Simple Distillation Lab Report

Procedure: The addition of 4.0 mL cyclohexanol, 1.0 mL of 85% phosphoric acid, and one boiling chip, were all added to a 10 mL round bottom flask that would be attached to the end of an assembled simple distillation set up. A sand bath was placed atop a hot plate, and the simple distillation mechanism was lowered into the sand bath with the bottom most piece (the 10 mL round bottom flask) submerged about half way. The distillation process was completed after a sufficient amount of liquid distillate had accumulated within the Hickman Still Head. Smaller volumes were removed from the Hickman Still Head and into a clean test tube with a Pasteur pipet until only 1 mL - 2 mL of the distilled mixture remained in the round bottom flask and all
A Pasteur pipet was used to remove the bottom most aqueous layer that should have formed in the test tube containing the distillate product. Calcium chloride pellets were added to the test tube following the initial removal of the aqueous layer to ensure full removal of water. A 3 mL vial was weighted and weighed again with the addition of the product from the test tube in the vial to provide actual yield data that would be used later on in quantitative analysis of percent yield of cyclohexene. Lastly, a bromine test was carried out to quantitatively test the presence of cyclohexene product in the prepared sample. A total of 2-3 drops of 3% bromine in dichloromethane was added to a new test tube as well one drop of the prepared cyclohexene. Upon observing a color change from brown to clear, one can confirm the presence of cyclohexene in the obtained
The observable change in color was due to the fact that the bromine was used up when reacting with the prepared cyclohexene, which to yield 1,2-dibromocyclohexane product. Quantitatively, the calculation of percent yield being 77.43% indicates that the overall success was sufficient although not excellent. It may be noted that during the step in which the distillate bottom layer was to form at the bottom of the test tube that it was transferred into, there was never a distinct layer formed and estimated minimal amounts were removed before adding the calcium chloride pellets to aid in removing all excess water. This unclear removal of the aqueous bottom layer may have affected overall purity and information regarding actual yield that was