Objectives:

 To get different fraction from the mixture where their driving force is their boiling point.
 To explain how distillation occurs.

Introduction:
Distillation is a method for separating a liquid from a mixture of two or more liquids. It is a
physical process used to separate chemicals from a mixture by the difference in how easily they
vaporize. For example, liquid ethanol can be separated from a mixture of ethanol and water by
distillation. This method works because the liquids in the mixture have different boiling points.
When the mixture is heated, one liquid evaporates before the other.

A water and ethanol mixture is heated in a flask using an electric heater. Vapour forms in

the air above the mixture in the flask.

One way to check the purity of the separated liquids is to measure their boiling points. For example,
pure ethanol boils at 78°C and pure water boils at 100°C.
When most of the ethanol has left, water vapour at 100°C passes into the condenser,
where it is cooled and condensed. Liquid water now drips into the beaker.

This method involves boiling the mixture at first, and the compound with the lowest boiling point
will start vaporizing. Let’s consider a mixture of two liquids. The vapour formed will be rich in
the compound which has the lowest boiling point. At this point, the temperature remains steady
until the fraction of the compound with the lowest boiling point in the liquid mixture reaches zero.
Thereafter, the temperature again starts to rise until it reaches the boiling point of the compound
with the highest boiling point. (Gil, Botia, & Ortiz, 2009)

In this experiment, methanol, water and butanol mixture are separated according to their boiling
points, with the one with the least boiling point vaporizing first and then collected in a small
beaker. Remaining liquids are collected in a similar way.
Theory:
The successful application of distillation techniques depends on several factors. These include the
difference in vapor pressure (related to the difference in the boiling points) of the components
present, the size of the sample, and the distillation apparatus. It also depends on the fact that the
liquid is relatively pure to begin with.
Heat is slowly applied to the distillation flask. The amount of heat to apply is determined by the
rate of distillation. The liquid should gently bubble and vaporize. As vapor rises from the liquid,
it raises the temperature of the apparatus. The vapor will fill the distillation flask and most of the
distillation head. The thermometer bulb should be completely surrounded by the vapor. If vapor
creeps past the thermometer bulb without contacting it, the measured boiling point will be low.
The vapor condenses and drips into the receiving flask via the condenser tube. Typically, the liquid
should drip into the receiving flask at a rate of about 15-20 drops per minute. If the rate of
distillation is too rapid, the distillation flask must be removed from the sand bath. With too rapid
a rate, the measured boiling point is likely to be inaccurate and the purity of the distilled liquid
will be decreased. If the liquid being collected has a low boiling point (<40oC) receiving flask
should be cooled using an ice-water bath. (Pahlavan, 2014)
As the liquid evaporates and the vapor comes into contact with the thermometer bulb, the
temperature rises. The temperature stabilizes at the boiling point and most of the liquid distills
over into the receiving flask. The temperature drops when almost all of the liquid has been distilled.

Figure: Boiling point of a pure substance as a function of amount of liquid distilled

Materials:
 Bolt head flask
 Thermometer
 Condenser
 Clamp-stand setup
 Methanol
 Butanol
 Distilled water
 Heating mantle
 Beaker

Procedure:
1. The boiling temperature of methanol, water and butanol are 67.4oC, 100oC and 118oC
respectively.
2. The simple distillation apparatus is setup which consists of Bolt head flask, thermometer,
condenser, clamp stand, heating mantle and a small beaker for collecting the condensate.
3. The mixture - consisting of 30ml of methanol, water and butanol each - is heated using
heating mantle, causing the temperature to rise until it reaches the temperature of the lowest
boiling substance(methanol), which is around 67.4oC, in the mixture, while the other
components of the mixture remain in their original phase in the mixture.
4. The resultant hot vapor passes into a condenser and is converted to the liquid. The
condenser(water-jacketed type) cools the vapor causing it to liquify (condense) and directs
this condensate into the receiving beaker. The vapor is then collected in a receiver beaker.
5. This process is continued until the temperature reaches around 100oC, when the receiver
beaker is replaced with another, ready to receive condensates of water when it boils at
100oC.
6. Procedure is continued for water and the vapor is collected in a receiver beaker until
temperature reaches around 118oC. The receiver beaker is replaced, and finally at 118oC
the remaining butanol is collected.
7. The 3 condensates collected are then taken for further testing to determine the refractive
index of each substance collected.
 8. The refractometer is first calibrated using distilled water.
9. Then a sample of methanol, water and butanol condensates collected are placed
respectively into the refractometer to determine the refractive index.

Calculation:
0.01
For methanol, Rf = 1.590 + ×7
20

=1.5935
0.01
For water, Rf = 1.36 + × 16
20

=1.368
0.01
For butanol, Rf = 1.320 + × 11
20

=1.3255

Result:
Rf of methanol, water and butanol are 1.5935, 1.368 and 1.3255 respectively.

Discussion:
About 20 ml of each component was collected after distillation. Some of the components were
evaporated out while some parts condensed on the surface of the apparatus. Other sources of error
arose due to the fact that temperature could not be properly maintained as heating mantle could
not maintain steady temperature at the boiling temperatures of each component of the mixture.
This might have led to some methanol being evaporated along with water and some water and
methanol too evaporating alongside butanol, resulting in contamination of the condensates of the
components thus introducing errors into the experiment. Otherwise, the apparatus and chemicals
provided were adequate to carry out this experiment.

References:
Gil, I., Botia, D., & Ortiz, P. (2009). Extractive Distillation of Acetone/Methanol Mixture Using
Water as Entraine. Industrial & Engineering Chemistry Research, 4858.
Pahlavan, D. (2014). Distillation of liquid mixtures.