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Volume No. 5 Issue No.

3
Date of Submission: N/A
Date of Acceptance: November 13, 2015

Analysis and Purification of Compounds Using Different


Distillation Methods Simple and Steam
Macatantan, Sedfrey L.1; Gavio, Patricia Anne L.; Lat, Dheya O.; Manalo, Jayvee Bien D.; Dr. De Castro- Cruz,
Kathlia A.2
Mapua Institute of Technology, Muralla Street, Intramuros, Manila, Metro Manila, Philippines

ABSTRACT
Volatility is the tendency of a substance to vaporize. It is directly related to a substance's vapor pressure. At a given
temperature, a substance with higher vapor pressure vaporizes more readily than a substance with a lower vapor.
Factors that can affect volatility are weight and intermolecular forces of attraction. Substances with heavier weight
and stronger intermolecular forces of attraction tend to be less volatile as more energy will be needed to break them
down. Simple and steam distillation are two methods used in this experiment. Simple distillation is best used when
substances to be separated have high volatility differences. When a compound only exerts little vapor pressure,
steam distillation is used, as it would require the assistance of water so that less pressure would be in the sample
container and only a lower temperature will be required which can prevents decomposition of products.
Keywords volatility, intermolecular, simple, steam, temperature, pressure

Student, CHM142L/B21, School of Chemical Engineering, Chemistry and Biotechnology, Mapua Institute of
Technology; sedfreymac@yahoo.com
2
Professor, School of Chemical Engineering, Chemistry and Biotechnology, Mapua Institute of Technology;
kadecastro@mapua.edu.ph

1. INTRODUCTION
In organic chemistry, volatility of
compounds is an important thing to be considered
and noted as we are already dealing with all sorts of
different compounds that are being studied and
process and the idea of volatility contributes greatly
in the comparison and handling of the compounds.
First, we need to know, what is volatility? To make it
simple, volatility refers to the tendency of a pure
substance to go into the vapor phase. It can also be
perceived as how much a certain substance wants to
be a gas. Different compounds have different vapor
pressures given a certain temperature as this stands as
a variation for the vapor pressure. In a manner, two
factors should be considered in discussing volatility
the substances weight and intermolecular forces of
attraction (Trubiano). Surely, it can be easily
understood that if a compound has a greater weight,
then it will more likely stay in the liquid phase which
is due to the high energy that would be needed to
convert the compound into the gas phase. This idea
can be most notable with hydrocarbons, especially
alkanes. Carbon atoms are the main foundation of the
structures (as well as hydrogen atoms) as they
contribute to the overall molecular mass more. As we
can see, as the sequence of methane, ethane, propane
goes, the more carbon atoms they have, the greater
temperature it is needed to put up with their boiling
point. This means that a substance with greater
weight would require more energy for them to be
vaporized. In terms of the attraction of intermolecular
forces, it would just be a continuation of what is said
with the weight. To be clear, as whats previously
said and concluded, if a substance has strong
intermolecular forces of attraction, then they are less
likely to be volatile as what will happen is the forces
that hold them would not be easily be broken down.
This means that it would be hard for those substances
to be vaporized, taking much heat and energy to do
so. (Baluyot & De Castro)
It is possible for compounds to be separated
basing it on their volatilities. This process of
separation of compounds is called distillation. This is
1

a process of separating the components from a liquid


mixture by selective evaporation and condensation.
In this experiment, we have used two methods of
distillation simple and steam. In the method of
simple distillation, there is just a liquid mixture
which contains a volatile and nonvolatile compound.
When heat is applied, the volatile compound would
be converted to vapor and the nonvolatile compound
would remain making it the residue. Because of the
water that the already vaporized volatile compound
will undergo, it would again be converted to liquid
due to temperature differences. In doing this method,
we should only be minded that the compounds to be
separated must have high volatility differences so that
they would not be both turned into vapor. (Yoder,
2015)
On the other note, there is also the steam
distillation. This is used whenever the compound that
is used only has a little vapor pressure to give, as this
means that even though at high temperature, the
compound would still not be converted into vapor
leading to a decomposed compound. In steam
distillation, water will be used to add more vapor
pressure to the nonvolatile compound which is
needed to be turned into vapor while heat is still
being applied. With this, the compound will boil and
less temperature will be needed for it to be turned
into vapor, hence separating the compounds.
(Pahlavan, 2013)
For the experiment, we are to use both
methods of distillation to provide analysis to given
compounds.

