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

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

2011. composed of plates arranged in a


<http://scorecard.goodguide.com/chem horizontal manner, which enhances the
ical-profiles/uses.tcl? separation by allowing condensation,
edf_substance_id=67-64-1§>. evaporation and re-condensation of the
(3) Rep. Web. Dorota Panek*, separated components. 4 The behaviour
Krystyna Konieczn of the measured boiling point during
<http://www.desline.com/articoli/7850. the course of a simple distillation is
pdf§> distillation and fractional graphed in the figure below.
distillation are used to separate a
mixture of such miscible liquids.

Fractional distillation is a type of (4)Sandhyarani, Ningthoujam.


distillation that involves the separation "Fractional Distillation." Buzzle Web
of a mixture into its constituent Portal: Intelligent Life on the Web.
substances based on the differences in Web. 17 Feb. 2011.

their boiling point (volatility). It is <http://www.buzzle.com/articles/fracti


practiced for those mixtures, in which onal-distillation.html>.
the boiling point of the components In this experiment a mixture of acetone
differ by less than 25ºC at one and toluene is separated and the
atmospheric pressure. The component volume of two solvents obtained at the
with the least boiling point (acetone in end of the experiment are measured
this case) is separated first, while the and recorded.
component with the highest boiling
point (toluene) is drawn off at the last. Results and Discussion:
The fractionating column is usually

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

The two solvents obtained were in pure area. The vapour of the component
form and the volumes were recorded to substance after passing the
be 57 ml for acetone and 49 ml for fractionating column is passed to the
toluene. The volume of impurities was condenser, which is fixed with a water
6 ml. inlet and water outlet pipe. In the water
inlet pipe, cold water is constantly
The fractionating column is assembled supplied to cool down or condense the
by first applying grease to all the joints separated vapours. Eventually, warm
and then clipping all the joints to water after being circulated through the
prevent any leakage. The volumes of condenser is removed via the outlet
acetone and toluene are separately pipe. The component undergoes
measured using a measuring cylinder condensation in the condenser, which
and recorded. is then collected in the collection flask
SOLVENT INITIAL as a purified liquid. The components
VOLUME with lower boiling point tend to collect
Acetone 60 ml at the top portion of the fractionating
Toluene 60 ml column, while those with high boiling
Total 120 ml point settle at the bottom of the
column. Though fractional distillation
Before measuring the volume the provides better separation of
apparatus is properly washed first by constituents, it requires more energy
soap and tap water, then by distilled and longer time than the usual simple
water and finally rinsed with the distillation. The more the number of
solvent that is to be measured in the plates, the longer is the distillation. For
measuring flask. these reasons, fractional distillation is
implemented for purifying complex
Both the solvents are placed in the mixtures with many components. 5
round bottom flask and to promote
even boiling of the liquid, magnetic At this stage the distillate should be
stirrer is added to the liquid before dropping with the rate of Ten Drops
starting to heat the flask. The magnetic per Minute. If the rate is too fast, the
stirrer agitates the the liquid which in higher boiling impurities may escape
turn promotes even boiling. Also, the into the receiving flask. If rate is too
surface of the stirrer provides sites for slow, distillation will take much longer
bubbles of vapour to form. Here an time. 6
important caution to take is that a stir slow, distillation will take much longer
bar is never added to a hot liquid. This (5)"Fractional Distillation." The Titi
can cause a seemingly calm liquid to Tudorancea Bulletin, English Edition.
boil suddenly and violently. Magnetic 07 Oct. 2010. Web. 18 Feb. 2011.
stirrer is especially used when heating <http://www.tititudorancea.com/z/fract
volatile solvents to prevent bumping. ional_distillation.htm>.
Due to its small size, a stirring bar is Also if the distillation is conducted too
more easily cleaned and sterilized than rapidly and if the exit tube is not large
other stirring devices. It also does not enough, the vapours are choked
require lubricants§ which could causing an increase in pressure and a
contaminate the reaction vessel and the corresponding rise in temperature. The
products. consequence is this that the observed
boiling point is too high. 7
A fractionating column contains The volumes of distillate obtained are:
column packing with large surface

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

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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