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Exp 3 Formal Lab Report

The document summarizes an experiment to purify benzoic acid through sublimation and determine its melting point. 5 grams of impure benzoic acid was sublimated, collecting 0.51 grams of sublimate, for a 10.2% recovery. The sublimate's melting point range was 118-121°C, and pure benzoic acid's was 113-120°C. While sublimation can purify compounds, limitations meant the sublimate and benzoic acid still contained impurities, shown by their melting point ranges exceeding the 1-2°C of a pure substance.

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Romulo Vincent Perez
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2K views3 pages

Exp 3 Formal Lab Report

The document summarizes an experiment to purify benzoic acid through sublimation and determine its melting point. 5 grams of impure benzoic acid was sublimated, collecting 0.51 grams of sublimate, for a 10.2% recovery. The sublimate's melting point range was 118-121°C, and pure benzoic acid's was 113-120°C. While sublimation can purify compounds, limitations meant the sublimate and benzoic acid still contained impurities, shown by their melting point ranges exceeding the 1-2°C of a pure substance.

Uploaded by

Romulo Vincent Perez
Copyright
© Attribution Non-Commercial (BY-NC)
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SUBLIMATION AND MELTING POINT DETERMINATION OF BENZOIC ACID

Dianne I. Pascua, Francesca F. Perez, Romulo Vincent S. Perez, Lia S. Priela and Zeth Raquedan Group 8 2C Medical Technology Organic Chemistry Laboratory

ABSTRACT
5.00 grams of impure benzoic acid was used in the sublimation and determination of melting point. The sample was heated for 10 minutes then the sublimate was collected and weighed. The sublimate weighed 0.51 grams with which the percentage recovery was 10.2%. The sublimate was then placed into a capillary tube together with another tube that contained pure benzoic acid to serve as the standard. Both of the capillary tubes were heated in an oil bath where the initial and final temperatures of their respective melting points were noted. The sublimate had a melting point range of 118-121C and the pure benzoic acid had a melting point range of 113-120C.

INTRODUCTION
Sublimation is a phase transition process from a solid to a gas without ever entering an intermediate liquid phase. It is adopted as a technique for purification of solids because: the loss of product is typically minimal compared to other techniques; it is more appropriate for any heat sensitive compound; and solvents are not involed in the process unlike recrystallization. A melting point is the temperature at which a solid or liquid form 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 will then convert the solid into a liquid with no temperature change. The melting temperature of crystalline solids is a characteristic figure and is used to identify pure compounds and elements. Most mixtures and amorphous solids melt over a range of temperatures. The objectives of the study were: (1) to purify benzoic acid by sublimation, (2) to determine and compare the melting point of the product with the standard, and (3) to calculate the percentage recovery. 2. Melting point determination of benzoic acid The sublimate was ground into fine powder and placed inside a capillary tube. It was ensured that the sublimate in the tube was well-packed by dropping the closed end of the tube down through a glass tubing several times. The same was done with a capillary tube containing pure benzoic which served as the standard. Both capillary tubes were then attached to a thermometer with a piece of rubber band. The closed ends of the tubes were aligned with the mercury bulb of the thermometer. The thermometer along with the two capillary tubes were immersed in an oil bath which was stirred constantly. The temperature at which the sublimate and the pure benzoic acid started and completely melted were noted.

EXPERIMENTAL
A. Compounds Tested (or Samples used) Impure benzoic acid, pure benzoic acid, cooking oil B. Procedure 1. Sublimation of benzoic acid 5.00 grams of impure benzoic acid was placed in an evaporating dish covered with a perforated filter paper. A pre-weighed watchglass was then placed on top of the filter paper. The evaporated dish was then heated for 10 minutes, allowing the sample to undergo sublimation. To collect the sublimate, the pre-weighed watchglass was inverted. The sublimate was then weighed and the percentage recovery calculated.

