ORGANIC CHEMISTRY 201 LABORATORY FORMAL REPORT

Separation of an Unknown Binary Mixture by Simple and Fractional

Distillation
Pilapil, Emerson M. , Pimentel, Maria Danica B. *, Rendor, Jake Vincent O.
Group 13
Department of Chemistry, College of Science
University of Santo Tomas, Espaa, Manila 1008

Abstract. Distillation is a method or process of separating mixtures based on differences in their volatilities in a
boiling liquid mixture. Distillation is done with the use of specific set-up shown in Figure 1 and 2. Through this
process, the identities of the unknown components in the solution can be determined through the obtained boiling
points. In the experiment, the percent low boiling point and percent high boiling point were computed. There is a list
of probable unknown volatile components in the mixtures. This list was obtained through comparisons of the boiling
points.

INTRODUCTION

Distillation is an old process of separating two or more volatile mixtures. It was already

being done as early as the 2nd millennium BC. Distillation uses the different boiling points of

volatile mixtures or substances in order to separate them. Volatile mixtures or substances are

solids and liquids that readily changes to its gaseous state. The rate of change in physical

properties or phase of this mixtures or substances can be increase through heating.

The application of distillation can be seen in the fields of food processing, industrial

distillation, laboratory scale, and herbal distillate. The food and herbal distillate differs from the

industrial and laboratory scale because distillation is not used as purification method but more as

a transferring method of volatile components. There is a specific difference between industrial

and laboratory scale because in laboratory scale it is performed by batch-wise while in industrial

distillation it is commonly continuous.

There are a lot of different types or kinds of distillation but in this experiment only two

are being introduce and used, simple and fractional. Simple and fractional distillation are

examples of laboratory scale distillation. Simple distillation is the most basic set-up for

1
 ORGANIC CHEMISTRY 201 LABORATORY FORMAL REPORT

distillation. In simple distillation, the volatile mixtures are heated, thus vapors are produced.

These vapors are immediately channeled in the condenser where it is cooled and condense. The

distillate produced in the simple distillation is not pure because its composition will be similar to

the composition of vapors at a specific temperature and pressure. Because of this, simple

distillation is not usually used. It is used when separating volatile components whose boiling

points are more than 25C or volatile components from involatile mixtures such as oil. Fractional

distillation is commonly used in volatile mixtures that have boiling points lower than 25C.

Since the components usually have low boiling points, it is necessary to repeatedly vaporize and

condense the components. In fractional distillation, the sample or mixture is heated to form

vapors. As the vapors are produce, it rises to the fractioning column where it cools and condenses

on the condenser walls and the surfaces of the packing material (tin foil). Here, the condensate

continues to be heated by the rising hot vapors and it vaporizes once more. Through this process

the components are repeatedly vaporized and condensed.

In the experiment, the components of an unknown solution can be separated and

determine how many components are present. After the experiment, a distillation curve can be

easily constructed and the percentage of the components can be calculated. There is a distinction

between the efficiency of both distillation processes in separating mixtures.

EXPERIMENTAL

Eight pieces of 13 x 100 mm test tubes were calibrated to 3mL. All the glassware needed

to perform simple/ fractional distillation was laid out with aluminum foil coiled as a packing

material. The apparatus were assembled according to the figures 1 and 2. An amount of 25mL of

the unknown assigned was placed on the 50mL distilling flask and 2 pieces of boiling chips was

added. The water was turned on gently in the condenser. The distilling flask was heated until the

2
 ORGANIC CHEMISTRY 201 LABORATORY FORMAL REPORT

first drop of distillate reached the receiver. The temperature of the first drop was recorded. The

heat was adjusted to have a rate of 1-2 drops per second. The temperature after every 3mL of

distillate was recorded. After the 8 calibrated test tubes were filled, the data was recorded with

temperature versus volume (mL). The temperature of the first drop corresponds to the zero

volume. Stop the distillation when all of the 8 test tube is filled or when there is not much left in

the round bottom flask. The boiling temperature was graph with temperature versus volume of

the distillate. The percent of low and high boiling component was calculated. The weight of the

left over unknown, if any, was measured to compute for the percentage loss.

Figure 1: the set-up for simple distillation

3
 ORGANIC CHEMISTRY 201 LABORATORY FORMAL REPORT

Figure 2: The set-up for fractional distillation

RESULTS AND DISCUSSION

Tables 1 show the different temperature recorded during the distillation process, both in

simple and fractional, in their corresponding volume.

Table 1: The recorded temperature versus the corresponding volume in both simple
and fractional distillation
TEMPERATURE OF DISTILLATE (C)
SIMPLE FRACTIONAL

VOLUME(mL) DISTILLATION DISTILLATION

1st drop (0)
65 57

3 81 67

6 84 68

9 89 61
12 92 130

4
 ORGANIC CHEMISTRY 201 LABORATORY FORMAL REPORT

15 98 134

18 98.5 132
NO MORE UNKNOWN
21 110 SOULTION
NO MORE UNKNOWN
24 130 SOLUTION

In Figure 3, the temperature of the distillate in the simple distillation was graph in

correspond to its volume.

