Adding an appropriate solvent to the impure material

When choosing a solvent for recrystallization, the impure compound should have poor solubility in
the solvent at low temperatures but be completely soluble at high temperatures. This allows the
solid to completely dissolve when heated, but crash out of solution when cooled. Ideally, you
should add the smallest amount of solvent possible that will still completely dissolve the sample
when heated. When adding solvent, it's best to err on the side of adding too little, as you can
always add more as you're heating it.

Heating the suspension until everything dissolves

Once you have added the solvent to the sample, you need to heat the suspension to dissolve the
sample. Heating is probably best done with either a steam bath or a hot water bath, as heating
with these sources is controlled and gentle. Alternatively, you could use a hot plate (as shown in
Figure 3) or a heat gun

Cooling the solution to allow the product to crystallize

Once all of the sample is dissolved from heating, the flask is placed in an icebath (or refrigerator)
to cool it down. See Figure 5. Often, it's desirable to allow the solution to cool to room
temperature in open air before placing it in the icebath, as slow cooling often leads to purer
crystals
After cooling for some time, crystals should form on the bottom of the flask, as shown in Figure 6.
You can often aid crystallization in stubborn cases by scratching the inside of the flask
with a glass rod at the air-solvent junction. This scratching flecks off small shards of glass
that form a surface upon which the solid can crystallize. Sometimes, the solution can be
"seeded" by adding a small seed crystal of pure sample to the cold solution. This seed
crystal also forms a surface for the solid to crystallize upon. If no crystals form upon
cooling, you may have used too much solvent, and should evaporate some of the solvent
and try again

Isolating the purified solid by vacuum filtration

Once the solid has crystallized, you then filter the suspension to obtain the pure solid. This is
typically done via vacuum filtration (Figure 7). Once the solid has been filtered, it is sometimes
washed with additional quantities of chilled solvent. If you wash the sample, make sure not to
overdo it because the added solvent will dissolve some of your sample (this is why it's important
to add cold solvent to wash the sample).

Drying the purified solid

Once you have the product, it should be dried. Much of the drying can be done by aspirating the
product in the vacuum filtration apparatus for several minutes before removing it. The purified
solid can be dried in open air or under a vacuum. If you need a small amount of dry sample (to do
a melting point analysis, for example), you can rub a small amount of the solid on a shard of
porous porcelain, or between two sheets of filter paper. In difficult cases, it may be necessary to
perform more than one recrystallization to completely purify the sample

2. The

first consideration in purifying a solid by recrystallization is to find a suitable solvent.

There are four important properties that you should look for in a good solvent for
recrystallization.
1. The compound should be very soluble at the boiling point of the solvent and only
sparingly soluble in the solvent at room temperature. This difference in solubility at hot
versus cold temperatures is essential for the recrystallization process. If the compound is
insoluble in the chosen solvent at high temperatures, then it will not dissolve. If the
compound is very soluble in the solvent at room temperature, then getting the compound

to crystallize in pure form from solution is difficult. For example, water is an excellent
solvent for the recrystallization of benzoic acid. At 10C only 2.1 g of benzoic acid
dissolves in 1 liter of water, while at 95 C the solubility is 68 g/L.
2. The unwanted impurities should be either very soluble in the solvent at room temperature
or insoluble in the hot solvent. This way, after the impure solid is dissolved in the hot
solvent, any undissolved impurities can be removed by filtration. After the solution cools
and the desired compound crystallizes out, any remaining soluble impurities will remain
dissolved in the solvent.
3. The solvent should not react with the compound being purified. The desired compound
may be lost during recrystallization if the solvent reacts with the compound.
4. The solvent should be volatile enough to be easily removed from the solvent after the
compound has crystallized. This allows for easy and rapid drying of the solid compound
after it has been isolated from the solution
3. Solubility of acetanilide in hot and cold water
1. The solubility of acetanilide in hot water (5.5g/ 100 mL @ 100
degrees) is not very great, and its solubility in cold water (0.53g/ 100 mL @
0 degrees) is significant