Beruflich Dokumente
Kultur Dokumente
Objectives
This experiment aims to elucidate the meaning of purity chemically by
applying the method of recrystallization in purifying a solid sample. Melting point
determination will also be used to compare the melting point of a pure vs. impure
sample of a substance.
II.
The table below shows the data gathered and the yield for Naphthalene.
Table 1: Naphthalene Data
Crude Naphthalene
Pre-weighed filter paper
Filter paper + naphthalene crystals
Recovered purified naphthalene
Percentage yield
As seen on the table, the percentage yield was only 20.79%. Errors must have
occurred during the experiment. These errors with this magnitude, however, were
already anticipated. Recrystallization needs a lot of careful handling and practice
since the procedure itself can induce errors. Loss of sample cannot be avoided in
filtering: some materials might be left behind. This error, however, can be
minimized by practice. Some loss may be caused by the prolonged contact of the
solid and its recrystallization solvent. This is because the solid is somehow still
soluble in the solvent even at low temperature. Another cause might root in rinsing
the crystals during vacuum filtration. It may be that too much solvent is used.
Melting Point Determination
Verification of the purity of the recrystallized solids must be done. Using a
melting point apparatus, the meting points of the crude and recrystallized solids
were taken. Small amount of the solids were put into capillary tubes to be placed
in the apparatus. Four temperatures were taken in the following time frames: Stage
1 the appearance of bubbles and darkening of the solution; Stage 2 the
breaking down of the solid; Stage 3 formation of meniscus; Stage 4 complete
liquefaction of the solids.
Table 2: Naphthalene Meting Point Data
Stage 1
Stage 2
Crude
80 C
81.1 C
Naphthalene
Recrystallized
80.2 C
81.3 C
Naphthalene
Stage 3
81.5 C
Stage 4
82.0 C
81.7 C
82.0 C
The table above shows the melting point of the crude and recrystallized
naphthalene. As expected, the melting point of the crude naphthalene is lower than
the recrystallized one. The range of the crude sample is wider than the
recrystallized naphthalene.
Table 3: Caffeine Meting Point Data
Stage 1
Stage 2
Crude Caffeine 231
Recrystallized
232
Caffeine
Stage 3
234
233
Stage 4
235
235
The table above shows the melting point of the crude and recrystallized caffeine.
The stage 1 melting point wasnt observed since it was hard to tell if there were
already bubbles. Errors can also appear in this part of the experiment because it
depends on visual judgments.
III.
Questions
1. What is a crystal and what is meant by recrystallization?
A crystal is "a three-dimensional atomic, ionic, or molecular structure consisting
of periodically repeated, identically constituted, congruent unit cells" and to
crystallize is "to cause to form crystals or assume a crystalline form". (American
Heritage Dictionary of the English Language, 1973) Recrystallization, then, is a
process in which impure crystals undergo series of procedures from dissolution in
a selected solvent to subjection in a low temperature to attain their purest state.
2. How does recrystallization free a substance from impurities? Explain how each
step in recrystallization contributes to the removal of the impurities.
Recrystallization takes advantage of the solubility properties of the impure
organic crystal/solid in a hot solvent to remove its impurities. The first thing that
must be done is selecting a suitable solvent where the impure solid is dissolved.
In choosing the appropriate solvent, one must take note of the temperature in
which the solid is dissolved. Ideally, the solubility of the solid should be at its
maximum in the solvent with an elevated temperature and at its minimum in the
solvent with low temperatures. This step is crucial because the properties of the
chosen solvent make the whole process possible. After choosing, the solid must
be dissolved in it (selected solvent) while subjected to heat. By doing so, the
impurities on the solid will be vulnerable to separation. The next step would be
the addition of decolorizing charcoal (activated carbon). This is only done,
however, if the solution is colored. What the activated carbon does is making the
colored molecules be adsorbed on its surface thus decolorizing the solution. This
step is then followed by cooling the solution to reform crystals, now, without the
soluble impurities that remained in solution. Suction filtration is done next to
separate the solid compound to its soluble impurities. The recovered solids are
then dried to remove the remainder of the recrystallized solvent (also an
impurity).
3. What must be considered in choosing a solvent for recrystallization?
A solvent considered for recrystallization must satisfy the following: (a) the
solvent must dissolve the organic solid in an elevated temperature (ideally about 5
g/100 mL) and must not able to do so in low temperature/ room temperature; (b)
the impurities must be insoluble or partially soluble in the cold solvent; (c) the
solvents boiling point should be low enough so that it is easily removed from the
recrystallized solid by merely letting it dry; (d) the boiling point of the solvent
must be lower than that of the purified solids melting point; (e) lastly, the solvent
should not react with the organic solid chemically to avoid complications.
4. What is melting point? Why can it be used as an index of purity?
The melting point of a solid is defined as the temperature at which the solid and
liquid phases are in equilibrium. In recrystallization, the meting point taken (as
basis of purity) is temperature range at which a compound melts from the
observation of the initial melting of the first to the last crystal.
Taking account that crystals with high melting points have strong intermolecular
forces acting on its molecules, one can deduce that crystals or solids with
impurities will have a lower melting point. This is why melting point can be used
as an index of purity. The more pure the substance, the higher and sharper the
melting point.
IV.
Conclusion
Purity, in the chemical sense, is very important in organic chemistry
especially in carrying out chemical reactions. If the reactant used is in its purest state
then it is very likely for the reaction to succeed and thus, getting the desired product.
There are a lot of purifying techniques and one of these is recrystallization.
Recrystallization is a technique that aims to separate the solid from its impurities by
using the principle of solubility. This method was applied to the crude Naphthalene
and caffeine. Although the percentage yield wasnt that favourable in terms of
magnitude, the recrystallization was a success. This is proved by melting point
determination. The crude samples were found out to have lower melting point and a
broader range while the recrystallized samples have high and sharp melting points.
V.
References
______________________
Dagondon, Vanessa Olga J.
______________________
Sanchez, Diandra Dawn J.