Sublimation and Boiling Point determination of Impure Benzoic Acid Lazatin, V.D.; Lopez, A.T.; *Maningas, S.R.

; Martin, R.J.; Medina, P.C. 2B-MT

Impure benzoic acid was purified through the process of sublimation. Five grams of impure benzoic acid was purified. Sublimate collected was subjected to a calculation of percentage recovery. Sublimate was ground to fine powder, packed in a capillary tube and melting point was determined, and was compared with a standard.

Introduction
Some solids can easily change into vapours (volatilisation); these vapours (instead of condensing into a liquid and the liquid freezing back to the solid) can sublime, that is, the vapours form a solid without going through the liquid state. This process occurs if the vapour pressure of a substance is greater than the atmospheric pressure at the melting point. Since the vapour can solidify, the vaporization-solidification cycle can be used as purification process. Sublimation, therefore, can be used as a technique to purify solid mixtures. However, purification can only be done if the impurities are nonvolatile or have a significantly lower vapour pressure than the pure compound. The objective is to purify benzoic acid through sublimation, and to determine its melting point.

was placed on top(figure 1). The set-up was heated using a hot plate for 12 minutes. The set-up was set to cool, and the watch glass was carefully inverted, collecting the sublimate to the pre-weighed watch glass, the watch glass was weighed again with the crystals.

Figure 1
The crystals were collected in a mortar. The crystals were grinded into fine powder and packed in a capillary tube. After packing, the capillary tubes were attached to a thermometer, the closed end aligned with the mercury bulb. The thermometer, together with the capillary tubes containing the pure benzoic acid and sublimate were immersed in an oil bath(figure 2).

Methodology
The group weighed 5 grams of impure benzoic acid. The sample was placed in an evaporating dish, covered with perforated filter paper. An inverted, preweighed watch glass with moistened tissue

Melting Points Temp. 1 122C Pure benzoic 114C Sublimate

acid

Temp. 2 127C 118C

Figure 5 Discussion
After performing the sublimation procedure, the impure benzoic acid was successfully purified, giving a weight of 0.3249g. Recovery of the benzoic acid was computed at 6.49% by dividing the weight of sublimate by the weight of the impure benzoic acid used, then multiplied to 100. This means that only 6.49% of the sample was recovered. Immersion of the sample and a standard to an oil bath determined the melting point of the sample, an oil bath was used because of its higher boiling point. The standard benzoic acid started melting at 114C and was fully melted at 118C, while the sublimate collected started melting at 122C and was fully melted at 127C. Difference in melting point of the two substances indicate that the sample is not purified well.

Figure 2 Results Data Obtained

Weight of Impure Benzoic Acid

5.0043g

Weight of watch 94.6227g glass + sublimate Weight of watch 94.2918g glass(empty) Weight of 0.3249g sublimate Percentage 6.49% recovery Melting point of 122C-127C benzoic acid Figure 3
    

References (1) http://www.scribd.com/doc/67799 99/07-Sublimation (2) http://en.wikipedia.org/wiki/Subli mation_%28phase_transition%29

Description of Sublimate Appearance Color Shape Figure 4 Crystal like White Stellate