TITLE: SIMPLE DISTILATION AND FRACTIONAL DISTILATION AT ATMOSPHERE AT PRESSURE

Aim/Objectives:
In this experiment you should be able to:

 Purify methanol (containing a solid, non-volatile impurity) by simple distillation

 Separate a mixture of acetone (propanone) and xylene by fractional distillation

Introduction:
Liquids may be purified by the process of distillation. The liquid is boiled and the vapour which is formed is
pass through a cooled tube, known as a condenser. The vapour condenses back to liquid (the distillate) which
is collected in another vessel. Simple distillation may be used for purification of a liquid containing non-volatile
solute impurities.

The boiling point of a liquid is the temperature at which its vapour pressure equals the atmospheric pressure.
Thus the boiling point is variable, depending on the pressure of the atmosphere above it. If the pressure above
the liquid is very much lowered (by evacuating the distillation system with the water pump or oil pump) then
the boiling point will be lowered very considerably because of the much lower temperature at which vapour
pressure becomes equal to the reduced pressure above the liquid. This technique is known as vacuum
distillation and useful for purifying liquids, which at atmospheric pressure, have very high boiling points (e.g.
above 200˚C). To avoid decomposition of organic liquids it is desirable to avoid heating them to high
temperatures and vacuum distillation allows purification to be achieved without the need for excessive
heating.

In a mixture of two or more volatile liquids, all components contribute to the vapour pressure. When the
combine vapour pressure equal to that of the atmosphere above the liquid then distillation takes place and
the distillate is the mixture of original components. That component which is more volatile (ie. Has the highest
vapour pressure at any given temperature) will form the major part of the distillate and it is usually possible to
split the distillate into fractions by changing the receivers at intervals. In this way a partial separation is
possible. The process is made more efficient by allowing the vapours to pass up a vertical fractionating column
before collecting them. The fractionating column serves to hold back the higher boiling components until most
of the more volatile liquid distilled over. Then the receiver is change and the next most volatile component
begins to be collected.

Obviously, it is more difficult to separate liquid mixture when the components have the similar boiling points
(e.g. 80˚C, 83˚C and 88˚C) because they have similar vapour pressure at a given temperature. When the
component of the mixture have very different boiling points it is, however often possible to separate them
easily into pure fractions.

Materials/Apparatus and Chemical Reagents:

1.) Thermometer 4.) Clamp 7.) Three-way adapter 10.) Ice bath

2.) Condenser 5.) Receiving flask 8.) 30 cm3 of acetone-xylene mixture 11.) Heat source

3.) Distilling flask 6.) Vacuum adapter 9.) Boiling chips

PART A. DISTILLATION OF METHANOL
Procedures:
The typical set up of the experimental design conducted was indicated by the simple diagram on the next page
with specific apparatus used being clearly drawn.

The distillation apparatus from the equipment supply have been assembled or collected and set up as checked
by the demonstrator. A measuring cylinder was used to collect the distillate.

25 cm3 of methanol (coloured by a solid impurity) was placed in the distillation flask with addition of two
boiling chips. The flask was heated gently until the liquid started to boil.

After few minutes, the water condensed and ran down the condenser and was collected in the measuring
cylinder. The temperature when the distillation first occurred was taken every time so as every 5cm3 volume
being recorded as well. The heat was applied continually until maximum volume of 20cm3 has been reached.

 A complete, entire set up of simple distillation

Results:
The temperature and the volume of the distillate collected was shown in the table below.

Temperature (˚C) 30 44 66 66

Volume (cm3) 5 10 15 20
 Distillation of Methanol
70

60

50
Temperature (˚C)

40

30

20

10

0
0 5 10 15 20 25 30
Volume (cm3)

Percentage of methanol obtained:

25mL-5mL=20mL/25mLx100= 80% (exactly done)

30mL-5mL=25mL/25mLx100= 100 %( estimation)

Discussion:
From the graph it is seen that the temperature rises with respect to the volume and then remain constant all
throughout the entire state when the distillate is 15 mL and above at 60˚C maximum temperature. In a simple
sense of mind we know that the impurity used (Boiling chips) does not change the boiling point of methanol
why because the theoretical value of the boiling point of methanol alcohol is around 64.7˚C and so to see if it
has any effect on the boiling point of methanol, the normal boiling point 64.7˚C or experimentally determined
boiling point 60˚C should be increasing up to say 80˚C and above. In this way we can reason out that the
impurity has an impact on the boiling point of methanol.

Otherwise straight from the graph when the heat was applied the boiling temperature is 30˚C and it is equal to
atmospheric pressure outside that is likely to boil. We can also calculate the percentage of pure methanol
obtained from the given volumes on the graph that maintains a constant temperature. As shown in the result,
we only obtained 80% of pure methanol and that leads us to determine the boiling point of methanol be
exactly 60˚C. So we are just few figures away from the theoretical value. Only if we discontinue heating at
30mL/cm3 we may get that 100% which will be at normal boiling point of 64.7˚C which is the theoretical value.

PART B. FRACTIONAL DISTILLATION OF AN ACETONE-XYLENE MIXTURE

Materials/Apparatus and Chemical Reagent: (which not listed in part-A)

1.) 30cm3 of Acetone-Xylene mixture 4.) Standard vapour glassware

2.) 100 mL round-bottom flask

3.) Fractionating column

Procedures/Methods:

A complete set-up of fractional distillation

Acetone-Xylene mixture

The male joints on the standard vapour glassware was lightly greased and the 100 mL round-bottom flask was
then clamped to a ring stem bath. The steam bath has been set on the base of the ring stand and the weight
that was attached to the ring stand is now directly over its base. Hence, the apparatus is being prevented from
tipping over.

The distillation head was inserted in the top of the distillation flask and the clamp on the flask was adjusted so
that the apparatus is exactly vertical. The second joint of the distillation head was attached with the condenser
and was clamped to the ring stand. The condenser was set at an angle that is perfect to permit the flows of
distillate into the receiving flask.

The vacuum take-off adapter and the receiving flask have been attached and clamped in place as shown in the
diagram. This clamp was then connected to the ring stand to hold the condenser or to a third ring stand. A
rubber band was used around the vacuum adapter and the water inlet tube to hold the adapter in place after
changing the receiving flask.

The thermometer was carefully inserted into the thermometer adapter with a small amount of lubricant on
the rubber seal. The height of the thermometer was adjusted so that the bulb at the thermometer was now
below the side-arm of the distillation flask. After done with the arrangement, the thermometer responded to
the temperature of the hot vapour as it goes into the condenser.

The rubber tubing was attached to the inlet (bottom) and outlet (top) of the condenser and slowly water is
being put on. The water kept flowing through the condenser at a very slow stream. All joints was fitted tightly
as well as all parts are being securely clamped.

Results: