Boiling point and Distillation

Objective
1. To determine the boiling point of organic compounds using semi-microscale method
2. To set up distillation equipment and carry out the experiment for isolating liquid
sample
Introduction
As a liquid is heated, its vapour pressure increases to the point at which it just equals
the applied pressure (usually atmospheric pressure). At this point, the liquid is observed to boil.
The normal boiling point is measured at 760 mmHg (760 torr) or 1 atm. At a lower applied
pressure, the vapour pressure needed for boiling is also lowered, and the liquid boils at a lower
temperature. The relation between applied pressure and temperature of boiling for a liquid is
determined by its vapour pressure-temperature behaviour as shown in Figure 1.1

Figure 1.1 The vapour pressure-temperature curve for a typical liquid.

When you have large quantities of unknown liquid, you can simply record the boiling
point (or boiling range) as viewed on a thermometer while you perform a simple distillation.
Alternatively, you may find it convenient to use a direct method as shown in Figure 1.2. With
this method, the bulb of the thermometer can be immersed in vapour from the boiling liquid
for a period long enough to allow it to equilibrate and give a good temperature reading. With
smaller amounts of material, you can carry out a microscale or semi-microscale determination
of the boiling point by using the apparatus shown in Figure 1.2.

A) B) C)

Figure 1.2 Boiling-point determinations by A) macroscale, B) semi-microscale and C)

microscale methods
Distillation is the process of vaporising a liquid, condensing the vapour, and collecting
the condensate in another container. This technique is very useful for separating a liquid
mixture when the components have different boiling points or when one of the components
will not distil. It is one of the principal methods of purifying a liquid. Four basic distillation
methods are available to the chemist: simple distillation, fractional distillation, vacuum
distillation (distillation at reduced pressure), and steam distillation. Here we describe only
simple distillation method.
A typical modern distillation apparatus is shown in Figure 1.3. The liquid to be distilled is
placed in the distilling flask and heated, usually by a heating apparatus such as heating block,
heating mantle, sand bath on hot plate or Bunsen burner. The heated liquid vaporises and is
forced upward past the thermometer and into the condenser. The vapour is condensed to
liquid in the cooling condenser, and the liquid flows downward through the vacuum adapter
(no vacuum is used) and into the receiving flask.
Material
1. Distillation equipment consists of distillation flask, distillation head, thermometer
adapter, water condenser, vacuum adapter and receiving flask
2. Clamp
3. Hot plate
4. Sand bath
5. Contaminated ethanol
Safety and disposal
1. Safety during distillation is all about safe heating, well secured apparatus and
attention to the rate of heating
2. All organic chemicals in this experiment MUST be disposed in waste container.
 Figure 1.3 Distillation set up with the standard glassware and equipment.
Experimental procedure
You can see the distillation video from LabSkills software. Briefly, pour the unknown
solution into a round bottom flask about half of it and add anti-bumping granules. Place the
hot plate onto the clamp stand and top with a sand bath. Clamp the round bottom flask
around the joint and then place the still head into the neck of the round bottomed flask. Fit
the condenser onto the side arm of the still head and secure lightly with a clamp. Then fit the
receiver adapter to the end of the condenser and secure with clip. Fit a small round bottom
flask to the end of the receiver adapter and secure with another clip. Alternatively place a
beaker or conical flask under the receiver. Add the thermometer in an adapter through the top
of the still head. Make sure that the thermometer bulb is in the correct position, opposite the
entrance to the condenser. Turn on the water for the condenser making sure it goes in at the
low end and out at the high end. Turn on the hot plate, the solution will heat up and begin to
boil. It will begin to condense at the side arm and start to drip into the collection flask. Note
boiling temperature when the thermometer shows a constant temperature. Collect the
distillate that condenses over at the boiling point. Make sure there is still some solution left in
the round bottom flask as you should never heat until dry. Turn off the hot plate and leave to
cool before dismantling the distillation apparatus.
Chemical Hazards

Ethanol
Reference
Engel, R.G., et al. Introduction to Organic Laboratory Techniques: A Small Scale Approach,
Brooks/Cole CENGAGE learning, 3rd edition (2011): 179
LabSkills Software