Distillation

Purpose: To determine whether simple or Iractional distillation is more eIIective at puriIying a

liquid.

Theory:
The boiling point oI a pure liquid is deIined as the temperature at which the vapor pressure oI the
liquid exactly equals the pressure exerted on it by the atmosphere and is one oI its characteristic
physical properties. The boiling point is used to characterize a new organic liquid, and
knowledge oI the boiling point is used to compare one organic liquid with another, as in the
process oI identiIying an unknown organic substance. The boiling point oI a mixture is a
Iunction oI the vapor pressures oI the various components in the mixture. Impurities either raise
or lower the observed boiling point oI a sample, depending on how the impurity interacts with
the compound Ior which the boiling point is being measured.

In a simple distillation, only one vaporization and condensation occurs. This process would not
eIIectively separate a mixture oI multiple organic compounds. The Iirst vapor that condenses will
contain a large portion oI the more volatile compound, but also a small portion oI the other
compound. As additional vapor condenses into the receiving Ilask, the boiling point oI the
remaining mixture continues to increase.

In a fractional distillation, many vaporizations and condensations occur. Fractional distillation is
equivalent to multiple simple distillations. The Iractionation column is packed with glass beads
in order to give the maximum possible surIace area Ior vapor to condense on. Each time the
vapor condenses to a liquid it will trickle back down the column and will be reboiled by the new
vapor. This causes the vapor to be richer in the more volatile compound, whereas the liquid will
become increasingly richer in the less volatile compound.

Procedure:
Simple Distillation:
1. Set up a simple distillation apparatus with a 50 mL round bottom Ilask
2. Pack glass wool between your Ilask and the heating mantle
3. Adjust thermometer bulb and wrap the adaptor.
4. Collect your distillate in a 50 mL graduate
5. Place boiling chips in the Ilask and add 30 mL oI the hexane/toluene mixture
6. Measure the temperature every 2 mL.

Fractional Distillation
1. Fill a large diameter condenser (Iractionating column) with glass beads
2. Set up the heating mantle with glass wool and a 50 mL round bottom Ilask
3. Adjust the thermometer bulb just below the side arm oI the adapter
4. Place boiling chips in the Ilask and 30 mL oI mixture
5. Wrap column
6. Save three Iractions
a. Collect the Iirst 2 mL in a 10 mL graduate place in vial
b. Collect 12 mL in a 50 mL graduate
c. Collect the next 2 mL in a new 10 mL graduate place in vial
d. Collect 8 mL in the same 50 mL graduate
e. Save the pot residue in a vial

Data/Calculations:
Temperature (C)
Amount collected (mL) Simple Distillation Fractional Distillation
2 75.0 66.0
4 76.0 67.0
6 77.0 68.0
8 79.0 69.0
10 80.5 70.0
12 82.0 71.0
14 89.0 74.0
16 98.0 106.0
18 101.0 108.0
20 108.0 109.0
22 109.0 109.0
24 110.0 109.0
26 113.0 -


Results and Conclusions:
The results show that Iractional distillation is Iar more eIIicient than simple distillation. In the
simple distillation the vapor Iormed by boiling the compound is a mixture oI all oI the
components. In the Iractional distillation the glass beads allow the less volatile component to
recondense while the more volatile component rises to the condensing tube. When the results oI
both distillations are graphed next to an ideal distillation curve, the Iractional distillation is very
accurate in comparison to the simple distillation.

Comments:
Using the Iractionating column was interesting. Learning Iractional distillation will allow Ior
more eIIicient experiments in the Iuture instead oI having to do multiple simple distillations.