Preparation of Absolute Ethanol from

Grain Alcohol
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Absolute, or 99.5% water-free, Ethanol is frequently necessary in

many organic operations. It is quite easy to prepare from the
azeotrope with water such as "Everclear" brand grain alcohol,
"moonshine" or "Rectified Spirits" (an old term for the same
thing).

Dehydrate 75g of fresh anhydrous Calcium Oxide in a vacuum

dessicator for 24 hours (a bit redundant, I know) or heat in an
oven at 200C for 2 hours, then immediately transfer to the vacuum
dessicator until use. Setup glassware for simple refluxing with a
water-cooled condenser and a Calcium Chloride guard tube. Place
350mL of Ethanol into the flask, quickly add the Calcium Oxide
and hold at gentle reflux on the water bath or heating mantle for
6 hours. Allow the mixture to stand overnight, then distill off
the alcohol, discarding the first few mL (it may be more convenient
to just vent the condenser to the atmosphere for the first couple
of minutes after distillation has commenced). Yield should be
better than 315mL. Store the absolute Ethanol in a tightly closed
glass container as it will pick up water from the air rapidly.