CHM142L/B11 Organic Chemistry 1 Laboratory

1st Quarter AY 2012-2013

Mapua Institute of Technology

School of Chemical Engineering and Chemistry
Muralla St., Intramuros, Manila
Simple and Steam Distillation
Group No. 5
Oblena, Adrian D.1
Manacup, Cris Vincent L.2
Ong, Joshua Jyro B.3
Ng, Josephine A.4
Student, CHM142L/B11, School of Chemical Engineering, Chemistry, and Biotechnology, Mapua Institute of Technology; 2 Student,
CHM142L/B11, School of Chemical Engineering, Chemistry, and Biotechnology, Mapua Institute of Technology; 3 Student, Group
Leader, CHM142L/B11, School of Chemical Engineering, Chemistry, and Biotechnology, Mapua Institute of Technology; 4Professor,
School of Chemical Engineering, Chemistry, and Biotechnology, Mapua Institute of Technology
1

ABSTRACT
Another way to purify compounds is distillation. It is used to separate mixtures based on the
differences in volatilities of components in the mixture. There are types of distillation that are specific to
different industries and applications. Two of the distillation processes are simple and steam distillation.
The aim of this experiment is to familiarize the setups of simple and steam distillation and recognize
the significances of all parts. Simple distillation is consists of a one-necked pear-shaped flask attached to
an adapter holding a thermometer (to determine the boiling temperature of the liquid). The adapter
connects to a condenser into which cold water is constantly passed through. The condenser leads into a
collection flask for the purified liquid.
Steam distillation then consists of a safety tube, a steam generator (for additional vapor pressure),
connecting to a two-necked pear-shaped flask by a bent tube, and connected to a set of apparatus same
as the simple distillation.
In this experiment, the team was able to purify a sample using these two laboratory techniques:
impure carbon tetrachloride in simple distillation and impure para-dichlorobenzene in steam distillation.

INTRODUCTION
Distillation is a physical separation process
used in separating mixtures based on the
differences in volatilities of components in the
mixture through boiling. There are different
distillation processes in laboratories and specific to
different industries. Two of the distillation systems
involved in the experiment are simple and steam
distillation.
Simple distillation is a distillation process
usually used only to separate liquids whose boiling
points differ greatly (rule of thumb is 25 C), or to
separate liquids from involatile solids or oils. In
this manner, all the hot vapors produced are
immediately channeled into a condenser that cools
and condenses the vapors.
Steam distillation, on the other hand, is a

special type of distillation for the heat-sensitive

compounds since many organic compounds tend to
decompose at high sustained temperatures. As this
case, water or steam is added so the boiling points
of the compounds are depressed, allowing them to
evaporate at lower temperatures, preferably below
the temperatures at which the deterioration of the
material becomes appreciable.
Steam distillation is employed in the manufacture
of essential oils, for use in perfumes.
When a mixture of two immiscible liquids is
heated while being agitated to expose the surfaces
of both the liquids to the vapor phase, each
constituent independently exerts its own vapor
pressure as a function of temperature as if the
other constituent were not present. Consequently,
the vapor pressure of the whole system increases.
Boiling begins when the sum of the partial

Experiment 3 | Simple and Steam Distillation | Group 5 | July 30, 2012

CHM142L/B11 Organic Chemistry 1 Laboratory

1st Quarter AY 2012-2013
pressures of the two immiscible liquids just
exceeds the atmospheric pressure. In this way,
many organic compounds insoluble in water can be
purified at a temperature well below the point at
which decomposition occurs. This is the principle
behind steam distillation.

compound ensuring that it will not evaporate.

Weigh and determine the melting point, this time it
is pure.
Fig 3.2 Steam Distillation Setup

MATERIALS AND METHODS

Simple Distillation
Setup of the simple distillation is to be done
first. Pipette 15 mL of impure carbon tetrachloride
into the one-necked pear-shaped flask. Using a hot
plate, heat the pear-shaped flask regulated to
number 6. Record the volume and temperature in
every drop per second until 1 mL of the distilland
is left in the pear-shaped flask.
Fig 3.1 Simple Distillation Setup

REAGENTS:
Distilled
Dichlorobenzene

Water,

Impure

Para-

RESULTS AND ANALYSIS

I.
Simple Distillation

REAGENTS: Impure Carbon Tetrachloride

Steam Distillation
Slightly boil a 100 mL of distilled water in an
Erlenmeyer
flask
(the
steam
generator).
Determine the melting point of the impure pdichlorobenzene. Weigh another 2 grams of impure
p-dichlorobenzene and slightly dissolve with water
placed in a two-necked pear-shaped flask. Setup of
the steam distillation is to be prepared next.
Continue heat the distilled water as proceeding to
the distillation process. If there is clogging
occurring in the condenser, shut off the water in
the condenser and heat it with a Bunsen burner.
Continue distilling the solution for 15 minutes. Cool
the mixture to room temperature and after, in an
ice bath. Vacuum filter the solution and air dry the

Boiling point of the sample (

)
Total volume collected (mL)
Percentage recovery

76

12.8 mL
85%

Seen on the graph is a plot of volume vs.

temperature. The impure carbon tetrachloride
boiled at 76 deg C. At 40 deg C, bubbles started to
appear in the pear-shaped flask. The liquid state of
the sample started to vaporize after some time.
The vapor of the sample then went through the
condenser to change its state from gas to liquid
again. But this time it is now purer than before. It
is because theres a difference in volatilities in the
carbon tetrachloride and the impurities that made

Experiment 3 | Simple and Steam Distillation | Group 5 | July 30, 2012

CHM142L/B11 Organic Chemistry 1 Laboratory

1st Quarter AY 2012-2013
it pure using simple distillation.
II.
Steam Distillation
Melting point of crude sample (
)
Melting point of purified sample (
)
Weight of crude sample (g)
Weight of purified sample (g)
Percentage recovery
* Not finished

have any reaction with the water.

