Stage One Method:

• Put anti bumping granules into the 50ml pear shaped flask

• In a fume cupboard, measure out 10ml Ethanol and 12ml Glacial Ethanoic Acid and add these to the flask

• Carefully add 15 drops of concentrated Sulfuric Acid to the flask

• Place a 250ml beaker containing some water on a tripod and gauze over a Bunsen burner

• Clamp the pear shaped flask in the beaker of water so that the reaction mixture is below the water line

• Add a condenser so that it is set up for the heating with reflux. Clamp the condenser, do not insert a stopper

• Light the Bunsen burner to heat the hot water bath. Raise the temperature of the hot water until the mixture in the flask if gently boiling

• Continue to gently boil the reaction mixture for 15 mins

• Turn off the Bunsen burner and cool the mixture by removing the hot water bath

Stage Two Method:

• Prepare a saturated solution of Sodium Carbonate by combining 4.5g of Sodium Carbonate with 15ml of Deionised water in a 100ml beaker

• In a fume cupboard, transfer the reaction mixture from the pear shaped flask, from stage one, to the beaker and stir

• Transfer the mixture into a separating funnel. Stopper it and turn it upside down gently, then open the stopcock to vent the system

• Invert at least 15-20 times, opening the stopcock each time

• Allow the 2 layers to separate. Ethyl Ethanoate is less dense than water so the top layer is Ethyl Ethanoate

• Remove the stopper, open the stopcock and slowly drain the waste aqueous layer into a 50ml waste beaker and close the stopcock

• Transfer the remaining ethyl ethanoate into a dry boiling tube containing about 1g of Anhydrous Sodium Sulfate. Agitate the tube so that any water is absorbed into the Anhydrous solid

• Decant the Ethyl Ethanoate into a clean, dry 50ml pear shaped flask

Stage Three Method:

• Add a few anti bumping granules to the pear-shaped flask

• Set up the apparatus for distillation

• Place the flask in a 250ml beaker which contains some water, and clamp it so the crude Ethyl Ethanoate is below the water line

• Weigh a clean, dry 100ml conical flask on an analytical balance. Record the mass of the empty flask in a suitable table

• Place the conical flask under the receiver

• Light the Bunsen burner and heat the flask in the hot water bath. Heat until the Ethyl Ethanoate is gently boiling

• As the Ethyl Ethanoate vapours start to carry over and condense, record the temperature of the vapours in a suitable table

• Record this temperature at the beginning and end of the distillation

• Distil the Ethyl Ethanoate until no more distillate comes over. There should be some liquid remaining in the round bottom flask. Never distil to the point of dryness

• Turn off the Bunsen burner

• Reweigh the conical flask with the distilled Ethyl Ethanoate

Analysis: Yield Calculations:

Identify the limiting reagent and the percentage yield from the limiting reagent.