CHM142L Organic Chemistry 1 Laboratory

2nd Quarter SY 2014-2015

Simple and Steam Distillation

Terrado, Rence Christian L.

Professor Marilyn Miranda, School of Chemical Engineering, Chemistry and Biotechnology, Mapua Institute of Technology; Bote,Jairus Lemuel ; Brillas, Catherine Jill
1

CHM142L/B21, School of Chemical Engineering, Chemistry and Biotechnology, Mapua Institute of Technology

ABSTRACT
One of the best purifying techniques for mixtures of liquids is through distillation. Distillation is a
process used to separate liquids in a mixture based on their relative boiling points. It involves
heating a mixture and collecting the vapours or gas that rise from it. Since distillation does not
involve the creation or modification of the compounds within the mixture, and it is based on
vapour point and volatility, which are physical properties. The aim of this experiment is to have a
basic knowledge of distillation and what process will best fit for a mixture of organic compounds.
In this technique, the volatile compounds is converted to vapor leaving the non-volatile compound
as a residue. In simple distillation, Toluene was used for the experiment and the group obtained
27.59% recovery for toluene. For steam distillation, the set-up was connected with the simple
distillation set-up but the source of heat for this process is a steam coming from boiled water and
separated pure paradichlorobenzene which was used for bathroom deodorizers from impure
paradichlorobenzene. Then the pure sample was recrystallized. The resulting sample recovery
was 84.09% which is not bad for the experiment. Overall results was according to the objectives
and the group have met the objectives for the success of the experiment.
Keywords: Distillation, Simple Distillation, Steam Distillation

INTRODUCTION or modification of the compounds within the

mixture, and it is based on vapour point and
The volatility of a compound is based on the volatility, which are physical properties.
equilibrium vapour pressure exerted by the
Distillation is a physical process rather than a
compound at a partial temperature. Different
compounds will exert different vapour chemical one. The relationship between
pressures at a given temperature because of atmospheric pressure and boiling point tells us
variations in the intermolecular forces of that if we could reduce the atmospheric
attraction working in these different pressure in a controlled way, we could
compounds. Compounds that have strong
intentionally reduce the boiling point of a
intermolecular forces will be more difficult to
separate from each other and will therefore be liquid. In principle, if the atmospheric pressure
less volatile, that is, they will be readily is lowered enough, liquids will boil at or below
converted in the vapour phase. It is therefore room temperature. In the laboratory, the
possible to separate compounds from each atmospheric pressure is typically reduced by
other in a mixture based on volatility
attaching a vacuum line to the distillation
differences. Compounds that are more volatile
will be converted into vapour earlier than those apparatus. In a couple of weeks you will use
that have low volatilities. This process is called the rotary evaporators in the lab. These are
distillation. really reduced pressure distillation apparatus.
Reduced pressure distillation or vacuum
Distillation is a process used to separate distillation is useful when one wants to rapidly
liquids in a mixture based on their relative remove a volatile solvent from non-volatile
boiling points. It involves heating a mixture and compounds, when minimal heating is
collecting the vapours or gas that rise from it. important due to the thermal instability of a
Since distillation does not involve the creation compound or when a compound has such a

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 CHM142L Organic Chemistry 1 Laboratory
2nd Quarter SY 2014-2015
high boiling point that atmospheric distillation
is not feasible.
Simple distillation is a process used to
separate two liquids with boiling points that
differ by a fair amount 77 F (25 C or more) or
to separate a liquid from a non-volatile
compound with higher viscosity. The mixture is
heated to the boiling point of the more volatile
compound, which is the lower of the two
boiling points. The resulting vapor is collected
from the heating chamber and immediately
condensed back into liquid form. This can
result in an impure distillate. The advantages
of simple distillation are indicated: It uses low
heat because it just uses simple equipments
unlike in other distillation processes which
requires higher heat energy and this type of
distillation requires only cheap apparatus and
it consumes less time. However, there are also
limitations regarding in simple distillation, one
is it is prone to impurities and there are
azeotropic mixtures, these are mixtures of
liquids may be so constituted that, when
boiled, their vapour has the same composition
as the mixture itself. Simple distillation cannot
change this mixture's composition.
Steam distillation is a separation process
used to purify or isolate temperature sensitive
materials, like natural aromatic compounds.
Steam or water is added to the distillation
apparatus, lowering the boiling points of the
compounds. The goal is to heat and separate
the components at temperatures below their
decomposition point. In steam distillation,
steam is used to lower the distillation
temperatures of high boiling organic
compounds that are immiscible with water. In
the process, steam is charged to the matrix to
volatilise the hydrophobic liquid and carry it
across to a chilled condenser for subsequent
liquefaction and separation from water.
Variations in temperature, pressure and
distillation time are used to control the
process. Steam Distillations have many
Experiment 03 Group No. 4 Date 11/14/14
advantages in industries like quality control
because it allows you to control the
temperature and amount of steam you apply to
the plant material. Keeping the temperature
right at the boiling point of water allows for the
least amount of degradation to delicate
botanical oils. However, this type of distillation
is expensive and they require higher
equipment and operating costs.
The objectives of the experiment is to
assemble a simple and steam distillation set up
and to identify and recognize the significance
of all parts of the set up and to purify a sample
using simple and steam distillation.
MATERIALS AND METHODS
In part 1 of the experiment entitled Simple
Distillation. The group followed these
procedures for the success of the experiment.
The group first prepared the materials and
apparatuses needed and assembled the
distillation set up shown in Figure 1. Then 15
mL of toluene was transferred to the pear
shaped flask using the pipette and then the
toluene was heated by the hot plate. Then the
group collected the distillate at different
temperatures at a rate of 1 drop per second
and measured the volume collected until 1 to 2
mL of distillate left in the pear shaped flask
and then plotted the graph of the temperature
against the volume collected then recorded the
boiling point of the liquid.
In part 2 of the experiment called Steam
Distillation. These are the procedures that the
group followed: The group obtained 2 grams of
impure paradichlorobenzene given its melting
point and also prepared the steam generator
by boiling water in the erlenmeyer flask. The
group also assembled the steam distillation
setup shown in Figure 2 while it is connected to
the water out of the set-up of the simple
distillation. While water was waited to boil,
impure paradichlorobenzene was placed in the
pear shaped flask with arm and dissolved it in
5 mL water by slightly heating the mixture
then the group proceeded to the distillation.
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When the condenser is already clogged, pure

