Pruebas de solubilidad

PRUEBAS DE SOLUBILIDAD EN DISOLVENTES ORGÁNICOS:
CRISTALIZACIÓN SIMPLE

Nombre: Suárez Ruperto Adriana Química Orgánica (1311)

Procedimiento

A.- Cristalización simple
A) Solubilidad en disolventes orgánicos

Coloque en un tubo de ensayo 0.1 g de la muestra problema. Agregue 1 ml de disolvente a probar agite y observe. Si el sólido no se hadisuelto, agregue otro ml y observe con cuidado (pueden quedar impurezas insolubles). Si no se disuelve, repita el procedimiento hasta 3 ml máximo
Si el sólido no se ha disuelto, es insoluble en frío; si se disolvió, es soluble en frío.
Si la sustancia fue insoluble en frío, caliente la muestra en baño María hasta ebullición y con agitación constante, teniendo precaución de mantener inalterado elvolumen de la solución. Si el disolvente es agua, agregue cuerpos de ebullición y caliente en mechero hasta ebullición. Observe si hay solubilización o no.
Si la sustancia fue soluble en caliente, enfríela a temperatura ambiente y luego en baño de hielo-agua. Observe si hay formación de cristales.

Análisis del procedimiento.

En este caso se decidió utilizar Dibenzalacetona. El únicodisolvente no disponible fue el cloruro de metileno

|Disolvente |Hexano |Acetato de etilo |Acetona |Etanol |Metanol |Agua |
|Solubilidad en frío|No |Si |Si |No |No |No |
|Solubilidad en |No |Si |Si |Si|Si |No |
|caliente | | | | | | |
|Formación de | | | |Si |Si | |
|cristales | | | | || |

Se decidió utilizar el etanol por seguridad

B) Cristalización simple

Pese el resto que le haya sobrado de la muestra problema y colóquelo en un matraz Erlenmeyer de tamaño apropiado (siempre se usan matraces Erlenmeyer para cristalizar). Agregue poco a poco el disolvente ideal, previamente calentado (comience con 10 ml). Caliente la mezcla hastaebullición agitando constantemente y continúe agregando disolvente hasta disolución completa. (Utilice cuerpos porosos para controlar la ebullición).
Para eliminar las impurezas insolubles, filtre en caliente. Este paso debe hacerse rápidamente, para evitar que el producto cristalice en el embudo.
Para filtrar en caliente, doble el papel filtro para filtración rápida (Figura 1), precaliente un embudo devidrio y el matraz en el que recibirá el filtrado. Monte el embudo sobre el matraz dejando un hueco entre ambos para que “respire” (Figura 2). Humedezca el papel filtro con un poco del disolvente y filtre en caliente. Enjuague el matraz y el papel filtro con un poco (3 a 5 ml) del disolvente caliente.
Deje enfriar el filtrado a temperatura ambiente y luego en baño de hielo-agua para que se formenlos cristales. Si esto no ocurre, induzca la cristalización.

Una vez formados los cristales, sepárelos de las aguas madres por filtración al vacío.
Para esto, fije el matraz Kitasato con unas pinzas (para evitar que se vuelque y conéctelo a la llave del vació mediante su manguera; el embudo Buchner se le coloca dentro un círculo de papel filtro, cuidando que ajuste perfectamente y se conecteal Kitasato mediante un adaptador de hule. Se humedece el papel filtro con un poco del disolvente frío, se abre la llave del vacío suavemente, sólo a que se fije el papel, y se vierte el contenido del matraz de cristalización (primero se inclina el matraz Erlenmeyer y con la espátula se pasa la mayor parte de los cristales al fondo del mismo y luego se comienza a verter, moviendo el matraz y…

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