Annum Munir | Chem 230-Lab 3 | Group C

Mairah Talat | Shafqat Rasool :: group members

CHEM 230 - Experiment

performed on Friday, 11
February, 2011
Report submitted on Friday, 18
February, 2011

Separation of a Mixture of Acetone

and Toluene
By Fractional Distillation
Group C: Report submitted by Annum Munir (2013-10-0201)
Group members: Mairah Talat Khan & Shafqat Rasool

Lahore University of Management Sciences (LUMS)-

School of Science and Engineering, Chemistry Department,
Sector U, DHA Lahore 54792
Email: 13100201@lums.edu.pk§

Abstract: The experiment was aimed at practicing the technique of fractional

distillation which is an extremely important tool in organic chemistry for analyzing a
mixture of two or more miscible liquids. Here, the two known miscible solvents used
were Acetone and Toluene, with boiling points of 58 oC and 110 oC respectively.
Known volumes of the two solvents were mixed and then separated by fractional
distillation excluding any impurities that might be present in the samples. The
samples obtained at the end of the experiment were pure solvents and the volume
recovered was within a range of 80-95% of original volume taken.

Introduction:
The use of organic solvents such as
acetone and toluene has gained
immense importance because of their
use in industrial context. Both acetone
and toluene are widely used solvents in
paint, rubber, dilution, extraction and
pharmaceutical industries.1,2 The
occurrence of organic solvents and
volatile organics in the natural
environment has become an important
issue discussed widely in the field of
environment has become an important
(1)"TOLUENE – Industrial Uses."
Scorecard Home. Web. 17 Feb. 2011.
<http://scorecard.goodguide.com/chem
ical-profiles/uses.tcl?
edf_substance_id=108-88-3§>.
environmental protection. A
special focus should be given to the
hazard posed by the increasing amount
of petrochemical solvents, such as
benzene, toluene and acetone because
they are difficult to remove and exhibit
toxic properties. 3 Since the standards
of wastewater disposal are becoming
more and more rigorous, different
separation techniques, e.g. Simple
distillation, vacuum distillation, steam
"ACETONE -- Industrial
(2)
Uses." Scorecard Home. Web. 17 Feb.

1
Annum Munir | Chem 230-Lab 3 | Group C
Mairah Talat | Shafqat Rasool :: group members
2011.
<http://scorecard.goodguide.com/chem
ical-profiles/uses.tcl?
edf_substance_id=67-64-1§>.
(3) Rep. Web. Dorota Panek*,
Krystyna Konieczn
<http://www.desline.com/articoli/7850.
pdf§> distillation and fractional
distillation are used to separate a
mixture of such miscible liquids.
Fractional distillation is a type of
distillation that involves the separation
of a mixture into its constituent
substances based on the differences in
their boiling point (volatility). It is
practiced for those mixtures, in which
the boiling point of the components
differ by less than 25ºC at one
atmospheric pressure. The component
with the least boiling point (acetone in
this case) is separated first, while the
component with the highest boiling
point (toluene) is drawn off at the last.
The fractionating column is usually
composed of plates arranged in a
horizontal manner, which enhances the
separation by allowing condensation,
evaporation and re-condensation of the
separated components. 4 The behaviour
of the measured boiling point during
the course of a simple distillation is
graphed in the figure below.
(4)Sandhyarani, Ningthoujam.
"Fractional Distillation." Buzzle Web
Portal: Intelligent Life on the Web.
Web. 17 Feb. 2011.
<http://www.buzzle.com/articles/fracti
onal-distillation.html>.
In this experiment a mixture of acetone
and toluene is separated and the
volume of two solvents obtained at the
end of the experiment are measured
and recorded.
Results and Discussion:
2
Annum Munir | Chem 230-Lab 3 | Group C
Mairah Talat | Shafqat Rasool :: group members
The two solvents obtained were in pure
form and the volumes were recorded to
be 57 ml for acetone and 49 ml for
toluene. The volume of impurities was
6 ml.
The fractionating column is assembled
by first applying grease to all the joints
and then clipping all the joints to
prevent any leakage. The volumes of
acetone and toluene are separately
measured using a measuring cylinder
and recorded.
SOLVENT INITIAL
VOLUME
Acetone 60 ml
Toluene 60 ml
Total 120 ml
Before measuring the volume the
apparatus is properly washed first by
soap and tap water, then by distilled
water and finally rinsed with the
solvent that is to be measured in the
measuring flask.
Both the solvents are placed in the
round bottom flask and to promote
even boiling of the liquid, magnetic
stirrer is added to the liquid before
starting to heat the flask. The magnetic
stirrer agitates the the liquid which in
turn promotes even boiling. Also, the
surface of the stirrer provides sites for
bubbles of vapour to form. Here an
important caution to take is that a stir
bar is never added to a hot liquid. This
can cause a seemingly calm liquid to
boil suddenly and violently. Magnetic
stirrer is especially used when heating
volatile solvents to prevent bumping.
Due to its small size, a stirring bar is
more easily cleaned and sterilized than
other stirring devices. It also does not
require lubricants§ which could
contaminate the reaction vessel and the
products.
A fractionating column contains
column packing with large surface
area. The vapour of the component
substance after passing the
fractionating column is passed to the
condenser, which is fixed with a water
inlet and water outlet pipe. In the water
inlet pipe, cold water is constantly
supplied to cool down or condense the
separated vapours. Eventually, warm
water after being circulated through the
condenser is removed via the outlet
pipe. The component undergoes
condensation in the condenser, which
is then collected in the collection flask
as a purified liquid. The components
with lower boiling point tend to collect
at the top portion of the fractionating
column, while those with high boiling
point settle at the bottom of the
column. Though fractional distillation
provides better separation of
constituents, it requires more energy
and longer time than the usual simple
distillation. The more the number of
plates, the longer is the distillation. For
these reasons, fractional distillation is
implemented for purifying complex
mixtures with many components. 5
At this stage the distillate should be
dropping with the rate of Ten Drops
per Minute. If the rate is too fast, the
higher boiling impurities may escape
into the receiving flask. If rate is too
slow, distillation will take much longer
time. 6
slow, distillation will take much longer
(5)"Fractional Distillation." The Titi
Tudorancea Bulletin, English Edition.
07 Oct. 2010. Web. 18 Feb. 2011.
<http://www.tititudorancea.com/z/fract
ional_distillation.htm>.
Also if the distillation is conducted too
rapidly and if the exit tube is not large
enough, the vapours are choked
causing an increase in pressure and a
corresponding rise in temperature. The
consequence is this that the observed
boiling point is too high. 7
The volumes of distillate obtained are:
3
 Annum Munir | Chem 230-Lab 3 | Group C
Mairah Talat | Shafqat Rasool :: group members
EXTRACTED VOLUME the flask if the amount of volume left
SOLVENT RECOVERED
Acetone 57 ml (6) Experiment week 3, Lab Manual,
Chem 230 Organic Chemistry Lab-1, SSE
Toluene 49 ml
(7)"Behavior On Boiling And
Impurities 6 ml
Fractional Distillation."
Mixture left in the 8 ml
ChestofBooks.com: Read Books
flask
Total 120 mlGraph of Temperature against time taken for each distillate to separate
120

