Title: Fractional Distillation
Objectives: - To separate a mixture of two miscible liquids (liquids that mix in all
properties) with different boiling point.
-To purify a compound by separating it from a non-volatile or less-volatile
material.
Introduction
Fractional distillation is a useful technique to separate and identify two miscible
liquids. Miscible liquids in this case is defined as two distinct liquids with varying
boiling points that are able of mixing completely together. Fractional distillation is
done in the presence of an apparatus called a fractional distillation column. This
fractional distillation column is one of the main components that aids the distillation
process. This fractional distillation tube has multiple trays like structures throughout
the whole length of it. This is to ensure that a maximum surface area is readily
available for the cooling of liquids and also to provide hurdles to the rising vapour
and descending liquids. Distinct liquids boil at varying temperature is the core
principle of fractional distillation. This principle makes it easier to accept the fact that
miscible liquids, although mixed as one, have different boiling points and they
evaporate at different temperatures as well. Heating from the heating mantel causes
one of the liquids to boil and vaporize. Fractional distillation always starts with taking
a mixture of two liquids. Usually, one of the liquids will be more volatile than the
other. The mixture is taken in the distilling flask and is heated. The heating mantel is
set at a fairly low temperature to avoid instantaneous boiling and vaporisation of the
liquids. The mixture slowly boils and vapours start forming. The proportion of the
more volatile liquid is higher in the vapour formed compared to the less volatile
liquid. Vapours then, moves upward the fractionating column. The condensation of
the less volatile liquid heads of first. This cause the rising vapour to contain more of
the higher volatility liquid compared to the lower one and the liquid flowing down
will be more of the less volatile one. These distillation and condensation are repeated.
Vapours of the more volatile liquid reaches the top, taken into the condenser and is
transferred to the container. After repeated series of distillations, the distillation flask
is now filled with the liquid with higher boiling point.
Apparatus and Materials:
Unknown liquid A, unknown liquid B, 50ml round bottom flask, boiling chips, 10ml
graduated cylinder, thermometer, distillation apparatus, heating mantel and test tubes.
Experimental Procedures:
25ml of unknowns A and B were measured and poured into the 50ml round bottom
flask which was the distillation flask in this experiment. The assigned fractional
distillation apparatus were assembled. A few boiling chips were added and the liquids
were distilled into a 10ml graduated cylinder which is the receiving flask in this
experiment. The thermometer was set so that its bulb was right below the arm of the
distillation head. It was also made sure that the bottom of the distilling flask was
touching the heat surface of the heating mantel. The
heating mantel was plugged in and the water was slowly turned on for the condenser,
andheating was begun. The heating mantel was adjusted to maintain a distillation rate
of one drop per second. As the lower boiling component was distilled, the boiling
point of the mixture in the distillation flask will increase. The temperature was
recorded after the first drop was collected and the temperature was continuously
recorded for every 2ml collected. After 10ml of distillate was collected, the graduated
cylinder was emptied into a test tube. The test tube was labelled as component A and
it was kept aside. The next 10ml of distillate was collected and the temperature was
recorded for every 1ml collected. The second 10ml was emptied into a test tube and
was discarded into the organic waste bottle. The collection of the last portion of
distillate was continued until the temperature remained constant. Since the distillation
flask was approaching dryness, the heat source was removed and the distillate
was emptied into a third test tube and was labelled as component B. the boiling point
range of the first fraction of the collected liquid and the third portion was determined.
The unknowns were identified by their boiling points using the possible boiling points
of compounds as a guide. A table of results containing the volume distilled and the
temperature was recorded and a graph of distillate temperature against volume of
distillate was plotted.
Results and Calculations:
Volume distilled (ml) Temperature without column (°C)
0 22
2 53
4 53
6 53
8 53
10 53.5
11 53.5
12 53.5
13 53.8
14 54
15 54
16 54
17 54.2
18 54.5
19 54.5
20 54.8
21 55
22 55
23 55
24 55.2
25 55.2
26 55.5
27 55.8
28 56
29 56
30 56.2
31 56.5
32 57
33 57.1
34 57.5
35 57.8
36 58
37 58
38 58
Observed boiling point of the first compound (A): 52°C
Literature boiling point of the first compound (A): 56 - 57°C
Observed boiling point of the second compound (B): 58°C
Literature boiling point of the second compound (B): 57°C
Compound A is Acetone
Compound B is Methyl Acetate
Discussion
Fractional distillation of two unknown liquids was done in this experiment.
Theoretically, it is expected that the unknown liquid A is acetone and the unknown
liquid B is methanol.
The graph shows the relationship between the temperature and the volume of
distillate. The boiling point of the collected material is actually a range rather than a
point. Based on the graph, the boiling point of unknown A is ˚C and the boiling point
of unknown B is ˚C. We can identify the compound based on their boiling point.
Unknown A is acetone with literature boiling point of 56-57˚C.Unknown B is methyl
acetate with literature boiling point of 57˚C. From the graph, we also can conclude
that unknown B has a higher boiling point compare to unknown A.
These obtained values vary from the theoretical values. This may be caused by a few
factors. Firstly, this difference in temperature may have been caused by the boiling
chips added to the mixture liquid. This is because; the boiling chip may have caused
the liquid to boil at a fast rate causing it to be difficult to have recorded a precise
boiling point. Besides, since the boiling chip was more than required, the temperature
of the heating mantel should have been set in an even lower temperature, to slow
down the boiling process. The position of the thermometer also may have affected the
results. This is because; perhaps the thermometer bulb was placed too low causing the
impure vapour to reach it and give a higher temperature than the theoretical
temperature. Elevation of boiling point is due to the presence of impurities that causes
the observed boiling point to be slightly lower than its true value.
Conclusion
The compound A was found to be acetone with a boiling point °C and the compound B was
methyl acetate with a boiling point of °C. However, compound B obtained was differ from
the theoretical compound due to experimental errors.
References
(1) Distillation Guide. n.d. www.chemhelper.com/distillation.html (accessed July
22, 2018).
(2) “Fractional Distillation .” In Chemical Laboratory II, 49-56. Kampar:
Universiti Tunku Abdul Rahman, 2018.
(3) Fractional Distillation.
n.d.http://academics.wellesley.edu/Chemistry/chem211lab/Orgo_Lab_Manual/
(4) Appendix/Techniques/FractionalDistill/fractional_distill.html (accessed
July 22, 2018).
