Experiment 4

Distillation: Saparation and purification of organic liquid.

Nabaa Hussian Mubarak

202209097
CHEMY221
Department of Chemistry
University of Bahrain
Aim
1- Distillation of a two-component mixture by simple and fractional distillation
method
2- Compare the efficiency of simple and fractional distillation by evaluating the
separation of mixtures

Introduction
Discovery that dilute solutions of alcohol resulting from fermentation can be separated
into other parts specific to alcohol and others desired by students by heating the
solution until boiling and condensing the vapour (distillation method).
Distillation is a process involving the conversion of a liquid into vapour that is
subsequently condensed back to liquid form.
Normally ethanol boils at 78 °C and water at 100 °C, but when you heat a mixture of
ethanol and water, the water in it boils at a temperature close to 87 °C, and the steam
above it is not 100% ethanol.
Pure liquids (cyclohexane and toluene) boil at 78 and 111 °C, respectively, and thus the
temperature of the liquid and the temperature of the vapour are equal, which means
that the temperature of the vapour remains constant throughout the distillation process.
Raoult's law states that the vapour pressure of cyclohexane is equal to:
Pc = P°c * Nc
Pc is is partial pressure of cyclohexane.
P°c : is the vapour pressure of pure cyclohexane.
Nc: is the mole fraction of cyclohexane in the mixture.
Also the total vapour pressure above the solution:
Pt = P°t * Nt
Dalton's low:
Xc = Pc / total vapour presser
Observations and calculations:

Without column

With column
2. From the distillation curves, estimate the volume of liquid boiling below 85°C with
and without a column.
Without column = 7 ml
With column = 9 ml
3. Which procedure was more efficient at separating the mixture into its components?
Separation with column
4. A pure liquid has a constant boiling point, but a liquid with a constant boiling point is
not necessarily pure. Explain.
Because the pure liquid consists of only one substance, and through the properties of
this substance, its boiling point is determined.
5. What effect does a reduction in the atmospheric pressure have on the boiling point of
a liquid?
It leads to lowering the boiling point of the liquid, and this is due to the boiling
temperature being equal when the vapor pressure of the liquid is equal to the
atmospheric pressure.
6. Why doesn't a pure liquid in a distilling flask vaporize all at once when the boiling
temperature is reached?
Because the boiling process is gradual, when the liquid reaches the boiling point, the
particles begin to gradually release as the boiling point increases.
7. Why is it dangerous to heat a liquid in a distilling apparatus that is closed tightly at
every joint and has no vent to the atmosphere?
Because the pressure inside the device can build up to dangerous levels, when the liquid
is heated, the molecules begin to release, and thus the volume of the gas increases,
which leads to a buildup of pressure inside the device, and when the pressure exceeds
the limits, it may cause an explosion or rupture of the container.
8. Why is it important that the cooling water in a distillation apparatus enter the
condenser jacket at the lower end and exit at the upper end, and not vice versa?
Due to the principle of heat exchange and cooling efficiency, if water enters from the
lowest point, the condenser will be permanent filled with cold water to ensure effective
cooling. So the water should always flow to the condenser at its lowest point and out at
its highest point.
9. Why should a distilling flask be filled to not more than two-thirds of its capacity at the
beginning of a distillation procedure?
To prevent the liquid from boiling and to leave enough space for steam to form and rise.
If the flask is full, the boiling liquid may cause foam or strong bubbles, which leads to
contamination of the still or the liquid splashing out of the flask.

Discussion
Distillation is the process of converting a liquid into vapor and then condensing it back
into a liquid.
In the first part of the experiment, which it is a simple distillation, it is the separation
method used to separate the solvent from the solution.
At first, 15 ml of hexane was taken in a round-bottom flask, and 2 anti-bumping
granules were added. Then, it was heated until the hexane boiled. The temperature was
adjusted to 68 °C to maintain a constant dripping rate. Initially, the temperature of the
solution rose from 61°C to 64°C and then stabilized. This indicates that the solution is
very pure, as its temperature did not change.
Also, equal amounts of toluene were mixed with the purified hexane from the first part
(10 ml of each) and then it was placed on the distillation device and the temperature
was set to approximately 68°C. At the beginning of distillation, the first 2 ml of the
distilled solution was not counted due to a difference. The boiling point between hexane
and toluene, as the boiling point of toluene is much higher than that of hexane, so
hexane begins to evaporate first because it boils at a lower temperature, and the first 2
ml of the solution is not counted because it usually contains a higher amount of hexane.
When the volume of the distilled solution reached 8 ml, the distillation stopped, and we
had to raise the temperature to 100°C to continue the distillation. Thus, the
temperature of the mixture consisting of hexane and toluene.
In the second part of the experiment, which is fractional distillation, it is very
similar to simple distillation, but differs in that it contains a steel column, and the
main purpose of this column is to separate the materials from each other.
In this part, in the beginning, equal amounts of toluene were also mixed with
hexane (10 ml of each) and then it was placed on the distillation device and the
temperature was set to approximately 68°C. Thus, the temperature of the solution
also increased, but when the volume of the solution reached... Distilled 6 ml, the
distillation stopped, which forced us here also to raise the temperature to 100°C to
continue the distillation until it reached 16 ml, and the temperature of the solution
was approximately 110°C.
The errors that may occur in the experiment is a the increasing in temperature, or the
temperature may be read incorrectly from the thermometer, or the separation of the
components may also be incomplete.

CONCLUSION
The aim of the experiment was achieved as we learned the comparison between the
two types of distillation and we discovered that partial distillation is more efficient due
to the presence of the steel column that separates the materials and on which the vapor
condenses and then evaporates and then condenses again. For this reason, the
compound is distilled many times.