UNMSM/FQIQ/EPIQ/DAADP/INGLÉS TÉCNICO/EF3/2020-I

SEPARATION AND PURIFICATION TECHNIQUES

2.2. Recrystallization

Crystallization is the deposition of crystals from a solution or melt of a given material. During
the process of crystal formation, a molecule will tend to become attached to a growing crystal composed
of the same type of molecules because of a better fit in a crystal lattice for molecules of the same
structure than for other molecules. If the crystallisation process is allowed to occur under near-
equilibrium conditions, the preference of molecules to deposit on surfaces composed of like molecules
will lead to an increase in the purity of the crystalline material. Thus the process of recrystallisation is
one of the most important methods available to the chemist for the purification of solids. Additional
procedures can be incorporated into the recrystallisation process to remove impurities. These include
filtration to remove undissolved solids and adsorption to remove highly polar impurities.
Recrystallisation depends on the differential solubility of a substance in a hot and cold
solvent. It is desirable that the solubility of the substance be high in the hot solvent and low in the
cold solvent to facilitate the recovery of the starting material. The solution remaining after crystals
have deposited is known as the mother liquor. The proper choice of solvent is critical and may
require trial tests with small quantities of the material in a variety of solvents or solvent pairs
(combinations of two solvents)

Recrystallisation procedures

The solvent, or solvent pair, to be used in the recrystallisation of a substance is chosen in the
following manner. A small amount of the substance is placed in a small test tube and a few drops of
solvent are added. The test tube is gently heated to see if the sample dissolves in the heated solvent. In
general, one should first use a nonpolar solvent, for example, hexane or petroleum ether. If the sample
does not dissolve, try using a more polar solvent such as ethanol or acetone. Should the sample
completely dissolve in any solvent, chill the solution to see whether crystals will form (sometimes it is
necessary to chill the solution using a Dry Ice-acetone bath in order to cause crystallisation). If no
crystals appear, the material is too soluble in that solvent, and that solvent should not be used for the
recrystallisation. If no single solvent provides suitable results, a mixture of two solvents can be
employed, one of the solvents being a good solvent for tthe sample, and the other being a poor solvent
for the sample. The sample is first dissolved in the solvent in which the sample is most soluble, and
then small portions of the other solvent are added until a cludiness is formed upon addition of the
second solvent. A small amount of the better solvent is added to remove the cludiness, and the solution
is allowed to cool. The correct proportion of the two solvents must be determined by trial and error.
Once the proper solvent has been chosen, the remainder of the sample is recrystallized.
For gram- or multigram-scale recrystallisations, the material to be recryustallised is placed in a
suitable container such as an Erlenmeyer flask.

Translate the section of the text indicated.

1) Decide if these statements, RELATED TO THE TRANSLATED TEXT, are true or false.

a) To select the most suitable solvent, you can work with the total sample
b) By selecting the most suitable solvent, you start to test with the most polar ones.
c) When the desired results are not achieved with one of the solvents, the use of two solvents is used.
d) If two solvents are used, the sample is first dissolved in the one in which it is least soluble.
e) There is a precise formula that allows calculating the proportions in which the two solvents must be
added.
2) The following questions refer to the sections NOT INCLUDED IN THE TRANSLATION of the text.
Answer them.

a) Why does the crystallization process take place?

b) What is this process for?
c) With what other methods can it be combined and what are they used for?
d) What is the foundation of the recrystallization process?
e) What is defined in the text as “mother liquid”?
f) How is the most suitable solvent chosen?
g) When is activated carbon used in this type of process?

