National Autonomous University of Mexico

Faculty of Chemistry
organic chemistry lab
Lire Borja David
crystallization report

Objectives.

• Apply the crystallization technique as a purification method.

• Observe the factors that can affect the purification of a product during the crystallization
process.

Observations.

During the experimental process, the compound to be purified obtained a canary yellow
coloration, being this specific coloration of the compound, therefore it was not necessary to add
activated carbon. This is why the use of activated carbon must be specified during this technique,
if, on the contrary, the coloring is not specific to the compound, activated carbon must be added to
remove impurities.

The correct addition of ethanol during the process should also be noted, because in the particular
case of this student, the addition of ethanol stopped when turbidity did not appear, causing the
addition of more ethanol during the subsequent stages of the experiment.

Results.

The experimental activity began by weighing 0.2079 grams of "impure" dibenzalacetone after
recrystallization, a mass of 0.1767 dry grams was obtained, calculated yield gave 85% total yield.
The melting point of the substance was obtained, resulting in 106-107 degrees Celsius.

Group results and comparison.

The crystallization technique is a method of purifying solid compounds, there are two methods
that are by simple crystallization or by a pair of solvents, in this case a pair of solvents was used.
Once crystallization is complete, the easiest way to determine the purity of a compound is to
obtain the melting point using the Fisher-Johns apparatus and compare this value with that of the
literature, keeping in mind that there should be a small range for say that the compound is pure.
Contrasting the results of each team, there are variations in the performance obtained, but these
variations can be attributed to many issues, perhaps the most common would be cooling to room
temperature and subsequent ice bath.

Questionnaire.

• Why is it important to maintain the volume of the solution during heating?

It's important because when it's hot, the compound tends to dissolve more effectively, plus the
solvent doesn't have a chance to dissolve the compound.

• Why is it necessary to remove the turbidity from the solution?

Turbidity means that the crystals of our sample are forming rapidly, by crystallizing in this way we
would be obtaining smaller and less pure crystals, and therefore of lower quality. For this reason,
this small turbidity is dissolved with a little bit of the solvent where the sample is soluble and
heating a little if necessary.

• What qualities did each of the solvents exhibit to be used in a solvent pair crystallization?

That one is very soluble and the other very little, cold and hot

• What are the differences you find between the purified and unpurified substances?

In the impure substance there is a greater interval in the melting point, while in the pure substance
the interval is less between 1 or 0.5 degrees.

• In the crystallization process, two types of filtrations are performed. How do they differ,
and what types of impurities are removed in each of them?

In the first filtration impurities are separated, boiling bodies and the substance is dissolved. In the
second filtration, the crystals are recovered and dried under vacuum.

• Identify the differences between a simple crystallization and a solvent pair crystallization.

In simple crystallization the same solvent forms the crystals at a certain temperature. In a solvent
pair crystallization, one substance cannot dissolve and crystallize, so another substance is required.

Conclusions.

Solvent pair crystallization is used when a substance does not have a specific solvent and is used to
find two solvents that are miscible with each other, one that dissolves the solute when cold and
the other does not dissolve it when cold or hot; practically both have similar characteristics such as
their boiling points and thus obtain a medium solvent for the substance and it can be purified. We
resort to a solvent pair crystallization when we do not have a specific ideal solvent.

Bibliography.

Aguado, R. “Técnicas de cristalización”. Recuperado de:

https://riubu.ubu.es/bitstream/handle/10259.3/63/21.3%20-
%20T%E9cnicas%20de%20Cristalizaci%F3n%20y%20Sublimaci%F3n.pdf;jsessionid=4E1DF589F795
FE7FAE5D32EE4FEA8960?sequence=11. Fecha de consulta: 27/08/2023.
 Guaymas, O., Palacios, M., Villalba, M. “Breve fundamento de técnicas de purificación y
caracterización de sólidos”. Recuperado de:
file:///C:/Users/LENOVO/Downloads/breve%20fundamento%20de%20purificaci%C3%B2n%20y%2
0caracterizacion%20de%20s%C3%B2lidos2020.pdf. Fecha de consulta: 27/08/2023