RESULTS

Reading
Mass of sample (a) 4.00 g

Mass of filter paper (b) 0.3350 g

Mass of filter paper + crystal (c) 0.6343 g

Mass of crystal (c-b) 0.2993 g

Percentage of product yield

Melting point of pure crystal 114.3 ℃

Melting point of crystal yield 114.1 ℃

Condition Observation

Boiling the solution The solution became light pink when distilled water
was added onto the sample and some of the samples
slowly dissolved.

Cooling the solution Precipitation of crystal formed

DISCUSSION

Based on the experiment, the process of recrystallization was used to purity a sample
compound. The impure sample prepared was 4.0 g and this sample then was added with 30
ml of water and the solution was heated until boil and then 5 ml of water was added into the
solution and the colour of solution turned pink powdery substance. Then we cooled the
solution for 5 minutes and decolorized charcoals were added into the solution. The function
of decolorized charcoal was added is to bind high molecular weight, coloured impurities.
Charcoal is added once a hot saturated solution of the desired product produced and once
added it needs to be removed (along with the adsorbed coloured impurities) by hot gravity
filtration. The solution was heated again until boil and the solution was cooled 5 minutes
before filtered. Crystals began to form indicating that the compound was ready to be cooled
in the ice bath. We get the crystals 0.2993 g from the compound. The crystals were dried and
we take some of the pure crystals to be tested for melting point. The percentage of the
product yield was 7.48%. The percent yield was very low may because of some precautions
did not been taken care of and there might be many errors occur during handling the
experiment. One of the errors that might occur was during the cooling of the sample. There
might some crystals that were not fully formed from the solution and we had filtered it before
it was fully formed. The other assumption was during the boiling of the sample, some of the
sample had boiling out from the flask. The melting point of the crystal yield was 114.1‫ﹾ‬C and
the melting point of pure crystal was 114.3‫ﹾ‬C. The melting point of the crystals yield was 0.2
away from the actual point proving it to be nearly pure crystals.

QUESTIONS

1. What is the purpose to add the decolorized charcoal in the solution?

Decolorized charcoal is added during a recrystallization to bind high molecular
weight and coloured impurities.

2. Why the usage of water must be controlled in this process?

Water can hold certain of amount of solute. This is called the solubility of a solution.
The molecules of water can move together with the solid substances and can pass
through the filter.
3. Why the solution must be filtered while it is hot?
The solution must be filtered while it is hot because the solute must dissolve while hot
in order to rid its lattice of impurities, but must not remain dissolved at room
temperature.

4. How do you choose the solvent for the recrystallization process?

If the solvent is not specified, you will need to test a variety of solvents to determine
what will work best for the solute you are trying to recrystallize. This testing can be
accomplished by putting a small amount of your solute (about the size of a pea) into
three small test tubes. In each test tube, place 0.5 mL of each potential solvent. Use a
stirring rod to agitate the solute or "flick" the bottom of the test tube with one finger
while holding the top with the other hand. If the solute dissolves at room temperature
with stirring, the solvent should be discarded as a potential recrystallization solvent. If
the sample does not dissolve at room temperature, place the test tube in a hot water
bath and stir the contents. If the solute partially dissolves add more solvent and
continue stirring. If the solute dissolves completely, remove it from heat and place it
in an ice-water bath. If crystals do not form, try to scratch the inside of the test tube
with a stirring rod. If crystals form, you have found an appropriate recrystallization
solvent; if no crystals form, keep looking for the right match between solvent and
solute.

If no solvent can be found, perhaps you will need to use a mixed solvent. If two
solvents in which the solute has different solubility characteristics are mixed,
sometimes an appropriate solvent can be found. For instance, if your solute is
insoluble in water but soluble in ethanol at room temperature, a mixture of the two
solvents may produce an appropriate solvent in which the solute is insoluble at room
temperature but very soluble at a significantly higher temperature. To find the proper
proportion of water to ethanol in this example, first, completely dissolve your solute
in ethanol at room temperature. Then, begin to add water until the solution becomes
cloudy (this is because all of the solute is no longer held in solution). Add just enough
ethanol to make your solution clear and begin the recrystallization procedure.

5. Explain the meaning of recrystallization process and give the precautions in order to
obtain a high yield product.
 The principle behind recrystallization is that the amount of solute that can be
dissolved by a solvent increases with temperature. In recrystallization, a solution is
created by dissolving a solute in a solvent at or near its boiling point. At this high
temperature, the solute has a greatly increased solubility in the solvent, so a much
smaller quantity of hot solvent is needed than when the solvent is at room
temperature. When the solution is later cooled, after filtering out insoluble impurities,
the amount of solute that remains dissolved drops precipitously. At the cooler
temperature, the solution is saturated at a much lower concentration of solute. The
solute that can no longer be held in solution forms purified crystals of solute, which
can later be collected.
Precautions include using just enough water to dissolve the sample at high
temperature, doing the filtration when the solution is hot, and cooling slowly if we
want nice crystals, and then cooling on ice to improve yield and obtain a high yield
product.

6. Compare the melting point of the pure crystal and the melting point of the crystal
obtained in the experiment. Discuss the difference.
The melting point of the pure crystal is higher 0.2 than the melting point of the crystal
obtained. It may because the melting point of the apparatus does not been calibrated
before used. Other than that, maybe the crystals yield has been contaminated and
mixed with others substances.

CONCLUSION

In conclusion, the process of recrystallization successfully purified an impure compound. The

purity was confirmed due to the nearly identical melting point of the recrystallized (114.1‫ﹾ‬C)
and the pure crystal was 114.3‫ﹾ‬C.

REFERENCE

1. http://www.wiredchemist.com/chemistry/instructional/laboratory-
tutorials/recrystallization
2. https://www.coursehero.com/file/p2ojg3j/The-best-solvent-is-one-that-doesnt-
dissolve-the-compound-is-at-low-temperature/
3. http://www.pitt.edu/~bandik/organicweb/recrystallization.html