paradichlorobenzene is obtained to the
distillate collector by heating the condenser
with Bunsen burner then distillation was
continued until all pure paradichlorobenzene
was collected. Mixture in the receiving tube
was cooled then filtered using the Buchners
funnel and applying air pressure then air-dried
the solid paradichlorobenzene. The group
obtained the weight of the solid
paradichlorobenzene and its melting point by
using the Thomas-Hoover melting point
apparatus and computed its percentage
recovery. (Table 1. List of apparatuses used)

Thomas-Hoover Buchner Quick Fit

Melting Point Funnel
Apparatus

Pipette Erlenmeyer Capillary

Flask tubes

Hot plate

(Table 2. List of reagents used)

Ice Impure
paradichlorobenzene

Toluen Distilled Water

e

RESULTS and DISCUSSIONS

The part 1 of the experiment entitled Simple

Figure 2: Steam Distillation Set-up
Distillation. In simple distillation, the vapour is
immediately channelled into a condenser.
Consequently, the distillate is not pure but
rather its composition is identical to the
composition of the vapours at the given
temperature and pressure. The data obtained
from the part 1 of the experiment is shown
within the plot:

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 CHM142L Organic Chemistry 1 Laboratory
2nd Quarter SY 2014-2015
In the experiment, the group was able to gain
the accurate results regarding the distillation of
toluene. The plot shows the graph between the
temperature and the volume of the distillate
collected. The graph shows toluene itself
evaporated and between 9 mL to 13 mL, the
temperature does not rise because it has
reached the toluenes boiling point which the
temperature will remain constant. The constant
temperature serves as the pure toluene was all
vaporized and condensed and became a liquid.
Wider temperature range and steeper slope
means a more effective separation of the pure
toluene to its impurities.
Table 4. Table of Results
Boiling Point of Sample, 100-
C 105
Total Volume Collected, 14.5
mL
Percentage Recovery, % 27.59
Bumping is a process in which a solvent
becomes superheated and then undergoes a
sudden release of a large vapour bubble,
explosively forcing liquid outside of a flask.
Boiling chips or glass beads are made of a
porous material and have a nonreactive Teflon
coating - they provide nucleation sites
(extremely localized budding for gaseous
bubbles) so the liquid boils smoothly/more
easily. The air bubbles break the surface
tension of the liquid being heated and prevent
Experiment 03 Group No. 4 Date 11/14/14
superheating and bumping. An appropriate
rate of distillation is approximately 20 drops
per minute. Distillation must occur slowly
enough that all the vapours condense to liquid
in the condenser. Many organic compounds are
flammable and if vapours pass through the
condenser without condensing, they may ignite
as they come in contact with the heat source.
In part 2 of the experiment entitled Steam
Distillation, table of results and data are shown
below.
Table 5. Table of Results regarding Melting points, Weights
and % Recovery
Melting Point of Crude Sample, 36-
C 45
Melting Point of Purified 50-
Sample, C 54
Weight of Crude Sample, g 2.2
Weight of Purified Sample, g 1.85
Percent Recovery, % 84.0
9
To obtain accurate results, the set-up must be
secured and properly locked to avoid leaks.
And to put glass beads to avoid overheating of
the mixtures resulting to accidents.
Mixtures of organic compounds tend to break
and decompose at high temperatures. Simple
Distillation may not be applicable on this case.
So steam is introduced into the process called
Steam Distillation. But steam distillation have
also its disadvantages like the set up needed
to be secured and not even a small hole in the
connection between the quick fit is present
because the compound distilling may come out
and mix with the air, no compound will then be
collected. Sometimes an organic compound
exert very little vapour pressure even at high
temperatures. This sometimes results in
decomposition of the organic compound even
before it begins to boil. This is where steam
distillation is very effective because in here we
can provide additional vapour pressure so that
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overall mixture achieves atmospheric pressure

at lower temperature, then the mixture boils
off at that lower temperature.

The condenser must always be filled with water

coming from the sink. This is important
because both the water and the organic
compound will distillate in this process and
water can control the temperature of the
condenser which the distillate will flow, if there
is no water the distillate will come out very hot
and large amount of water will come out too
and also the compound being steam distilled
must not have any reaction with water.

CONCLUSIONS AND RECOMMENDATIONS

The group obtained the results accurately and

prcised. Because of the right setups and
preparations. Even though on the part 1, the
group did not meet the exact boiling point
range because of the impurities of toluene. But
in the steam distillation, acceptable data was
obtained. Therefore the group did the
experiment well because of the right set up
and right procedures that the group followed.

REFERENCES

1. Soderberg, T (n.d.) Organic Chemistry With

a Biological Emphasis (University of Minnesota,
Morris)

2. Samuel H. Yalkowsky , Joseph F.

Krzyzaniak , Paul B. Myrdal Ind. Eng.
Chem. Res., 1994, 33 (7), pp 18721877

3. Chang, R. (2008). General Chemistry: The

Essential Concepts (5th Ed.). NewYork:
McGraw-Hill.

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