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Reminder: These notes are a supplement to the procedure for Recrystallization.

RECRYSTALLIZATION - Recrystallization is a technique used to purify organic solids. That is, you
will separate molecules of impurity from molecules of desired material.

A Recrystallization solvent should have the following properties:


1. Does not dissolve the compound to be purified when cold.
2. Does dissolve the compound when 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 then get the crystals back in the
end in a pure state.

See the following website for an excellent movie on the procedure of recrystallization
http://www.scivee.tv/node/3005 There are many recrystallization videos on the internet. Just search a bit
if you need to see more.

There are seven steps to Recrystallization. They are:

1. Choose a solvent that doesn’t dissolve the compound when cold but does so readily when near
boiling.
2. Add hot solvent until the compound you are trying to purify just dissolves. Do not add too much
solvent. Use a minimal amount. In this experiment you are given a recommended amount. That
may not always be true so you will have to be patient.
3. 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.
4. FILTER BY GRAVITY WHILE HOT. 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 undissolved impurities. Use fluted
filter paper. This provides a large surface area allowing for fast filtration.
Recall: When you want the filtrate, use gravity filtration.
5. 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.
6. Perform suction filtration to isolate the compound. Dissolved impurities stay in this filtrate.
Recall: When you want the solid, use suction filtration.
7. Dry the crystals in a safe place in your drawer. Do not bottle them as they need to dry. Do keep
them safe.

Next week you will identify your compound using melting point. A list of possibilities is given in the
experiment handout. Determine the melting point of your pure compound. Pure samples melt over a
narrow range close to the literature value of the melting point. Samples containing soluble impurities
have a melting point range that is broader and lower that the melting point range of a pure sample. If your
compound has a mp higher than the literature value, it is not that compound. It is something else. You
should use mixed melting point to determine the identity of your compound. In that case, mix the crystals
of your unknown with the compound you think it might be. If they are one in the same, there will be no
change in melting point. If they are not identical, there will be a depression in melting point since one
compound acts as an impurity for the other. Determine the percent recovery of your material. Percent
recovery equals the weight of compound recovered divided by the weight of compound you started with
times 100%. Note that you cannot get a 100% recovery.

Finally, this experiment will allow us to introduce the concept of spectroscopy. You will record an IR of
your compound and an NMR will be provided.