Distillation of Mixture of Ethyl Acetate and Butyl Acetate

Distillation of Mixture of Ethyl Acetate and Butyl Acetate

Purpose:

To separate two organic liquids, ethyl acetate and butyl acetate by simple and fractional distillation. With separated organic liquid Gas Chromatography is used to analyze subject.

Chemical Equation:

Ethyl Acetate Butyl Acetate

Procedure:

Obtain 10-ml ethyl acetate and 10-ml butyl acetate, and place into 50-ml the distilling flask with a magnetic stir bar inside. Compile the fractional distillation setup with a 10-ml graduated cylinder as the collecting flask. For warmth purposes wrap tin foil around the vertical column coming from the 50-ml distilling flask. Obtain a heating mantle, which should be placed under the distilling flask and variable power supply for heating of the distillation and turn to 50 percent. Once boiling is detected drops will be start to collect in the graduated cylinder. Ideal distillation rate of 1 drop per second should be obtained by increasing the heat on the power supply but never surpassing 65 percent. As distillate is collected record the temperature of every 1 ml of solution until 10 ml is collected. Take the 10 ml distillate to the Mini GC, which should be turned on. Obtain a glass syringe and acetone and fill the syringe with 1/3 full of acetone. Remove the liquid onto a paper towel. Next, collect 0.20 L of distillate liquid in the syringe. Insert the needle in the injection port of the Mini GC. Add the distillate into the injection port while pressing collect at the same time to start data collection. Once the distillate is added the needle should be taken out as soon as possible. The data will be present within 6 minutes and should be analyzed by looking at peak integration, retention time, and peak area.

Calculations:

Corrected Boiling point (71.20-77.90) * 1.03 = 73.40 - 80.20 OC

Discussion:

During distillation, the temperature of each millimeter of distillate collected was recorded, shown in the following table:

Measured Temperature OC Corrected Temperature

Volume (ml) Without Beads With Beads Without Beads With Beads

1st drop 71.2 OC 74.1 OC 73.3 OC 76.3 OC

1st ml 74.5 OC 74.5 OC 76.7 OC 76.7 OC

2nd ml 76.1 OC 74.8 OC 78.4 OC 77.0 OC

3rd ml 76.5 OC 74.9 OC 78.8 OC 77.1 OC

4th ml 76.9 OC 75.0 OC 79.2 OC 77.3 OC

5th ml 75.0 OC 75.0 OC 77.3 OC 77.3OC

6th ml 75.1 OC 75.1 OC 77.4 OC 77.4 OC

7th ml 75.9 OC 76.9OC 78.2 OC 79.2OC

8th ml 74.9 OC XX 77.1 OC XX

9th ml 74.1 OC XX 76.3 OC XX

10th ml 77.9 OC XX 80.2 OC XX

Looking at the temperature throughout the distillation process they remain fairly