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Experiment 3-Sublimation and Melting Point Determination

Experiment 3-Sublimation and Melting Point Determination

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Published by: Emilyn Millares on Sep 20, 2011
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SUBLIMATION AND MELTING POINT DETERMINATION Margarita Ysabel S. Mangahas, Cara Camille M. Matute, Emilyn D.

Millares, John Acener C. Padua and Kathryn Cheshire P. Pangilinan Group 5 2A Medical Technology Organic Chemistry Laboratory ABSTRACT
In this experiment, sublimation was used to purify solid mixtures. The compound used to undergo purification is impure benzoic acid. The product obtained after the heating process is called the sublimate in the form of crystals. The weight of the impure benzoic acid gave a lot of difference from the sublimate obtained from 5.0014 g to 0.3213 g, respectively. Thus, the measured sublimate showed the low percentage recovery of the said compound. The sublimate was then subjected to melting point determination together with the pure benzoic acid through the oil bath. The oil bath was used since it is able to measure temperatures even those beyond 100 °C and are highly recommendable for compounds which have higher boiling points. As it was seen in the results for the melting point determination, the sublimate started to melt at 116 °C and stopped melting at 120 °C while the pure benzoic acid started to melt at 120 °C and ended at 121 °C. The temperatures measured indicated that the pure benzoic acid has a higher vapour pressure than the sublimate.

Sublimation is the direct vaporization of a solid by heating without passing through the liquid state. [1] The process of sublimation in this experiment is used to purify the impure benzoic acid. The impurities in the benzoic acid have amino compounds that are present in a larger extent and must be removed because of phenyl and benzyl compounds that seriously affect the product.[3] This process occurs if the vapour pressure of the substances greater than the atmospheric pressure at the melting point.[2] The process of purification involved in sublimation is applicable for impurities which are non-volatile or with lower vapor pressure than the pure compound or substance. The objectives of this experiment are: (1) to purify the impure benzoic acid through sublimation, (2) to calculate the percentage recovery of the benzoic acid after sublimation, and (3) to identify the melting points of the sublimate and the pure benzoic acid through the use of an oil bath.

extent because of the presence of hydrogenous compounds. [3]

B. Procedure 1. Sublimation
Sublimation set-up was used to purify the impure benzoic acid. Hot plate, evaporating dish, 5 g of impure benzoic acid, clean sheet of bond paper to cover and masking tape for sealing, watch glass, and moistened tissue paper were needed as materials. 5 g of impure benzoic acid was put into the evaporating dish and sealed with a clean sheet of bond paper with holes on it using a masking tape. Before putting the evaporating dish on the hot plate, a pre-weighed watch glass was set on the dish invertedly. While heating, the tissue paper was put above the watch glass and continuously moistened for 10-15 minutes until most of the sample has vaporized. The set-up was cooled and then the watch glass was carefully inverted to collect the sublimate in a transparent, crystalline, needle-like appearance. The sublimate was weighed for percentage recovery.

2. Melting Point Determination EXPERIMENTAL A. Sample Used
The samples used in the experiment were impure benzoic acid, its sublimate and the pure benzoic acid. The impure benzoic acid is said to be non-volatile meaning it has a lower vapor pressure than the pure compound. The impurities found in formed benzene affect it to quite a large The 0.3213 g of sublimate collected was ground with the mortar and pestle. The sublimate’s powdered form was well-packed into 3-5 mm capillary tube. The pure benzoic acid followed the same procedure separately with the sublimate. The capillary tubes were dropped into the glass tubing to get rid of air spaces when if present could affect the melting point of the compound. The closed ends of the capillary tubes

Table 1. The oil bath is a laboratory heating device which uses boiling oil as the temperature regulator. The impure benzoic acid is also said to have lower vapour pressure than the pure ones. [6] Stirring Rod Thermometer RESULTS AND DISCUSSION Sublimation was the process used in the experiment. [7] Determining the melting point is a simple and fast method used in many diverse areas of chemistry to obtain a first impression of the purity of a substance. it showed how sublimation affected the weight of the impure benzoic acid until it became a sublimate. Melting Point Determination set-up The melting point determination is the temperature at which the material changes from a solid to its liquid state. rubber band or copper wire.[5] It operates the same principle as water bath but oil Through the data obtained from the experiment. the tubes were immersed in an oil bath while being heated. The tubes are aligned with the mercury bulb of the thermometer.0014 g to 0. After attaching. or at least clearly enlarge its melting range.7262 g 3. It was noticed that during the process of sublimation the impure benzoic acid did not pass through the liquid phase.42 % 120 °C – 121 °C 116 °C – 120 °C Evaporating dish Hot plate Watch Glass with Moistened Tissue Paper Weight of the sublimate Percentage Recovery Melting Point of the pure benzoic acid Melting point of the sublimate Figure 1. Data Weight of the impure benzoic acid Weight of the watch glass + sublimate Weight of the watch glass (empty) 5.3213 g) showed the turning point of the where in the impure benzoic acid is to its .were attached to a thermometer with a thread.4049 g 0. The temperatures at which the sublimate and pure benzoic acid started melting as well as the temperature at which they were completely melted were both noted. The oil bath is stirred constantly. Sublimation set-up The sublimate collected was ground to be able to determine its melting point through the capillary tube method with the use of oil bath. The melting point determination in this experiment was done through the oil bath. The impure benzoic acid in the evaporating dish has to be heated to be able to form needle-like crystals which will eventually be called the sublimate.0014 g 3. The sublimate that passed through the holes of the paper used as its covering is to be collected to know its percentage recovery. This is because even small quantities of impurities change the melting point. The change in weight (from 5. The reason for is that because the benzoic acid has non-volatile impurities. has generally far higher boiling points than water and can be used to provide temperature greater than 100 °C.3213 g 6. Oil Bath Capillary Tube with the Sublimate Bunsen burner Capillary Tube with Pure Benzoic Acid Figure 2.

org/view/Oil_Bath Feb 3 2011 http://www. A. Oil Oil Bath as a Laboratory Bath. G.scribd. Lampa.chemicool.M. pp 74-82 Impure Benzoic Acid. http://www. (2006). The Essentials of Organic Chemistry. (2009).C&E Publishing. Pearson Education.S.html#ixzz1TsXTSUBZ.. Inc.biologyonline. Sublimation. and Torres. http://www.com/doc/48324739/meltingpoint-determination. It has a smaller dipole moment meaning the higher vapour pressure due to lower electrostatic attractive forces in the form of crystals. The pure benzoic acid has a high vapour pressure which made it melt in a higher temperature rather than the sublimate. A. . Technique. R.org/dictionary/Oil_bath.com/about_6629946_impurebenzoic-acid_.C. June 14 2007. F.V..gaseous state. Meting Point Determination. P. http://www.Laboratory Manual in Organic Chemistry. Inc Bruice.T. Peña. Sarile.html. Y.com/definition/sublimation .ehow.T. 1st Edition. P.F. http://www. de Guia. 2008. Cruz. C. 2010.homechemistry. March 2009...[1] REFERENCES Bayguen.


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