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1. Objectives : To purify the naphthalene by recrystallization procedure and to determine the recovery percentage. 2.

Introductions: Recrystallization is an important method for the purification of solids. Recrystallization involves dissolving a solid in a solvent and crystallizing it again, taking the opportunity to discard impurities along the way. One normally chooses a solvent in which the solubility increases significantly with temperature. The solid is dissolved in a minimal amount of hot solvent, and the solution is filtered to remove insoluble impurities (e.g.other compounds, dust, etc). On cooling of the solution, the desired compound crystallizes, leaving soluble impurities in solution. Normally, one would like to recover the entire desired solid completely free of contaminants. Unfortunately, this is rarely possible. Usually, if most of the material is recovered, it is not very pure, and extremely pure material can be obtained only in low yield. The trick is to find the proper balance between yield and purity. 3. Apparatus: a) Bunsen burner b) Stirrer rod c) Beaker d) Naphthalene e) Ice bath f) Erlenmeyer Flask

g) Buchner funnel h) Filter paper i) Distilled water

4. Procedure: a) 2g of naphthalene is weigh and put into 120ml or 250 Erlenmeyer flask. b) 50ml of water is added into the flask and is stirred vigorously. c) Bunsen burner is used to heat the solution just to the boiling point and is stirred continuously until the naphthalene dissolves. d) The flask is placed in an ice bath for 5 minutes and is stirred occasionally. e) A properly fitted piece of filter paper is placed in Buchner funnel. All the holes are covered. The paper is wet thoroughly with deionized water from wash bottle and vanillin crystals are vacuum filtered. The flask is rinsed once or twice with 5 ml of ice-cooled water and this water is used to wash the crystals in the funnel. f) The crystals are empty onto a weighed piece of filter paper and then are placed in desk for drying

5. Result and discussion

a) Mass of naphthalene before recrystallization = 2.0 g b) Mass of filter paper. = 0.52 g c) Mass of naphthalene + filter paper after recrystallization = 2.0156 g = 2.0156 0.52 =1.50 g e) The percent recovery = X 100%

d) Mass of crude naphthalene after recrystallization

= 75% f) The total lost = 100% - 75% = 25%.

g) Why is the naphthalene solution cooled in ice bath before vacuum filtration? The naphthalene solution is placed in an ice bath to maximize the amount of solid that can precipitate from the solution. The recrystallized solid is then collected by vacuum filtration and washed with cold solvent.

h) How does the recrystallization procedure remove soluble impurities?

Soluble impurities are the easiest to get rid off. When the solution is cooled down , the product will crystallize first. The soluble impurities will be carried away during the filtration.

i)

What additional step should be added to this procedure to remove the impurities insoluble in solvent?

Centrifugation step should be added. This step required to separate the recrystallized solid from the recrystallization solvent.

j)

Gravity and vacuum filtration separate insoluble solids from a liquid phase. The choices depend on conditions. Suggest criteria you would apply to choose between them? Gravity filtration is useful when removing minor amounts of solid impurities from solution. It can be done on a hot solution where the vacuum filtration cannot be done.

k) Suggest any ways you can think of improve any parts of this experiment?

Choosing an appropriate solvent is can improve the result that will be gained. The organic compound must have low solubility in the solvent at room temperature and moderate solubility at the boiling point. Ideally, the solubility of the impurities is greater than the organic compound at both high and low temperatures obviating the need for a hot filtration step. 6. Conclusion The recovery percentage of naphthalene is 75%.