Lab 1: Distillation (Exp.

3105-1)
Nate Hall (w/Kevin Guerra), Chem 3105
T.A.: Wei Ma
Purpose: To attempt to completely distill methanol from a 50-50 methanol-water mixture using
both the simple and fractional distillation techniques. Distilling utilizes the difference in boiling
points between water and methanol to boil out all of the methanol, which is then condensed
again.
Physical Properties Table (there is no reaction here):
Compound

MW (g/mol)

Amount

bp(C)

Methanol (CH3OH)

32.05

20.0 mL

65

Water (H2O)

18.02

20.0 mL

100

Safety:
Methanol (flammable, toxic, carcinogen)
- toxic if inhaled, touching skin, or ingested
- very flammable
- can cause irreversible effects
- wear goggles and gloves
Procedure:
1. Set up one of the following apparati. For simple distillation:

Notes: use a 100 mL round-bottomed flask for the distilling flask, and a a 50 or 100mL
graduated cylinder for the receiving flask
For fractional distillation:

2. Clamp the apparatus securely, but do not strain the glass, and set up the distilling flask on a hot
plate for heating.
3. Add 40 mL of the sample solution to the distilling flask.
4. Add a boiling chip and heat until the solution boils to a rate of roughly three drops per second
into the graduated cylinder. (DO NOT put the plate on high heat)
5. At every 2 mL of methanol distilled, have one person record the temperature at that particular
volume, until the temperature tops off at somewhere around 100C
6. At the above temperature mark, stop the distillation, so the flask is not boiled to dryness
7. Clean up, wash hands, etc.
8. Graph the results as Temp (C) vs. Volume of Distillate (mL) (y vs. x), showing both the
fractional and simple result curves

Data Tables/Graph:
Fractional
Distillation

Fractional vs. Simple Distillation (Temp. vs. Volume of Methanol Distilled)

100
95
90
Fractional

Polynomial (Fractional)

85
80

Temp (C)

75
70
65

Simple
60

Polynomial (Simple)

55
50

10

15

20

25

30

Volume of Methanol Distilled (mL)

Methanol
Distilled (mL)
2
4
6
8
10
12
14
16
18
20
22
Simple
Distillation
Methanol
Distilled (mL)

Temperature
(C)
65
67
70
72.5
73
75
76
78
82
88
99

Temperature
(C)
2
70
4
75

6
8
10
12
14
16
18
20
22
24

78
80
81
83
85
89
93
94
95
96

Conclusion:
The simple distillation that was attempted was relatively successful. The distillation
should have produced a somewhat impure distillate, since the boiling points for water and
methanol are 35C apart (simple distillation works best when the boiling points of the
substances are further apart, a difference of 30-40 is a minimum). This was true, as the
distillate collected exceeded 20 mL (half the original solution) before the temperature reached
100C, which means that some water must have also boiled off into the vapor to make up the
extra 4 mL or so, resulting in a slight impurity. The fractional distillation had a higher success
rate, which makes sense considering its higher efficiency with substances that have less
difference in boiling point. Adding the fractioning column however also results in a longer time
taken to distill the methanol out, as shown by the slower increase in temperature on the graph.
The fact that neither distillation reached 100C can be explained by not having the
thermometer bulb low enough during the experiment. If the bulb is not low enough, the
temperatures that are being measured are those of vapor having more time to condense and
lower in temperature. This effect could also account for the temperatures being a little lower
than expected at the 20 mL mark.
Post-Lab Questions:
1.
a) Higher atmospheric pressure results in a higher boiling point. Boiling occurs when
vapor pressure of a liquid equals atmospheric pressure. The higher atmospheric
pressure would require a higher vapor pressure, which can be achieved by add more
heat, or reaching a higher boiling point.
b) An uncalibrated thermometer would read temperature at a shifted value. So 100C
might read as 95C, or 110C. This would make the boiling point of water seem lower or
higher, respectively, to a viewer. However, the true boiling point of the water would
remain the same.
c) Rate of heating would have no effect on the boiling point. Boiling point only depends
on pressure, so changing the temperature faster would only allow one to reach the
boiling point quicker, not change it altogether.
2. Fractional distillation is more effective the more theoretical plates it creates with the
surrounding material. Having a packed column creates a lot of surface area, which
increases the plates in comparison with an unpacked column. However, the column
holdup that becomes an issue in both of the prior types of fractional distillation columns
is further reduced by having a spinning band column, since the bands send condensed
vapor to the distillation flask.

3.

a) Not adding boiling chips would make the boiling solution much more chaotic and
turbulent, which might allow some of the unseparated solution to spew into the
condenser and then into the distillate container.
b) Heating the flask too quickly can result in a higher impurity of the distillate, since the
vapor will move faster through the system, and could carry some of the other substances
with it.