20.00 g of cyclohexanol is massed out and 3.00 ml of concentrated phosphoric acid is added as a catalyst to the boiling flask.  Two boiling chips are added and the distillation can begin.   The cooling water for the condenser is turned on and the flask is heated gently so that the temperature of the vapor does not exceed 135oC. The heating is continued until all but 1 -2 ml of residue remain in the boiling flask and it turns a dark yellow

Chemistry
10th Edition
ISBN:9781305957404
Author:Steven S. Zumdahl, Susan A. Zumdahl, Donald J. DeCoste
Publisher:Steven S. Zumdahl, Susan A. Zumdahl, Donald J. DeCoste
Chapter1: Chemical Foundations
Section: Chapter Questions
Problem 1RQ: Define and explain the differences between the following terms. a. law and theory b. theory and...
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  • Procedure part 1:
    • Once the distillation is set up, 20.00 g of cyclohexanol is massed out and 3.00 ml of concentrated phosphoric acid is added as a catalyst to the boiling flask.  Two boiling chips are added and the distillation can begin.  
    • The cooling water for the condenser is turned on and the flask is heated gently so that the temperature of the vapor does not exceed 135oC.
    • The heating is continued until all but 1 -2 ml of residue remain in the boiling flask and it turns a dark yellow color.  At this point the heat is turned off and the remaining liquid is placed into a waste container.
    • In the receiving flask at the opposite end of the distillation apparatus, you will notice that the product appears in two layers. 
      • Question 1: Based on what we learned about the density of organic compounds, which layer is the organic layer (top or bottom)? Cyclohexanol + water

      •  Question 2: Looking at the reaction listed at the start of the lab, what two compounds are making the two layers? phopshoric acid + water

         

         
                                                                                                          

 

  • Procedure part 2:
    • At this point both layers of product are transferred to a separatory funnel.  To the contents of the separatory funnel, 1 ml of saturated NaCl solution and 2ml of 10% sodium carbonate are added to neutralize any side products that may be present in the flask with our product.  The Separatory funnel is then mixed and vented for a few minutes to ensure everything has fully reacted.
    • The funnel is then allowed to sit for a few more minutes to allow the layers to separate once again. The two layers are then separated by draining off the lower layer into one container and the top layer into another.  
    • Now that you have the organic product, you can weigh it and determine your final mass of product (actual yield) and your percent yield for the reaction.
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