2. EXPERIMENTAL SECTION
Materials Used. Quick fit (includes all apparatus
needed for simple and steam distillation set-ups),
pipette, hot plate, Erlenmeyer flask (or beaker)
Reagents Used. Ice, impure carbon tetrachloride,
impure p-dichlorobenzene, distilled water

Student, CHM142L/B21, School of Chemical Engineering, Chemistry and Biotechnology, Mapua Institute of
Technology; ishy.gavino@yahoo.com.ph
2
Professor, School of Chemical Engineering, Chemistry and Biotechnology, Mapua Institute of Technology;
kadecastro@mapua.edu.ph

Simple Distillation. Set-up for simple distillation


will be assembled. Fifteen milliliters of impure
carbon tetrachloride will be put to the pear-shaped
flask to serve as the sample for the experiment. Heat
will be applied on the sample using the hot plate.
Continuously, distillate will come out and its volume
will be measured at different temperatures.

Temperature, C
90
80
70
60

Steam Distillation. The set-up for steam distillation


will be assembled. One hundred milliliters of water
would be slightly boiled, that is, for later use. The pdichlorobenzene sample would then be placed in the
pear-shaped container and it will be dissolved in 5
mL of water. The container with water will now be
heated as it is connected to the container containing
the liquid mixture. If no mixture is coming out, the
condenser might be clogged and a Bunsen burner
should be used to clear it out. The mixture in the
receiving container will then be cooled. It will then
be filtered and the remaining compound will be air
dried.

3. RESULTS AND DISCUSSION


In the experiment, we have performed the
methods of simple and steam distillation. Simple
distillation was used for impure carbon tetrachloride
while steam distillation was used for pdichlorobenzene. In a manner, the volatility of these
compounds would surely affect the resulting
distillate/mixture that we will get.

Temperature
, C

50
40
30
20
10
0
0

10

15

Figure 1. Graph of temperature vs. volume of


distillate collected during simple distillation
Figure 1 shows the graph of the temperature
of the distillate gotten vs. the amount of the distillate
that is collected. During the process of simple
distillation, the temperature of the distillate suddenly
dropped to 78C when the hot plate is at 275C. At
the beginning, the rate of drop was 5 drops per
minute, but as the temperature increases, the rate has
finally become 44 drops per minute. In here, an
impure carbon tetrachloride has been used as a
compound sample. From the compound itself being
impure, it means that it has a weak intermolecular
forces of attraction which is why it is better suited
with simple distillation due to the temperatures of the
volatile and nonvolatile components. The rate of the
distillate that is coming out has increased as the
temperature increased. It is because at a higher
temperature, the compound will be acquiring more
energy, hence breaking the intermolecular forces of
attraction binding it and turning it into vapor quicker
than when only a low temperature is applied. When
the original sample is applied with heat, it is turned
into vapor, but because of the path that it will
undergo which is surrounded with water, a difference
in temperature would be noted which is why when it

Student, CHM142L/B21, School of Chemical Engineering, Chemistry and Biotechnology, Mapua Institute of
Technology; ishy.gavino@yahoo.com.ph
2
Professor, School of Chemical Engineering, Chemistry and Biotechnology, Mapua Institute of Technology;
kadecastro@mapua.edu.ph