100

80
Temperature/ Celcius

60

40

20

0
0 5 10 15 20 25 30 35
Time/min

Online for Free. Web. 18 Feb. 2011.

The impurities are collected in a
different flask as after collection of 57
ml of Acetone at a fixed temperature of
58 oC, the temperature started to fall
indicating that another fraction was
now coming out as a distillate. At this
point the flask was changed and
impurities were collected. Then after
sometime, no more distillate came out
and the temperature again started to
rise. After reaching 110 oC, it
remained steady till the time all the
acetone was collected. About 8ml of
the liquid was left in the flask because
otherwise heating could have caused
breakage of the flask if the amount of
volume left is too less.
The graph obtained by plotting the
volume on x-axis and temperature on
y-axis, we get the following figure.
<http://chestofbooks.com/health/aroma
therapy/The-Volatile-Oils-
Vol1/Behavior-On-Boiling-And-
Fractional-Distillation.html>.
Summary and Conclusion:
The experiment was performed to
separate two miscible liquids whose
boiling points were close together.
Acetone separated at 58 oC and
toluene boiled at a higher temperature
of 110 oC. 57 ml of acetone and 49 ml
of toluene were recovered.
Materials and Method:
The lab equipment required for the
experiment include a round bottom

4
Annum Munir | Chem 230-Lab 3 | Group C
Mairah Talat | Shafqat Rasool :: group members
flask (250 mL), a stir bar, a distilling rubber tubing to the sink whereas the
head, a condenser, grease, a lower opening on the condenser brings
thermometer with adaptor, three water in.The water supply is then
receiving flasks, three extension turned on slowly. A small flow of
clamps and fasteners, a heating mantle, water is all that is needed to cool the
two pieces of rubber tubing, a vacuum condenser; too much flow will cause
adaptor, four keck clamps, a heating the tubing to pop off. 9
mantle and a fractionating column
The collecting flasks are replaced
(vigreux condenser).8
thrice. The first ten droplets are
The first step is to place the two stands discarded as they might be impurities.
next to each other within the reach of The next flask collects acetone at 58
o
rubber tubing and the sink as the C. After all the acetone has been
rubber tubing is connected to the sink collected, the next fraction collected
and the condenser and it can be consists of impurities as the
difficult to move the apparatus once it temperature fluctuated between 60-100
o
is completed. Next one of the clamps is C. The last fraction at 110 oC was
attached to the lab stand by screwing toluene and it was collected in the
the open end at the back to provide a fourth flask.
solid attachment to the long, metal rod (9) Dick,, Daniel. "How to Set Up a
on the stand. Fractional Distillation Apparatus |
(8) Experiment week 3, Lab Manual, EHow.com." EHow | How To Do Just
Chem 230 Organic Chemistry Lab-1, SSE About Everything! | How To Videos &
Articles. 07 May 2010. Web. 20 Feb.
2011.
The round-bottomed flask is placed in <http://www.ehow.com/how_6338774
the grip of the clamp such that the _set-up-fractional-distillation-
opening on the flask faces upwards. At apparatus.html>
this point a magnetic stirrer is also
placed into the flask.The fractioning
column is then fitted into the opening The overall assembly looks like as in
on the round-bottomed flask and the Y the photograph below.
shaped adaptor is placed onto the top
of the fractioning column. The other
lab clamp is then attached to the other
lab stand. The grips of this clamp are
horizontal to hold the condenser into
the grips of this second clamp. The
water intake and outflow must be be
facing the sink. Next the condenser is
connected to the Y adaptor and the
connections are secured with a
connector clip. At the outflow of the
condenser, a collection flask is placed.
Lastly, the thermometer is fitted onto
the top of the Y adaptor. The
thermometer must be inside the Y
adapter near the outflow of the adaptor
into the condenser. The higher end of
the condenser is connected with the

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Annum Munir | Chem 230-Lab 3 | Group C
Mairah Talat | Shafqat Rasool :: group members

The samples collected were covered

with aluminium foil and labelled as
shown.

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Annum Munir | Chem 230-Lab 3 | Group C
Mairah Talat | Shafqat Rasool :: group members