Rekristalisasi

The first experiment was recrystallization of aspirin. Recrystallization is

the process of purifying a solid compound by dissolving the compound in hot
conditions using the appropriate solvent then being converted to solid state again.
The selected solvent must be suitable for the sample used in this case salicylic
acid. The solvent used in this experiment is water. The selected solvent must
fulfill several conditions.
The first is that the solvent must not react with the sample. If the solvent
reacts with the sample, the resulting product will be produced so that the final
result will be different from the initial sample. In this case the water does not react
with salicylic acid but only dissolves it. The second is that the solvent must be
able to dissolve the impurities present in the sample. Water has polar properties
and generally the impurities in a compound are also polar. So water meets this
requirement. The third is the boiling point of the solvent must be smaller than the
boiling point of the sample. This has the purpose that the solvent is easily
separated from the sample. Water has a boiling point of ... while salicylic acid has
a higher boiling point which is equal to ... thus water meets this requirement.
(Kotz, 2009)
Fourth, there are differences in polarity between samples and solvents.
Salicylic acid has polar and nonpolar groups. The polar group is –OH and the
non-polar group is the benzene ring group. The structure of salicylic acid (below)
can dissolve in some polar solvents and some nonpolar solvents, but is difficult to
dissolve in solvents which have only polar or nonpolar groups. This is because it
has polar and nonpolar groups in one group, making it easier to dissolve in
semipolar solvents. However, if a semipolar solvent is used, salicylic acid will
dissolve completely with the solvent at room temperature to form a homogeneous
solution. This will make it difficult to refine salicylic acid because the impurities
are no longer distinguishable from the original. This condition also relates to the
fifth condition, namely the solvent must dissolve the sample in hot temperatures
and slightly dissolve the sample in cold temperatures. The water in this hail
fulfills the fourth and fifth conditions where water is polar which can dissolve
semipolar salicylic acid in hot conditions and slightly dissolve it in cold
conditions. This facilitates the purification of salicylic acid. Salicylic acid and its
impurities will dissolve in hot conditions and when cooled salicylic acid will
crystallize and the impurities will not crystallize but will remain in the solvent.
(Kotz, 2009)
In this experiment 1 gram of salicylic acid was weighed using the O’haus
balance sheet. Then put into a 125 mL erlenmeyer flask and add 5 mL of water.
The resulting mixture is white and is a heterogeneous solution. Therefore, it is
then heated using an electric stove until a homogeneous solution is formed.
After being heated and shaken a few while salicylic acid is still insoluble,
it is therefore gradually added to the water solvent into erlenmeyer. The total
volume of water added to salicylic acid dissolves is 28 mL.After salicylic acid is
dissolved and a clear solution is formed, the homogeneous solution is filtered in
hot condition using a buchner filter flask. On the surface of the pumpkin buchner
coated with filter paper. Pumpkin buchner is connected with a side pipe
erlenmeyer and connected to a vacuum pump. Filtering is done while the solution
is still hot, before the substance crystallizes from a cold solution.
According to Firdaus (2007) the purpose of heat filtering is to perfect
filtering before substances begin to crystallize to separate the impurities of
substances which are insoluble or suspended in solution, such as sand dust and so
on. For this reason, the funnel that is always used is a funnel without a handle to
prevent the formation of crystals in the stalk which can clog the flow of the
filtrate. The results of this filtration obtained a colorless filtrate and there is a little
white sediment, while the residue left in the filter paper on the buchner funnel.
From this filtration flit containing salicylic acid which might also still
contain a small amount of impurities. To perfect the separation of salicylic acid
from impurities which may still be left in the crystal it is reheated until the
dissolved crystals are complete. But this dissolution process does not run easily
crystals are very difficult to dissolve. This is caused by the heat released by the
stove is not stable.
After that the solution is cooled at room temperature until crystals are
formed. After the crystals are formed, the solution is filtered back using a Bucher
funnel connected by vacuum. Crystals formed on filter paper are white crystals.
This is in accordance with the theory which according to ... The crystal color of
aspirin (salicylic acid) is white.Then the crystals were dried using a desiccator for
2 days. After drying the crystals are weighed using an Ohaus balance and
measured their melting point using a meelting block connected to a thermometer.
The mass obtained from weighing is 1.1 grams. After reducing the mass of
filter paper by 0.7 grams, a crystal mass of 0.4 grams is obtained. The yield is
calculated at 40%. The yield obtained should be 100%. This difference is caused
by the screening process carried out before the crystal is completely formed. So
reducing the mass of the crystal obtained.
The melting point is measured by inserting crystals into the capillary tube.
The capillary tube is inserted into the meelting block which is connected to a
thermometer and heated with an electric stove. Based on ... The melting point of
salicylic acid is as big as ... In this experiment the melting point of salicylic acid
was obtained at 159 ° C. This result is in accordance with the existing theory and
indicates if the crystalline formed has good purity.
To be sure to test the crystals with FeCl3. A little crystal is put into the test
tube and dripped with FeCl3 solution. According to ... Iron (III) chloride reacts
with phenol groups to form purple complexes. Salicylic acid (pure) will turn
purple if FeCl3 is added, because salicylic acid has a phenol group.

+ FeCl3
From the results of observations made after being dropped the crystal
FeCl3 solution turns purple. This proves that the crystal obtained is pure salicylate
acid.