*
*
2.00 g
0.6301 g
31.51%

REFERENCES
http://orgchem.colorado.edu/Technique/Procedure
s/Distillation/Distillation.html. (n.d.).
http://www.chemhelper.com/distillation.html.
(n.d.).
Mohrig, J. R., Hammond, C. N., & Schatz, P. F.
Techniques in Organic Chemistry. W.H. Freeman.

In this part, the team was not able to determine

the melting points of the crude and purified pdichlorobenzene because the Thomas-Hoover
apparatus malfunctioned and theres no ample
time for conventional determination of melting
point. But luckily, the team obtained crystals
weighing 0.6301 g after three trials of
experimentation: two of which is failed and the last
trial succeeded.
A steam generator was introduced to the process
because the sample has a high boiling point; so to
boil it faster, an additional vapor pressure is
brought in. This prevents also the decomposition of
the p-dichlorobenzene being distilled.

CONCLUSION
In this experiment, objectives were achieved. From
the setups of simple and steam distillation, to the
significance of its parts, and to purify a sample of
impure
carbon
tetrachloride
and
paradichlorobenzene using these distillations. But the
team cant ensure that the crystals from impure pdichlorobenzene were pure because the melting
point was not determined.
Precautions were also introduced to us for both
distillation processes to be effective. They are the
following:
Both the steam generator and the sample flask
must contain boiling chips before heating is
started;
Heat is applied to both the steam generator
and the sample flask gently;
The condenser must always be filled with fresh
water during the entire process; and
The compound being steam distilled must not
Experiment 3 | Simple and Steam Distillation | Group 5 | July 30, 2012

CHM142L/B11 Organic Chemistry 1 Laboratory

1st Quarter AY 2012-2013
Answers to Guide Questions
1. What are the advantages and limitations of simple distillation? In what situation is simple distillation
the choice for purification technique?
Simple distillation is an easier setup. It takes less time in every distillation. Thus, it consumes less
energy than any other kind of distillation system. But, in return, it gives poorer separation and only
works well with relatively pure liquids. It requires also the liquids to have large boiling point
differences. So, with the said characteristics of simple distillation, it is suitable in separating relatively
pure liquids with large boiling differences or liquid with impurities.
2. What is bumping? How is it prevented by the addition of glass beads in the distilling flask? Why must
the beads be added before, and not during, distillation?
Bumping, in distillation, is an event occurring in solvent, while heating, in which it becomes
superheated and then undergoes an abrupt release of vapor bubbles, explosively forcing liquid outside
of the flask. Addition of glass beads will prevent bumping to occur. It is because it has pores that
provide nucleation sites (cavities to trap air) so the liquid boils smoothly. The air bubbles break the
surface tension of the liquid being heated preventing superheating or bumping. It should be added before
distillation because it could induce flash boiling if added during.
3. Why is the heating rate controlled during simple distillation?
It is important to control heating rate during simple distillation because you must ensure that the
distillate is pure. Also, to be able to separate two compounds in a mixture successfully, you must
regulate heat since the two compounds have different boiling points.
4. What are the advantages and limitations of steam distillation? In what situation is steam distillation the
choice for purification technique?
Steam distillation is used to distill compounds that are sensitive to heat that can lower the pressure in
the flask so that you don't have to heat the compound as high; high temperatures can often
decompose organic compounds, so it must be avoided. But, not many compounds can be steam
distilled - usually aromatic ones; the process does not completely take out impurities - just leaves the
larger molecules out, but still leaves other bits of elements. Steam distillation works with immiscible
liquids, water and other organic compounds that exert very little vapor pressure even at high
temperatures.
5. What is the function of the safety tube during steam distillation?
Safety tube, in steam distillation process, is used to allow water to escape when the pressure gets
higher. It also used to control the delivery of gases opening to the outer air.
6. Explain the importance of each precaution listed in the theoretical discussion of this experiment.
a. Both steam generator and the sample flask must contain boiling chips before heating is started.
Boiling chips must be contained in the steam generator and the sample flask before heating is started
because it will prevent bumping to occur. It is because it has pores that provide nucleation sites ( to
trap air) so the liquid boils smoothly. The air bubbles break the surface tension of the liquid being heated
preventing superheating or bumping. It should be added before distillation because it could induce
flash boiling if added during.
b. Heat is applied to both the steam generator and the sample flask gently.
Experiment 3 | Simple and Steam Distillation | Group 5 | July 30, 2012

CHM142L/B11 Organic Chemistry 1 Laboratory

1st Quarter AY 2012-2013

Heat is applied to both the steam generator and the sample flask gently to avoid sudden change in
temperature so as to monitor it for the different values of boiling points of the components in the
sample for separation to occur effectively.
c. The condenser must always be filled with fresh water during the entire process.
The condenser must always be filled with fresh water during the entire process to ensure the most
effective cooling of the vapor since the flow of water is such that the coldest part of the condenser is at
the end just before the vapor escapes from the condenser.
d. The compound being steam distilled must not have any reaction with water.
The compound being steam distilled must not have any reaction with water for the sample to be
purified successfully. Another thing is, steam distillation is best suitable in separating organic
compounds into other components, and most of these organic compounds are immiscible or insoluble
in water so there is no reaction occurring.

Experiment 3 | Simple and Steam Distillation | Group 5 | July 30, 2012