MATERIALS AND METHODS

For this experiment, the researchers used the following apparatus: quick fit, pipette, hot plate, rubber tubing,
and Erlenmeyer flask.
This experiment required the use of the following reagents: ice, impure toluene, impure p-dichlorobenzene
and distilled water. This reagents were provided and prepared beforehand by the Chemistry Stockroom and
laboratory assistant.
For the first part of the experiment which was simple distillation, the setup must be assembled first. Then,
with the use of pipette, the researchers transferred 15 ml of impure toluene into the one-neck pear-shaped
flask. This was then placed in a hot plate set on number 6 in the switch. The distillate at different
temperatures must be collected at a rate of one drop per second. The volume of the distillate collected was
then measured. The distillation was continued until 1 ml of distillate was left in the flask. After getting all the
data, The researchers were asked to plot a graph of temperature against volume of distillate collected and to
record the temperature at which most of the liquid distilled as the boiling point.
For the second part which was steam distillation, the researchers acquired 2 g of impure p-dichlorobenzene
and determined the melting point range of the mixture. The setup was then assembled. In an Erlenmeyer
flask, they boiled 100 ml of water. The sample and a small amount of water were mixed and was then
placed in a two-neck pear-shaped flask. The hot plate was switched on and the apparatus was to be
connected with each other. If the crystals were formed at the condenser, the researchers asked the
laboratory assistant to heat the condenser with Bunsen burner. The process was then continued until all the
sample was distilled or the sample was about one inch away from the neck of the pear-shaped flask. After
letting the mixture to be cooled, the researchers disconnected the apparatus.Filter the obtained pdichlorobenzene and it was air-dried. They weighed the dried sample and determined the melting point
range. Also, the samples percentage recovery was to be computed.

INTRODUCTION
One of the most common separation techniques used in chemistry is distillation. Distillation is the process of
separating compounds based on their volatility differences. The volatility of a compound is based on the
equilibrium vapor pressure exerted by the compound at a particular temperature. Different compound will
have different vapor pressure at a given temperature because of variation in the intermolecular forces of
attraction working in these compounds. If a compound has a strong intermolecular forces, it will be more
difficult to separate from each other meaning it will be less volatile.
In a simple distillation, applying heat will help separate the volatile compound to a nonvolatile compound.
The volatile compound will be converted to vapor leaving only the nonvolatile compound as a residue. The
vapor of the volatile compound exit the distilling flask through a sidearm and then reaches the condenser
which is surrounded by water all throughout the distillation. The temperature difference between vapor in the
condenser and water forces the vapor to change back to liquid form which will be collected in another flask.
For simple distillation to be successful, one must note that the: the substances to be separated must have a
large volatility difference, the condenser must be connected to a source of water, glass beads should be
present inside the distilling flask prior to heating. Heat must be supplied gently, and the thermometer used
must be at the level of the sidearm.
In a steam distillation, water is used to provide additional vapor pressure to help a nonvolatile organic
compound to boil off and be distilled at a temperature lower than its normal boiling point. Both water and

organic compound distill off together. The apparatus used for this process has three major parts: steam
generator which supplies steam to add t the vapor pressure of the organic compound, the sample flask,
which holds to sample mixed with water, and heat sources for both steam generator and sample flask. The
water in the acquired distillate is separated using a funnel.One must note that steam distillation; has both
steam generator and sample flask and heat is applied to them, the compound being steam distilled must not
have any contact with water and make sure that the condenser should be connected to a source of water all
the time.

RESULTS AND DISCUSSION

On the first part of the experiment, the researchers were asked to purify an impure toluene using simple
distillation. In the setup, the tip of the thermometer must be correctly positioned slightly below the center of
the condenser to accurately reflect the temperature of the vapors and the water supply should be connected
to the lower port in the condenser and the drainage tube connected to the upper port of the condenser. Also
make sure that each apparatus are connected properly to each other to prevent leakage that will hinder
acquiring desired results in the experiment.
After assembling the simple distillation setup, the researchers put glass beads on the pear-shaped flask. If
these beads are not present, bumping or overheating of the sample may occur. Bumping occurs when
liquids are heated very rapidly and no nucleation occurs, thus when the liquid finally boils, a large vapor
bubble is formed that pushes the liquid out of the test tube. This expulsion of boiling liquid poses a serious
hazard to others and oneself in the lab. Glass beads work by providing nucleation sites so the liquid boils
smoothly without becoming superheated or bumping. They should not be added to liquid that is already near
its boiling point or during the distillation process, as this could also induce flash boiling.
After this, the researchers poured 15-ml impure toluene to the pear-shaped flask then proceeded to do
simple distillation. They waited for the sample to boil and observed if the vapor from the hot mixture is
collected and recondensed into liquid that will be transferred to a volumetric cylinder. Acquiring 1 ml of the
recondensed liquid, the temperature reading was 72C. As the temperature changes, the volume reading
must be recorded. Overall, the researchers obtained 13.1 ml of the recondensed liquid. Figure 1 shows
volume acquired in reference to its temperature.

Looking at Figure 1, the changes in terms of temperature were minimal at 107C-111C. Therefore, this
range was considered the boiling point of the sample. To get the percentage recovery of the sample, the
researchers used equation on Figure 2.

% recovery

T2 - T1
100%
volume acquired

T1 represents the first temperature at which the changes in terms of temperature were minimal and T2
represents the last temperature at which the changes in terms of temperature were minimal. The obtained
volume at 107C and 111C were 5.5 ml and 12.5 ml respectively. Substituting these values on equation at
Figure 2, the researchers obtained 53.44% recovery of the sample.