TÉCNICAS DE SEPARACIÓN Y PURIFICACIÓN

Recristalización
La cristalización es la deposición de cristales de una solución o fusión de un material dado. Durante el proceso de
formación de cristales, una molécula tenderá a unirse a un cristal en crecimiento compuesto por el mismo tipo de
moléculas debido a un mejor ajuste en una red cristalina para moléculas de la misma estructura que para otras
moléculas. Si se permite que el proceso de cristalización ocurra en condiciones de casi equilibrio, la preferencia de las
moléculas para depositarse en superficies compuestas de moléculas similares conducirá a un aumento en la pureza del
material cristalino. Así, el proceso de recristalización es uno de los métodos más importantes disponibles para el
químico para la purificación de sólidos. Se pueden incorporar procedimientos adicionales en el proceso de
recristalización para eliminar impurezas. Estos incluyen filtración para eliminar sólidos no disueltos y adsorción para
eliminar impurezas altamente polares.
La recristalización depende de la solubilidad diferencial de una sustancia en un solvente frío y caliente. Es deseable
que la solubilidad de la sustancia sea alta en el disolvente caliente y baja en el disolvente frío para facilitar la
recuperación del material de partida. La solución que queda después de que los cristales se han depositado se conoce
como las aguas madres. La elección adecuada del solvente es crítica y puede requerir pruebas de prueba con pequeñas
cantidades del material en una variedad de solventes o pares de solventes (combinaciones de dos solventes)
Procedimientos de recristalización
El disolvente, o par de disolventes, que se utilizará en la recristalización de una sustancia se elige de la siguiente
manera. Se coloca una pequeña cantidad de la sustancia en un tubo de ensayo pequeño y se añaden unas gotas
de disolvente. El tubo de ensayo se calienta suavemente para ver si la muestra se disuelve en el disolvente
calentado. En general, primero se debe usar un solvente no polar, por ejemplo, hexano o éter de petróleo. Si la
muestra no se disuelve, intente usar un solvente más polar como etanol o acetona. Si la muestra se disuelve por
completo en cualquier solvente, enfríe la solución para ver si se formarán cristales (a veces es necesario enfriar
la solución usando un baño de hielo seco-acetona para provocar la cristalización). Si no aparecen cristales, el
material es demasiado soluble en ese solvente, y ese solvente no debe usarse para la recristalización. Si ningún
solvente individual proporciona resultados adecuados, se puede emplear una mezcla de dos solventes, uno de
los cuales es un buen solvente para la muestra, y el otro es un solvente pobre para la muestra. La muestra se
disuelve primero en el solvente en el que la muestra es más soluble, y luego se agregan pequeñas porciones del
otro solvente hasta que se forma una capa turbia al agregar el segundo solvente. Se agrega una pequeña
cantidad del mejor solvente para eliminar la suciedad, y la solución se deja enfriar. La proporción correcta de
los dos solventes debe determinarse por ensayo y error. Una vez que se ha elegido el solvente apropiado, el resto
de la muestra se recristaliza.
Para recristalizaciones a escala de gramo o multigramo, el material a recristalizar se coloca en un recipiente
adecuado, como un matraz Erlenmeyer.
1) Decide if these statements, RELATED TO THE TRANSLATED TEXT, are true or false.

f) To select the most suitable solvent, you can work with the total sample FALSE
g) By selecting the most suitable solvent, you start to test with the most polar ones. FALSE
h) When the desired results are not achieved with one of the solvents, the use of two solvents is used.
TRUE
i) If two solvents are used, the sample is first dissolved in the one in which it is least soluble. FALSE
j) There is a precise formula that allows calculating the proportions in which the two solvents must be
added. FALSE

2) The following questions refer to the sections NOT INCLUDED IN THE TRANSLATION of the text.
Answer them.

a) Why does the crystallization process take place?

Crystallization is the deposition of crystals from a solution or melt of a given material. During the
process of crystal formation, a molecule will tend to become attached to a growing crystal
composed of the same type of molecules because of a better fit in a crystal lattice for molecules of
the same structure than for other molecules.

b) What is this process for?

This process is for the recovery of the starting material.

c) With what other methods can it be combined and what are they used for?

Additional procedures can be incorporated into the recrystallisation process to remove impurities.
These include filtration to remove undissolved solids and adsorption to remove highly polar
impurities.

d) What is the foundation of the recrystallization process?

Recrystallization occurs when the crystallization is brought to near equilibrium conditions, which
generates a greater preference for the molecules to join surfaces composed of similar molecules,
thereby achieving greater purity of the crystalline material.

e) What is defined in the text as “mother liquid”?

The solution remaining after crystals have deposited is known as the mother liquor

f) How is the most suitable solvent chosen?

The proper choice of solvent is critical and may require trial tests with small quantities of the
material in a variety of solvents or solvent pairs (combinations of two solvents)

g) When is activated carbon used in this type of process?

Activated carbon is used as an additional procedure to remove highly polar impurities.