CMT 200

Experiment 1
SIMPLE EQUILIBRIUM DISTILLATION

NAME :

STUDENT I.D
Abstract:

In this experiment, an unknown mixture was separated using simple distillation

techniques. Graphs of temperature vs time of distillate collected showed the changes in
vapor temperature in each minutes. The unknown mixture is determined by the boiling
point of first distillate and second distillate. First distillate was 2-methylpropan-2-ol and
second distillate was 2-methyl-2-butanol.

Introduction:

Simple distillation is a procedure by which two liquids with different boiling points
can be separated. Simple distillation can be used effectively to separate liquids that have
at least fifty degrees difference in their boiling points. As the liquid being distilled is
heated, the vapours that form will be richest in the component of the mixture that boils at
the lowest temperature. Purified compounds will boil, and thus turn into vapours, over a
relatively small temperature range (2 or 3°C); by carefully watching the temperature in
the distillation flask, it is possible to affect a reasonably good separation. As distillation
progresses, the concentration of the lowest boiling component will steadily decrease.

Eventually the temperature within the apparatus will begin to change; a pure
compound is no longer being distilled. The temperature will continue to increase until the
boiling point of the next-lowest-boiling compound is approached. When the temperature
again stabilizes, another pure fraction of the distillate can be collected. This fraction of
distillate will be primarily the compound that boils at the second lowest temperature. This
process can be repeated until all the fractions of the original mixture have been separated.

Objective:

To illustrate the use of distillation for separating a mixture of two volatile liquid with
different boiling point.

Chemicals:

Unknown mixture

Apparatus:

Round bottom flask

Distilling head
Heating mantle
Thermometer with adapter
Receiving flask
Retort stand with clamp
Condenser
Vacuum adapter
Procedure:

1. The apparatus are arranged according to the diagram in laboratory manual.

2. The unknown mixture is placed into the round bottom flask until it reaches about half
of the flask.
3. The mixture is heated to boil by turning on the heating mantel until the first drop of
distillate produce.
4. The temperature is recorded for every minute until the first drop of the distillate
appears.
5. The temperature of distillate is recorded.
6. The heating mantle level is controlled in order to mantain the temperature of the first
distillate.
7. Step 6 is continued until there was no more drop of distillate produce.
8. The heating mantle level is increased until another drop of distillate produce.
9. The temperature of second distillate is recorded.
10. All reading are recorded into a table.

Results and Calculation:

Distillate Temperature (°C) Expected Compound

First 82 2-methylpropan-2-ol
Second 102 2-methyl-2-butanol

(graph is plotted)
Discussion:

The expected compound of first distillate was 2-methylpropan-2-ol. It is because it has

82°C boiling point which is same as 2-methylpropan-2-ol. The characteristics of the
unknown mixture also matched with expected compound such as colourless liquid with
camphor-like odour and its boiling point is 82.3°C which is very close to our results. In
this experiment, we need to control the temperature of the first distillate because we don’t
want the mixture go overheat and affect our results. If we go too fast we will fail to
separate the mixture and ruining the experiment.

The expected compound of second distillate was 2-methyl-2-butanol. The boiling

point the we get from the result is 102°C. The characteristics of the unknown mixture are
also matched with expected compound; colourless liquid with a mousy odour and slightly
soluble in water. Its boling point is very close with our result which is 102.4 °C.

What happen in the distillation process was the boiling point is

reached when the vapour pressure of the liquid equals the atmospheric
pressure. In this experiment we do not have mainly one pure
compound but a mixture of two compounds. Ideal solutions are those
in which the molecules are considered not to interact with each other.
For ideal solutions of two miscible liquids in which the boiling points of
the two liquids are separated by more than 100 °C, then the boiling
point of the mixture will rise rapidly to the boiling point of the lower
boiling liquid and remain constant while it is distilling. When all of the
lower boiling compound has distilled, then the temperature will rise to
the boiling point of the higher-boiling component and will remain
constant until all of this material has distilled.

Volatility is the property of a solid or a liquid to convert readily into

vapours. Hence, the more is a substance volatile earlier it will be
converted to vapours and the less will be the temperature at which it
starts vaporizing. So volatility is inversely related to boiling point.
Hence, we can say that a More Volatile Component (MVC) will have less
boiling point and Less Volatile Component (LVC) will have high boiling
point . So we can relate that the first distillate mixture is MVC and the
second distillate mixture is LVC.

There are many precaution steps that need to be taken while carried out this
experiment so excellent results will be achieved. We need to add boiling chips because its
provide space for nucleation so it can promotes vaporization. It also helps to disperse heat
and prevents hot spot and bumping. Before start the experiment, be sure all joints are
sealed and and apparatus is secure. Don’t forget to check the thermometer position. Then,
do not stop the distillation too soon because the temperature may fluctuate a bit. Continue
the distillation until only about 0.4mL solution remains in the round-bottom flask. If we
continue the process until dry, flask may overheat and break.
Questions:

1. Why we need to control the temperature of the first distillate?

We need to control temperature carefully because we don’t want the mixture go overheat.
If not, the separation results will be poor.

2. Suggest what type of unknown mixture [Mixture A]? Is the mixture homogenous or
heterogenous ? Why?

The mixture A is 2-methylpropan-2-ol and the mixture is homogenous. Homogeneous

mixtures have the same composition throughout and the individual parts of the mixture A
are not easily identifiable. Homogeneous mixtures are also referred to as solutions.

Conclusion:

The mixture A‘s boiling point is 82°C . The mixture B’s boiling point is 102°C. The
expected compound for mixture A is 2-methylpropan-2-ol while mixture B is 2-methyl-2-
butanol. To improve the experiment and obtaining the best result, the experiment should
have been repeated three times in order to get the average readings and to get the reading
more accurately. This will reduce the deviation from theoretical result and reduce the
error of reading. In addition, we also can compare our result to the other group or we can
make a group discussion with the other group to make sure that our results are accurate or
not. We should also increase our knowledge on how to handle the experiment better

References and Appendices:

Web:

Characteristic of compound
https://pubchem.ncbi.nlm.nih.gov

Homogenous compound
https://en.wikipedia.org/wiki/Homogeneous_(chemistry)

Volatility
https://www.physicsforums.com/threads/is-the-boiling-point-directly-related-to-the-
volatility-of-a-substance.503283/
Books:

Haynes, W.M. (ed.). CRC Handbook of Chemistry and Physics. 94th Edition. CRC Press
LLC, Boca Raton: FL 2013-2014, p. 3-392