RECRYSTALLIZATION
Recrystallization is a technique used to purify organic solids. That is, you will separate molecules of impurity from molecules of desired materials
A Recrystallization solvent should have the following properties:
1. Does not dissolve the compound to be purified when cold
2. Does dissolve the compound then hot (near boiling)
3. Has a relatively low bp for easy evaporation from the purified compound
4. Does not react with the compound being purified,
5. The cold solvent will keep impurities dissolved.
So- you’ll start with impure crystals, dissolve them in a hot solvent and the get the crystals back in the end in a pure state
There are several steps to Recrystallization. They are:
- Choose a solvent that does not dissolve the compound when cold but does so readily when near boiling
- Add hot solvent until the compound you are trying to purify just dissolves; do not add too much solvent. Use a minimal amount
- Add decolorizing carbon (charcoal) to remove colored impurities. The step is skipped most often. Do not add the charcoal to a boiling solution because it will bump and boil over. Add a small amount of charcoal because you will lose good compound as well as colored impurities by adsorption to the charcoal.
- FILTER BY GRAVITY WHILE HOT (gravity filtration). This is the step that makes the recrystallization a success. It should never be omitted from a recrystallization. Remember this step for future recrystallizations. This step removes the charcoal and any undisclosed impurities. Use fluted filter paper. This provides a large surface area allowed for fast filtration. Recall: when you want the filtrate, use gravity filtration.
- Cool the filtrate from #4. Cool first in air and then later in an ice/water bath, ask your TA what to do if crystals don’t form.
- Perform suction filtration to isolate the compound, dissolved impurities stay in this filtrate. Recall: when you want the solid, use suction filtration.
- Dry the crystals in a safe place in your drawer. Do not bottle them as they need to dry. Do keep them safe.
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