Experiment Number 2 Recrystallization and Melting Point Determination

Maugri Grace Kristi P.
Laluma November 30 and December 3, 2010

Group Number 4 December 10, 2010
Experiment Number 2
Recrystallization and Melting Point Determination
I. Objectives
1. To clarify the meaning of purity in the chemical sense.
2. To apply the method of recrystallization in the purification of a solid sample.
3. To recognize the melting point as a physical property that can serve as an index of
purity.
4. To determine the melting point of a substance using a simple apparatus.
5. To compare the melting point of a pure versus impure sample of a substance.
II. Theoretical Background
In this experiment the techniques called recrystallization will be studied and the melting
point of the collected crystals will be determined to check and analyze its purity content and to
check its percent recovery from the original solid organic sample.
Recrystallization is a technique often use in purification of solid organic compounds to isolate
the purity of the sample and extract impurities. Using this technique will enable you to achieve
the highest possible state of purity of the sample. In the step-by-step process of the sample, many
simple techniques of separation and solubility will be used that would in turn help in extracting
the impurities in the sample.
III. Data and Results
Characteristics of Resulting Crystals

Characteristic
SOLVENT
s
Water 95% Ethanol CCl4
Size visible No crystal formed but the No crystal formed
Color Cloudy white solution looked immiscible but the solution
having the upper layer looked immiscible
viscose than the lower having the upper
layer. layer viscose than
the lower layer. But
Spiky formation on top when it was put in
Crystal Form and cloudy-like an ice-water bath in
formation at the bottom the next period
crystals formed
cloudy-like and
powdery.
Melting Point Determination

TRIAL 1 TRIAL 2
Melting Point Range
118˚C-121˚C 119˚C-122˚C
(Temperature 1 to Temperature 2)
Change in color (if any) none It became transparent
Shrink and became
Shrinking of sample (if any) No shrinkage
compacted
Recorded Measures
Weight of Evaporating Dish= 58.7523g

Weight of Evaporating Dish + Scraped Crystal= 58.9156g
Weight of Crystal Formed= 0.1633g Note: This is not the total weight of
the crystal since it was not
measured when it crystallized in
the Erlenmeyer flask.
IV. Discussions
In this experiment, we are given benzoic acid as the crude sample. In choosing its solvent
to be used among water, 95% ethanol and CCl4, it wasn’t sure what principle behind was to take
into account so we used CCl4. Well in fact, water should be the one to be used since in the
recrystallization process there are interactions on the bonds of molecules that are polar and some
are exhibiting hydrogen bonding. Thus in choosing the good solvent, the polarity of the solvent
should be taken into account. Among the three, water is the most polar and it was experimented
that it is indeed a good solvent for benzoic acid. Since the solute is insoluble at room temperature
and soluble at high temperature and it is accompanied that its impurities are soluble at all
temperature. Nevertheless, when we used CCl4 we had a hard time to recrystallized it but after
the next period it crystallized when it was out into an ice-water bath.
Polar compounds are normally soluble in polar solvents and insoluble in nonpolar
solvents, whereas nonpolar compounds are more soluble in nonpolar solvents being “like
dissolves like”. Of course, although a highly polar compound is unlikely to be soluble in a hot,
nonpolar solvent, it may be very soluble in a cold, very polar solvent. In this case, a solvent of
intermediate polarity may be the choice for a satisfactory recrystallization.
Recrystallization of solids is one of the many techniques used for purification of solid
organic compounds. It is a process that involves the dissolution of a solid in a chosen solvent at
an elevated temperature and re-formation of crystals upon cooling. As the compound crystallizes
from the solution, the molecules of the other compounds dissolved in solution are excluded from
the growing crystal lattice, giving a pure solid which are the impurities.
Its principle is behind the fact that almost all solids are more soluble in a hot than in a cold
solvent. If the solid is first dissolved in an amount of the hot solvent where it is insufficient to
dissolve it when cold, crystals will form when the hot solution will be allowed to cool. But then
the extent of crystallization of the solid depends on the difference in its solubility with the
particular chosen solvent and the solid should recover at enough temperatures or the solvent will
freeze
All in all for the first part of the experiment, the resulting crystals that formed is very
visible for water but for the 95% ethanol it dissolved and in CCl 4. But in CCl4 when it was put in
an ice-water bath in the next period it crystallized.
For the melting point determination for the collected crystal of benzoic acid and CCl4,
we have recorded it to be approximately 118˚C-122˚C for the two trials. It is very precise with
the theoretical melting point of benzoic acid which is 121˚C-122˚C which means we have atleast
collected back the crude sample.
V. Calculations
VI. Answers to Questions
1. What is a crystal and what is meant by recrystallization?
Crystals are solids that form by a regular repeated pattern of molecules connecting
together. Its structure is a unique arrangement of atoms and molecules in a crystalline liquid or
solid.
Recrystallization of solids is one of the many techniques used for purification of solid
organic compounds. It is a process that involves the dissolution of a solid in a chosen solvent at
an elevated temperature and re-formation of crystals upon cooling. As the compound crystallizes
from the solution, the molecules of the other compounds dissolved in solution are excluded from
the growing crystal lattice, giving a pure solid which are the impurities.
2. How does recrystallization free a substance from impurities?

Explain how each step in recrystallization contributes to the removal of impurities.
The formed crystals should be a pure material since the impurities have dissolved in the
solution and is still dissolved after it was cooled. Also if it did not dissolve in the solution then it
was removed during filtration before cooling. And to check in the final part if the collected
output is really the pure one, the melting point of the solid is determined and it is compared with
the original sample to check if it is really pure or not.
3. What must be considered in choosing a solvent for recrystallization?
The choice of solvent is perhaps the most critical step in the process of recrystallization since the
correct solvent must be selected to form a product of high purity and in good recovery or yield.
(a) The desired compound should be reasonably soluble in the hot solvent and insoluble or
nearly insoluble in the cold solvent.
(b) Conversely, the impurities should either be insoluble in the hot solvent or must remain at
least moderately soluble in the cold solvent and very soluble at room temperature.
(c) The boiling point of the solvent should be low enough so that it can readily be removed from
the crystals.
(d) The boiling point of the solvent should generally be lower than the melting point of the solid
being purified. It should be volatile enough for it to evaporate after it crystallized
(e) The solvent should not react chemically with the substance being purified.
4. What is melting point? Why can it be used as an index of purity?
The melting point of a substance is the temperature at which the material changes from a
solid to a liquid state. Pure crystalline substances have a clear, sharply defined melting point. It
can be used as an index of purity since it determines if the collected output is pure by comparing
the gathered melting point range with the theoretical melting point of the crude sample.

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What is a crystal and what is meant by recrystallization?

How does recrystallization free a substance from impurities? Explain how each step in recrystallization contributes to the removal of impurities.

Maugri Grace Kristi P.

Laluma November 30 and December 3, 2010

1. To clarify the meaning of purity in the chemical sense.

2. To apply the method of recrystallization in the purification of a solid sample.

4. To determine the melting point of a substance using a simple apparatus.

5. To compare the melting point of a pure versus impure sample of a substance.

II. Theoretical Background

Characteristics of Resulting Crystals

Melting Point Determination

Weight of Evaporating Dish= 58.7523g

VI. Answers to Questions

1. What is a crystal and what is meant by recrystallization?

2. How does recrystallization free a substance from impurities?

4. What is melting point? Why can it be used as an index of purity?

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