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Object of Recrystallization Method:Recrystallization is a purification process used to remove impurities from organic compounds that are solid at room temperature by dissolve the impure solid in the minimum amount of a hot solvent and then allow crystals to form slowly .
Steps of Recrystallization Method:1.
Choosing the crystallization solvent.
The general rule is “like dissolves like” If our solute is nonpolar, then we will likely choose a solvent like hexane or petroleum ether. If our solute is polar, then we will choose something more toward methanol or acetone., the best solvent will dissolve all of the solute when the solution is hot and none of the solute when cold.
Dissolving the solute.
The usual procedure is slowly (if not dropwise) adding the solvent with stirring. We want to be sure that we are also heating our solution over a hot plate or steam bath. We add just enough boiling solvent to get the crystals to dissolve (the MINIMUM amount).
Decolorizing the solution.
To remove colored impurities from the solution, we often add a bit of activated carbon (charcoal) to which impurities can adsorb onto the surface. Pelletized Norit is the most common form and can be easily removed by gravity filtration.
Removing suspended (undissolved) solids.
Vacuum filtration is not a good option because it cools the solution in the process. The two primary gravity filtration options are: (a) filtration through a cottonplugged Pasteur pipette; and (b) gravity filtration through a glass funnel fitted withfluted filter paper.
Crystallizing the solute.
The most important thing is to be sure that you do not have too much of your hot solvent if this the case, then boil some of it off until you reach the saturation point. Once you are at thispoint, then you will want to SLOWLY cool your solution to room temperature on the benchtop. If crystallization does not begin (after a reasonable amount of time), then you can employ a few tricks to aid in the process. Some of the tricks include: (a) adding a seed crystal the seed crystal has the same structure as the pure crystal to be recovered. ; (b) scratching the inside of the container with a glass stirring rod; or (c)further cooling the solution in an ice bath. Always remember to be patient. We want todo this step slowly to insure the formation of large, pure crystals.
Collecting and washing the crystals.
Once crystallization is complete, the crystals can be separated from the ice-cold mother liquor (the filtrate) by vacuum filtration. We will also want to remove excess impuritiesbthe may be dissolved in the solvent by washing with pure solvent. Keep in mind that we will want to wash with COLD solvent so that we do not redissolve any of the crystals.
The Properties of Ideal Recrystallization:• A suitable solvent should be: 1. Soluble at the boiling point of the solvent and slightly soluble at room temperature. (if soluble, hard to separate pure crystals because the molecules interact) 2. The solvent should not react since their interaction would result to a lesser yield of pure crystals.
The solvent should be many amount and volatile enough to be easily removed from the solute/s. This allows rapid drying of the solid compound after it has isolated from the solution.
• Cooling rate should be: Slowly as we can to produce a large and clear crystal.
References:-Carl wigal,Lebanon valley college
-"The Student's Lab Companion: Laboratory Techniques for Organic Chemistry”, by John W. Lehman "www-pub.naz.edu" (W. H. Bunnelle, L. A. Meyer, R. E. Glaser (Version3 - John Edward O. Tanchuco & Carolyn Marie D. Legaspi Section AB2
By : Mahmoud Ahmed Alashmawi Sec(5) no.198