Reflux And Distillation Report

Methods of purification – Reflux and Distillation
There are many ways of purification however reflux and distillation are two widely used methods. Having a similar apparatus makes it simple and easy to use both methods together. Heating under reflux allows a reaction mixture to be heated for a set amount of time without loss of products, reactants or solvent. Distillation is done to refine or isolate the substances from each other. When preparing an ester (an organic compound) the reactants are heated together under reflux so any material that evaporates is condensed and returned to the mixture. The mixture is then distilled to separate the product.
A reflux apparatus:

A distillation apparatus:

Preparation and testing of an organic liquid
Preparing and testing an organic liquid for purification has 3 distinct parts to it: Reflux, Separation and Distillation. Reflux and Distillation reactions must be carried out in a fume cupboard to avoid toxic vapours from escaping and must also be allowed time to boil and reflux/distil.
Safety measures:
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A separatory funnel is attached to the clamp stand with a conical flask below as a receiving flask for the unwanted solution. The separatory funnel works by adding a solution to the mixture and blocking the top with a bung. Then turning the funnel upside down and right way around combines the mixture and the solution aiding in separating the ester from the aqueous layer. The aqueous layer is then removed/released by turning the head of the funnel. The bung must be removed at this stage as Carbon Dioxide is released. By the end the organic layer must be basic enough for you to wash it in the saturated salt solution (using the separatory funnel for this). The liquid is then dried with a drying agent which should leave the liquid