Figure 3: The graph representing the data gathered in the simple distillation set-up

In Figure 4, the temperature of the distillate in the fractional distillation was graph

in correspond to its volume.

5
 ORGANIC CHEMISTRY 201 LABORATORY FORMAL REPORT

Figure 4: The graph representing the data gathered in the fractional distillation set-up

In Figure 5, both data gathered from simple and fractional distillation was graph together

for comparison reasons.

LEGEND:
-simple

-fractional

Figure 5: The graph representing both the data of simple and fractional distillation

Table 2 contain the percent (%) low boiling and percent (%) high boiling of both simple

and fractional distillation.

6
 ORGANIC CHEMISTRY 201 LABORATORY FORMAL REPORT

Simple Distillation Fractional Distillation

% Low boiling 60% 12%
% High boiling 36% 48%
Table 2: Tabular representation of the % low boiling point and
%high boiling point of simple and fractional distillation

COMPUTATIONS:

For simple:

For Fractional:

Table 3 show the possible unknown contain in the unknown solution and their

corresponding boiling point.

7
 ORGANIC CHEMISTRY 201 LABORATORY FORMAL REPORT

POSSIBLE UNKNOWN BOILING POINT(C)

ACETONE 56.53C
ISOAMYL ACETATE
142C
(banana oil)
CYCLOHEXYLAMINE
134C

FLUOBORIC ACID 130C

METHANOL 64.7C

ETHANOL 78.4C
Table 3: Tabular representation of possible identities of the unknown solution and their
corresponding boiling point

The key points in this experiment are boiling point and vapor pressure of liquids. Both

boiling point and vapor pressure are colligative properties. They are inversely proportional since

the higher the vapor pressure of a liquid at a given temperature, the lower the boiling point of the

liquid. The boiling point is the temperature at which the vapor pressure of the liquid equals the

environmental pressure surrounding the liquid while vapor pressure is the pressure of a vapor in

equilibrium with its non-vapor phases.

The basis for the separation of liquid mixture by distillation is the characteristics of the

mixture. The properties of the mixtures that are distilled have a big difference in their boiling

points and usually these mixtures are volatile mixtures, easily turn into its gaseous state. Since

boiling point is one of the basis, the one with the lowest or lower boiling point will be the first

one to be distilled than those with higher boiling point.

The condenser is a laboratory apparatus that help cool down the vapor. Water passes

through the whole length of the condenser to allow heat to transfer to the water. The water inlet is

8
 ORGANIC CHEMISTRY 201 LABORATORY FORMAL REPORT

on the bottom because when it is in the bottom it allows continuous and slow cooling and

condensing of the vapor.

The distilling flask or round bottom flask should be avoided to be empty because it could

explode or break the glass wares. It could explode since there is pressure inside and it is heated.

It could cause excited or increase in the energy of the atoms of the gaseous forms of the volatile

components.

Boiling chips provide surfaces on which bubbles can form as the liquid boils. If not used,

the liquid can get hot without boiling and it will "bump", sending liquid (instead of vapors) into

the distillation column or condenser. If it is added after the heating has started it would be too

late since it will already bump or liquid will be distillate instead of the vapors.

The fractionating column is an essential apparatus used in the distillation of liquid

mixtures to separate it into its component parts, or fractions, based on the differences in their

volatilities. It aids in separating the mixture by allowing the mixed vapors to cool, condense, and

vaporize again.

A packing material is used in the column instead of trays, especially when low pressure

drops across the column are required, as when operating under vacuum. This can either be

random dumped packing or coiled thin foil. Liquids tend to wet the surface of the packing and

the vapors pass across this wetted surface, where mass transfer takes place. The packing material

is also used so that the vapor does not go to the condenser immediately because it needs to be

repeatedly vaporize and condense.

9
 ORGANIC CHEMISTRY 201 LABORATORY FORMAL REPORT

CONCLUSION

In conclusion, fractional distillation is more reliable than simple distillation. In fractional

distillation, the components can be separated purely while in simple it is not. But in some cases,

simple distillation is enough to be able to separate the components purely.

REFERENCES

B.G., Segal.Chemistry; Experiment and Theory. New York, USA; Wiley.

(1989). pp. 215-216.

D. D., Ebbing. General chemistry. Boston : Houghton Mifflin. (1996). pp. 42-44.

J.W. , Hagen. Empirical Chemistry; a Quantitative Laboratory Program. San

Francisco: W.H. Freeman. (1972). pp. 283-286.

10