comes out as a distillate, it will be in a form of a


liquid again.
Table 1. Data regarding the analysis of the impure
carbon tetrachloride
Boiling point of the sample
79C
Total volume collected
12.1 mL
Percentage Recovery
80.67%
Table 1 simply shows the data that is
gathered from the impure carbon tetrachloride that
we have. Seventy-nine degree Celsius as a boiling
point is quite reasonable given that it is an impure
one. For the volume of the distillate collected, from
the original 15 mL, it means that there had been a
large amount of pure substance from the original
sample and a percentage recovery of 80.67% makes it
reasonable.
Table 2. Data regarding the analysis of pdichlorobenzene
Melting point of crude sample
52.47 C
Melting point of purified sample
54.7 C
Weight of crude sample
2g
Weight of purified sample
1.8 g
Percentage Recovery
90%
Table 2 shows the data we gathered
regarding the p-dichlorobenzene wherein steam
distillation is used. The water helped the sample boil
which then produced a steam. The steam got
crystallized as it clogged, so heat is applied and the as
it turns into liquid, it got crystallized again a while
after receiving container. Steam distillation has been
used in this compound probably because it only
exerts very little vapor pressure even if it is subjected
in a high temperature, and also to avoid
decomposition of the compound. With this, water is
used so that vapor pressure would be added which
will make the mixture achieve atmospheric pressure
even at a low temperature. Water is then heated so
that together, with the mixture, they will be distilled
off. The resulting container is in an ice bath so the
resulting mixture got crystallized. After crystals are
formed, it is now filtered so that only the pure
1

components would really be left. The resulting


purified sample weighed 1.8 g which is means that
the original sample somehow contains a big amount
of the pure one, and with that, we got 90% as the
percentage recovery.
From the two processes, it can be seen that
although both can work really well, steam distillation
is quit a preferable one. It is because as both deals
with temperature, it can be seen that steam distillation
tends to lower the temperature that will be required
by lowering the pressure that there is in the flask.
Therefore, it prevents the compound to be
decomposed.

4. CONCLUSION
In the experiment, we have dealt with the
analysis and purification of carbon tetrachloride and
p-dichlorobenzene, using simple and steam
distillation, respectively. It can be seen that simple
distillation works well when the substances to be
separated have a large difference in volatility. Also, in
here, increased temperature would make the rate of
distillate droppings to be faster as there would be
more energy applied in the sample, turning it into
vapor faster.
For steam distillation, it can be seen that some
compounds would only exert very little vapor
pressure. With that, one thing to do is find a way to
wherein there would be more vapor pressure, and it is
by adding water as a source. This will then lessen the
needed temperature by making the pressure inside the
flask less.
In a more practical manner, in both methods of
distillation, it should be noted that the condenser
should always be filled with water so that right when
the distillate reaches the resulting container, it will be
in the form of a liquid, due to temperature
differences.
5.

REFERENCES

Baluyot, J. Y., & De Castro, K. A. (n.d.).


Organic Chemistry Laboratory

Student, CHM142L/B21, School of Chemical Engineering, Chemistry and Biotechnology, Mapua Institute of
Technology; ishy.gavino@yahoo.com.ph
2
Professor, School of Chemical Engineering, Chemistry and Biotechnology, Mapua Institute of Technology;
kadecastro@mapua.edu.ph

Manual for Chemical


Engineering Students Part 1.
Pahlavan, D. (2013). Distillation Separation of a Mixture.
Trubiano, C. (n.d.). Simple Distillation
vs. Steam Distillation. Retrieved
2005, from eHow:
http://www.ehow.com/info_8407
975_steam-distillation-vssimple-distillation.html
Yoder, C. (2015). Chemistry. Retrieved
from Wired Chemist:
http://www.wiredchemist.com/c
hemistry/instructional/laborator
y-tutorials/distillation

Figure 3. Steam Distillation Set-up

6. SUPPORTING INFORMATION

Figure 2. Simple Distillation Set-up

Figure 3. Filtered p-dichlorobenzene

Student, CHM142L/B21, School of Chemical Engineering, Chemistry and Biotechnology, Mapua Institute of
Technology; ishy.gavino@yahoo.com.ph
2
Professor, School of Chemical Engineering, Chemistry and Biotechnology, Mapua Institute of Technology;
kadecastro@mapua.edu.ph

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