Abstract:Experiments with the recrystallization of benzoic acid and salicylic acid have been carried out. The recrystallization process depends on the various solubilities of solutes in a solvent to purify solid organic compounds. Recrystallization is used to purify solid compounds, where product purification may remove by-products and contaminants. Benzoic acid and salicylic acid were dissolved in a solvent (distilled water) and then thoroughly dissolved using a hot plate. The solutions and crystals are obtained after an ice bath. The formed crystals were used to calculate the percentage of crystal recovery. Benzoic acid and salicylic acid had recovery rates of 125% and 136%, respectively.As a result, the recovery rate is over than 100%. It is possible that the crystals contain moisture from water that did not filter well during the filtration process, and that the crystals did not dry in an oven, which can also affect the water contained in the crystal.
Recrystallization is the most common method of purifying nonvolatile organic solids. Recrystallization entails dissolving the material to be purified (the solute) in a suitable hot solvent. As the solvent cools, the solution becomes saturated with the solute, and the solute crystallises out (reforms a solid). Impurities are excluded from the crystal lattice as it develops, completing the purification process. The crystals can then be collected, washed, and dried. The attractive forces that hold solute molecules to other solute molecules (typically Van der Waals interactions) are overcome during the recrystallization process. Recrystallization does not involve the breaking of any chemical bonds.
A successful recrystallization is dependent on the solvent used. When the compound is hot, it must be soluble in the hot solvent but insoluble in the cold solvent. The greater the difference between hot and cold solubility when selecting a solvent, the more product recoverable after recrystallization. The pace of cooling determines the size and quality of the crystals: rapid cooling favours the creation of small crystals, whereas gradual cooling favours the growth of large, generally purer crystals. To be easily removed from the pure crystals, a suitable recrystallization solvent should be somewhat volatile.Aside from that, the solvent should not react with the compound being purified and its boiling point should be lower than the melting point of the compound being purified because solid melts before it dissolves.
The primary precursors of this experiment are benzoic acid and salicylic acid; the acids solute were prepared by a lab assistant at Makmal Gunasama Kimia 3. Makmal Biologi Struktur Dan Fungsi supplied distilled water, which was placed in a tank. Ice was made the day before the experiment by a lab assistant.
Benzoic acid was weighed out at around 1.00g using an analytical balance and transferred to a 125mL conical flask. 20mL of distilled water was measured with a measuring cylinder before being poured to a conical flask. The solution was properly stirred until the acid was dissolved. The solution was then heated on a hot plate until the benzoic acid was completely dissolved; while heating, 3 grains of boiling stones were added to the conical flask. After removing the flask from the hot plate, the solution was left to cool for 5 minutes before being placed in an ice bath for 15 minutes.
The conical flask was taken from the ice bath after 15 minutes. The solution was put into the Büchner funnel, and the filtration process was begun by turning on the vacuum pump. The flask was rinsed with 5mL distilled water before being poured back into the Buchner funnel. The pump was turned on for a few minutes to finish the filtration process. The crystals formed on filter paper. Crystals were let to dry in room temperature air for 15 minutes. By swapping salicylic acid for benzoic acid, all processes were repeated.
Before filtering, the filter paper was weighted. After the crystals formed on the filter paper, the weight of the filter paper and crystals was recorded.
Using a formula to calculate the percentage of crystal recovery
According to the table, the calculated %recovery for Benzoic acid and Salicylic acid is greater than 100% because the crystals of Benzoic acid and Salicylic acid may contain moisture from water that did not filter properly during the filtration crystal. Furthermore, the filtration process could not remove the water contained in the crystal well and it still had moisture of water because the method should be oven to dry well the crystal to get the %recovery more accurate and lower 100%.
Suction filtration is preferred over gravity filtration in this experiment because it is significantly faster, typically taking less than a minute with correct seals and a good vacuum source. Suction filtering is more effective in removing residual liquid, yielding a purer solid. Suction filtration is preferred when the solid is retained since gravity filtration is significantly less successful in eliminating remaining liquid from the solid on the filter paper.
Boiling stones, also known as boiling chips, are small particles of inert substance added to certain liquids to help them boil more slowly. In this experiment, boiling stones were used while heating the solution and it cannot be reused because their crevices become saturated with solvent after only one use and can no longer generate bubbles.
The solution was left to cool before being placed in the ice bath because rapid cooling of the solution before it can cool to room temperature results in the rapid precipitation of a solid with trapped impurities that have no chance of escaping, whereas slow cooling of the saturated solution promotes the formation and filtration of pure crystals while the impurities remain dissolved.
Recrystallization is a method used to purify a solid organic material. This method cleans organic compounds of soluble and insoluble contaminants. Because the contaminants are still soluble in cold conditions, the soluble impurities are filtered out of the filtration process based on this experiment. The experiment had unsatisfactory results, with benzoic acid recovering 124.80% and salicylic acid recovering 136.04%.Both outcomes are higher than 100%. One possible reason for the unsatisfactory results is that the filtration process did not vacuum well enough and the crystal did not dry completely.
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