. Canasa, Red Aian N. Caragdag Group 3 2A Medical Technology Organic Chemistry Laboratory

ABSTRACT
The compound used in the experiment was impure benzoic acid. After undergoing a heating process, sublimate was produced in the form of crystals. From the initial 5.00g of impure benzoic acid, only 0.100 sublimate was collected, indicating only a 2.00% recovery of the compound. The melting point of the sublimate was determined by subjecting it to an oil bath along side the sample of pure benzoic acid. The procedure showed that on the one hand, the impure benzoic acid sublimate started melting at 116 C and ended at 120 C, while on the other hand, the pure benzoic acid sample started melting at 120 C and ended at 123 C. The results of the boiling point determination indicate that the pure benzoic acid has a higher vapor pressure than the sublimate, likewise giving it a higher melting point.

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. [2] The vaporizationsolidification cycle, which is the sublimation process, used in the experiment is utilized in the purification of the impure benzoic acid. [1] The objectives of this experiment are: (1) to purify the benzoic acid sample through sublimation, (2) to determine and compare the melting point of the product with a standard, and (3) to calculate the percatage recovery of the compound after the procedure. perforated filter paper, masking tape, a hot plate for heating, and tissue paper. This set-up was used for the purification of the impure benzoic acid. The sample of the impure benzoic acid was placed in the evaporating dish, which was then sealed with the perforated filter paper secured by masking tape. The pre-weighed watch glass was then placed atop the evaporating dish invertedly for collection after sublimation. During heating on the hot plate, a piece of tissue paper placed on top of the inverted watch glass was continuously moistened for 10-15 minutes. After heating, the set-up was cooled. The watch glass was then carefully put upright to collect the crystalline like sublimate, along with the sublimate left on the perforated filter paper. The pre-weighed watch glass containing the collected sublimate was again weighed and the mass of the sublimate was calculated. From this result the percentage recovery was also calculated. 2. Melting Point Determination The 0.100g sublimate of the impure benzoic acid was then placed into a 3-5mm capillary tube. To make sure it was well-packed; the capillary tube was dropped down through glass tubing repeatedly. In the same manner, the pure benzoic acid sample was also placed in a 3-5mm capillary tube. The closed end of the capillary

EXPERIMENTAL
A. Compound/s Tested The compounds tested were impure benzoic acid, impure benzoic acid sublimate, and pure benzoic acid sample. B. Procedure 1. Sublimation The sublimation set-up was comprised of an evaporating dish, a pre-weighed watch glass,

tubes were attached parallel the mercury bulb of the thermometer with the use of a thread or a rubber band. The thermometer was then immersed into an oil bath and then heated. The oil bath was stirred constantly during heating. The temperatures in which the samples started melting, as well the temperatures they completely melted were noted. These temperatures for the sublimate and the pure benzoic acid sample were recorded separately.

determine the boiling point. The medium used for this was an oil bath. An oil bath was used because, unlike a water bath, it is able to provide a temperature higher than 100 C and also of its generally greater boiling point from water.

Thermometer

RESULTS AND DISCUSSION


The process of sublimation was used to purify the impure benzoic acid. The impure benzoic acid sample was put into a watch glass covered with perforated filter paper. The set-up was then heated to obtain a product, which was the sublimate. The weight of the sublimate (0.100g) was then used to calculate the percentage recovery.

Capillary tubes containing samples

Oil bath

Bunsen burner

Figure 3. Melting Point Determination Setup The melting point of a substance is the temperature in which it changes from a solid state to a liquid state. Impurities in a substance can cause a distinct change in its melting point. That is why determining a substances melting point is essential in this experiment because the substances used were that of a pure sample and an impure one. Table 1. Data
Weight of impure benzoic acid Weight of watch glass + sublimate
Evaporating dish Hot Plate

Figure 1. Percentage Recovery Calculation

5.00g 61.1g 61.0g 0.100g 2.00% T1= 116 C T1= 120 C T2=120 C T2=123 C

Inverted Pre-weighed Watch Glass

Weight of empty watch glass Weight of sublimate Percentage Recovery Melting Point of Benzoic Acid Sublimate Melting Point of Pure Benzoic Acid

Figure 2. Sublimation Set-up The sublimate was then grounded with the use of the mortar and pestle. This is done in order to

The melting point of the impure benzoic acid sublimate was considerably lower than that of the pure benzoic acid sample. The sublimate started melting at 116 C and ended at 120 C, while on the other hand, the pure benzoic acid sample started melting at 120 C and ended at 123 C. The results of the boiling point determination indicate that the pure benzoic acid has a higher vapor pressure than the sublimate, likewise giving it a higher melting point.

REFERENCES
[1] Bayquen, A.V., Cruz, C.T., de Guia,R.M, Lampa, F.F., Pea, G.T., Sarile, A.S.and Torres, P.C. (2009),Laboratory Manual inOrganic Chemistry,C&E Publishing, Inc [2]http://www.lenntech.com/chemistry/sublimati on.htm Date: July 23, 2012

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