Exercise No.

6: Volatility:
Distillation and
Determination of Boiling
Point
Introduction

Volatility is the relative ease with which a substance passes from the liquid to
the gaseous (vapor) state. To escape from the liquid into the gaseous state
an individual molecule requires energy – to break away from other liquid
molecules, and to maintain the vigorous movement characteristics of a
gaseous particle. The amount of a substance that is present as gas in the
space above the surface of the liquid contained in a closed vessel is
measured by its vapor pressure, which increase with temperature.
Evaporation is slow volatilization by the escape of surface molecules from
the liquid into the air. Boiling is the fast volatilization of a liquid; the
turbulence observed is due to the formation of vapor even in the body of the
liquid. Boiling occurs when the vapor pressure is equal to the atmospheric
pressure, and the temperature required for this quality is called the boiling
point. The less volatile a liquid is, the higher in its boiling point.
Distillation is the process of vaporizing a liquid and converting the vapor to
the liquid state by cooling. The sample mixture (generally a solution) is
heated to sustain boiling, and the vapor allowed to pass through a cooling
tube where it condenses to form the distillate. Thus distillation serves to
separate the volatile from the non-volatile component of a mixture.
If the original liquid sample contains only one volatile component, the vapor
produce will consist of this component alone, and its temperature will be near
the boiling point of the latter. (At a given pressure, the boiling point of a pure
liquid is a characteristic constant and serves as a clue to its identity, just as
the melting point does for a pure solid). Mixture containing two or more main
components that are volatile give a mixed vapor, the composition of which
depends on the relative volatility of these components and their respective
concentrations in the liquid phase. As distillation proceeds, the vapor
composition changes towards increasing concentration of the less volatile
component(s) as indicated by the variation of the vapor temperature.
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For instructional purposes only • 1 Semester SY 2020-2021 25

Learning Outcomes

1. To separate a mixture of substances using distillation.

2. To determine the boiling point of a liquid.

Figure 11 Distillation

DISTILLATION

Materials

 Hot plate Acetone Condenser

 Iron stand w/ clamp Methanol Watch glass
 50 mL grad. Cylinder 1-butanol Thermometer
 50 mL distilling flask Ethyl acetate 50 mL beaker
 Wash bottle Medicine dropper

Procedure

A. Comparison of Volatility by Rate of Evaporation

Arrange 5 small clean dry watchglass in a row on the bench

top. Near each, place a piece of paper as label to indicate the
compound under examination:

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 26 CHEM 120.1: Organic Chemistry Laboratory

a) acetone c) water
b) methanol d) 1-butanol e) ethyl acetate

When ready, place the two drops of the compound to be tested in the
center of the watch glass, and immediately note time on the label.
When the liquid has completely disappeared, note down the time
again.

B. Distillation of Water from Dissolved Non-volatile Solids; Boiling Point

Determination

Place 30 mL ordinary tap water in a 50-mL distilling flask, taking care

that no liquid enters the side arm. Add a piece of porcelain plate to
prevent bumping,and assemble the rest of the distillation apparatus.
The tip of the thermometer bulb should be in the center of the flask
neck, about 5 mm below the side arm. Check all connections for
tightness and turn the water on the condenser.(Figure 13). Heat the
flask contents to boiling, then adjust the flame to the condensate falls
from the condenser, and at the rate of one drop in 5 sec. Watch the
thermometer, when the volume of the distillate is 3 mL, then at each
succeeding 3-mL interval until a total of 15 mL has been collected.
The boiling range of water is the temperature indicated at the first
drop and at the last drop collected, provided the distillation has
proceeded at a steady rate.

---------------
1. The watchglass are to be used in succession by each group in
the class, and should be turned over clean and dry, as soon as
possible.
2. Bumping is the term given to irregular boiling, whereby the liquid
alternates between relative calm and violet motion, which may
lead to spillage.
3. Rate of heating must be controlled to avoid superheating of the
vapor. Add 50 mL of water and 2.4 g of calcium carbonate to the
beaker containing the tea. Boil the mixture gently on a hot plate
for 10 min.

Guide questions and instructions on how to prepare

and submit the laboratory

1. What does temperature of water obtained at the first drop and at the
last drop indicated?

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and innovative technologies for sustainable communities and environment. No. DOPAC-IM-
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For instructional purposes only • 1 Semester SY 2020-2021 27

2. Explain why the observed boiling point for the first drops of distillate
collected in the simple distillation of a 1:1 molar solution of pentane
and hexane is above the boiling point of pentane.
3. Arrange the following compounds in order of increasing boiling point:
pentane, octane, hexane, 2-methyl pentane. Offer an explanation for
your arrangement.
4. Water boils at 100°C at sea level (p = 1 atm). Assuming you are out
camping up the peak f Mt. Pangasugan, will the boiling point of water
be higher? Lower? Or remains the same. Explain.
5. Arrange the following compounds in order of decreasing volatility:
acetone, methanol, ethylacetate, 1- butanol and water. Give the basis
for your arrangement.

This guide questions will serve as your quiz and to be submitted along
with your lab report. The laboratory report sheets provided will be
submitted by the student after every exercise through email or courier.
See abridged for the schedule of submission.

Additional Resources

Use References style here

References

A. M. Acabal, A. D. Acabal, G. Albarico, K. Bandibas, Y. Bandibas, C. Calibo, J. G. Jansalin, Ma.

T. Loreto, E. Quevedo, A. Ramal, M. A. Villar and R.A. Villaber, Chem 120.1 Organic
Chemisty (Laboratory)[Laboratoty Manual]

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Vision: A globally competitive university for science, technology, and environmental conservation.
TP-IMD-04
Mission: Development of a highly competitive human resource, cutting-edge scientific knowledge V0 07-15-2020
and innovative technologies for sustainable communities and environment. No. DOPAC-IM-
SC003.1