Figure 1. The sublimate

Figure 2. The melting point set-up

RESULTS AND DISCUSSION


The weight of the sublimate collected was 0.51 grams. In order to obtain the percentage recovery, the following equation was used

point of 121-123C was not observed. The pure benzoic acid had a melting point range of 113120C. It could not also be considered as a pure substance because the melting point range has a difference of 7C. This was caused by the impurities in the environment which contaminated the pure benzoic acid. The impurities cause the melting point range to lower and to broaden. They disrupt the consistency and organization of the crystal lattice at the molecular level. The contaminants do not fit correctly into what would be the normal pure lattice. This disruption weakens the lattice making it easier to be broken. The weakened structure melts more easily at reduced temperatures. The disruption also causes non-uniformity at the molecular level, the molecules closest to the impurities melt the fastest while those further away where the crystal lattice is relatively undisturbed melts at or nearer the normal range. The limitations of sublimation is that it requires a vacuum to be more effective, the compound must be able to undergo sublimation, only a few compounds undergo sublimation and it requires that the compound should be volatile while the impurities are nonvolatile. Other methods for determining the melting point of substances include the Mel-Temp Melting Point Apparatus which uses long, thin meltingpoint capillaries and the Fisher-Johns Melting Point Apparatus which uses small round, glass coverslips.

Of the 5.00 grams of benzoic acid sublimated, only 0.51 grams or 10.2% of the substance was recovered. This may be due to the limitations of the sublimation technique. For a higher percentage recovery, sublimation must happen in a vacuum for reduced pressure. Sublimation is not as selective as recrystallization and requires that the compound should be volatile while the impurities be nonvolatile. Table 1 The initial and final melting points of the sublimate and the pure benzoic acid
TI Sublimate Pure benzoic acid 118C 113C TF 121C 120C

CONCLUSION
Based on the results, sublimation can be used as a technique for purification. However, due to its limitations like only a few substances sublime, other purification techniques may be more efficient. In the determination of the melting points of the sublimate and the pure benzoic acid, the theoretical melting point was not observed because the sublimate and the pure benzoic acid still contained impurities.

Table 1 shows the melting point range of the sublimate and the pure benzoic acid. The sublimate initially melted at a temperature of 118C and completely melted at a temperature of 121C. The pure benzoic acid initially melted at a temperature of 113C and completely melted at a temperature of 120C. In order to be considered as a pure substance, the melting point range of the sublimate should only have a difference of 1-2C. Since the difference was 3C, the sublimate was still impure and contained impurities. Because of the impurities still found in the sublimate, the standard melting

REFERENCES
1. Bayquen, A. V., Cruz, C. T., De Guia, R. M., Lampa, F. F., Pea, G. T., Sarile, A. S., & Torres, P. C. (2009). Sublimation and Melting Point Determination. In Laboratory Manual in Organic Chemistry (pp. 37-39). Quezon City, Philippines: C & E Publishing, Inc.

2. Chemistry Online @ UTSC. (n.d.). Retrieved July 27, 2013, from http://webapps.utsc.utoronto.ca/chemistr yonline/sublimation.php 3. Craine, L. E., Hart, D. J., Hart, H., & Vinod, T. K. (2012). Organic Chemistry: A Short Course (13th ed.). Boston, Massachussets: Houghton-Miflin. 4. Fisher-Johns Melting Point Apparatus. (2013, May 13). Retrieved July 27, 2013, from http://orgchem.colorado.edu/Technique/P rocedures/Meltingpt/FisherJohns.html 5. Mel-Temp Melting Point Apparatus. (2013, May 13). Retrieved July 27, 2013, from http://orgchem.colorado.edu/Technique/P rocedures/Meltingpt/Mel-Temp.html 6. melting point (chemistry) -- Encyclopedia Britannica. (n.d.). Retrieved July 27, 2013, from http://global.britannica.com/ EBchecked/topic/374185/melting-point

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