Name : ______________________________________________________ Partners Name :______________________________________

Group: _________ Date: ___________

PRACTICAL 9
Esterification
Aim
To make an ester and purify it.

Chemicals and apparatus needed:

Quick-fit apparatus Separating funnel Retort stands and clamps Conical flask Measuring cylinder 1-Butanol Ethanoic Acid (Glacial acetic acid) Concentrated sulfuric acid 0.5M sodium carbonate solution Fused calcium chloride

Instructions:
1. 2. 3. 4. 5. 6. 7. 8. 9. 10. Place about 20 mL of the 1-butanol and about 20 mL of ethanoic acid (glacial acetic acid) in the round bottom flask. Slowly add about 1 mL of concentrated sulfuric acid and a few granules of boiling chips. Reflux mixture for about 30 minutes. Carefully adjust the flame for steady boiling. After the refluxing process, transfer the reaction mixture into a container (reagent bottle) provided. Pour the cool mixture into the separating funnel, which contains about 40 mL of water. Stopper, shake and allow layers to separate. Check which is the aqueous layer and discard it. Repeat washing process of the organic layer in the separating funnel, this time with about 40 mL of sodium carbonate solution. Discard the aqueous layer. Repeat the washing with water. Add the organic product to a small dry and clean conical flask with some fused calcium chloride. Stopper, swirl and allow to stand for 10 minutes. Decant the organic liquid into a clean dry round bottom flask. Add some boiling chips and distill the ester. (Boiling point of 1-butyl acetate = 126.5C) Record the boiling range, odour and appearance of distillate.

Complete the report for this experiment: Title, aim, procedure, observations and results, questions and conclusion.

SAFETY Concentrated H2SO4 (aq) is caustic. Addition of H2SO4 (aq) to be done in fume cupboard. Observations and results Boiling Range of distillate = Odour of distillate = Appearance of distillate =

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Questions 1. Write an esterification equation for this experiment.

2. Identify the water inlet and water outlet in the diagrams below and draw a thermometer for second diagram at the appropriate place.

3. Briefly describe the purpose of adding the 40 mL of sodium carbonate solution to the separating funnel

4. Write the related chemical equations in 3.

5. Briefly describe the purpose of anhydrous calcium chloride in the experiment.

Conclusion

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