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Omar Alas

CHM 2210
Fractional Distillation Lab
Purpose
The purpose of this experiment was to separate a mixture of Methyl Chloride,
Cyclohexane and P-xylene using Fractional Distillation techniques. The separation
efficiency of Simple and Fractional distillation will be compared.
Theory
Simple distillation can be used to separate components of a mixture that have a large
difference in their boiling points. If two components have a boiling point difference of
less than 40o-50o, simple distillation will not be as successful at separating the
compounds.
When two compounds with relatively close boiling points are heated, the vapor above the
liquid will be composed of both components at the boiling point. Consider the simple
distillation of a mixture of 50:50 A and B, where A has a lower boiling point than B.
when the mixture begins to boil, the vapor will be richer in A, but still have a significant
proportion of B; lets assume the vapor above the boiling point liquid is 66:33 A: B this
vapor would get cooled in the condenser and drip into the receiving flask. A the end of
the simple distillation the receiving flask has been enriched in A and the liquid remaining
in the still pot is enriched in B. To purify A the liquid from the receiver flask composed
of 66: 33 would need to be set in another simple distillation set up, enriching perhaps to
80: 20 A: B. After a series of these vaporization/condensation cycles pure A would
finally be collected.
Fractional distillation can be considered as a series of simple distillations but rather
having many condensers and receivers, the evaporation/condensation cycles occurs at
once. The added surface area in the column can come from glass protrusions like in
Vigreux columns (condenser), the packing material for fractional distillation in this
experiment will come from glass beads (Hemple column).
In fractional distillation, vapor rises up the column and condenses on the packing, then
re-evaporates, rises further up the column and condenses again. This
evaporation/condensation continues up the column and with each cycle the vapor
becomes more and more pure in the lower boiling point component. In this way fractional
distillation accomplishes in one apparatus what would require several simple distillation
setups.
For a fractional distillation of volatile liquids to be successful, it is important that the two
liquids form a solution and that behave in an ideal manner i.e., when the liquids vaporize,
the vapor phase must be enriched in the more volatile component. It should make sense

that if one component has a lower boiling point than the other it should have weaker
forces and should have higher vapor pressure. This being the case, the molecules should
leave the solution at a higher overall rate thus producing enrichment.
It is also important to realize than when heating (or even at room temperature) both types
of molecules are vaporizing simultaneously, though hopefully one escapes in greater
quantity than the other. This is one of the most common misconceptions about
purification through distillation- that the more volatile component just jumps off the
surface of the solution, leaving the less volatile component behind. This would be true of
water in a solution of sodium, but not true at all of a solution of two reasonably volatile
liquids.
The total vapor pressure of a binary solution of two volatile components A and B can be
described as follows.
PxXAP*A + XBP8B
This equation is a combination of Raoults law and Daltons law of partial pressures.
What it is basically saying is that the total pressure of the system is the result o the partial
pressure of each components making up the solution. The partial pressures in turn depend
on the equal quantity of Cyclohexane (80.74o) and P-xylene (138.4o) for example.
Cyclohexane molecules would be escaping at a higher rate. If one had unequal quantities
of two compounds having the same vapor pressures, then the one in larger quantity would
be escaping at a higher rate.
A simple distillation apparatus is less efficient than fractional distillation apparatus, but is
used to purify materials containing only small amounts of impurities with much higher or
lower boiling points.
New Term Definitions
Distillation: is a technique of heating a liquid to create vapor, which is collected
when cooled separate from the original liquid.
Mole Fraction: a unit of concentration, defined to be equal to the number of moles
of a component divided by the total number of moles of a solution.
Vaporization: the phase transition of a substance from the liquid phase to the gas
phase.
Condensation: defined as the change in the state of matter from gas to liquid
phase.
Normal Boiling Point: a special case of the boiling point of a liquid, where the
vapor pressure of the liquid equals the ambient atmospheric pressure.
Distillate: a distillate is the vapor in a distillation that will be collected and
condensed into a liquid.
Refractive Index: dimensionless number that describes how light, or any other
radiation propagates through that medium.

Raoults Law: states that the vapor pressures of a solvent above a solution is equal
to the vapor pressure of the pure solvent at the same temperature scaled by the
mole fraction of the solvent present.
Daltons Law: the pressure of a gas mixture is the sum of the partial pressures of
the individual components of the gas mixture.

Substances Involved

Name

Formula

Molar Mass

Melting
Point

Boiling
Point

Refractive
Index

Density

Amount
Used

Dichloromethane

84.93g/mol

-94.7

39.6

1.424 1.325g/mol

8ml

Cyclohexane

86.16g/mol

6.47

80.74

1.4264 0.7739g/mol

8ml

P-Xylene

106.16g/mol

13.2

138.4

Apparatus

1.49582 0.861g/mol

8ml

Procedure
Three 10ml graduated cylinder were collected each one containing ~8ml of Methylene
Chloride, Cyclohexane and P-Xylene respectively. The three liquids were mixed together
in a 50ml round bottom flask with 2-3 boiling stones.
The fractional distillation apparatus was then assembled nearly identical to the simple
distillation set up, but modified with a packed column to improve separation. the
fractional distillation apparatus was assembled with a packed column between the roundbottom flask and distillation head; The packed column was assembled by filling a
condenser with glass beads. Thick insulation was applied to the fractional distillation
apparatus because reduction of heat loss was critical in this experiment.
The controller was then turned on in order to begin distillation. The procedure was
complete once the total volume reached about ~20ml in order to avoid the glassware to
crack or break.
Data and Calculation

Temperature C

Fractional Distillation Curve for all three


compounds
160
140
120
100
80
60
40
20
0
0

10
Volume (ml)

Mole Fraction
Dichloromethane
(8ml x 1.325g/ml) / 84.93g/mol = 0.1248mol
Cyclohexane
Refactive Index found: 1.4325
(8ml x 0.7739g/ml) / 84.16g/mol = 0.7356mol

15

20

P-xylene
Refractive Index found: 1.4332
(8ml x 0.861g/mol) / 106.16g/mol = 0.0648 mol

Recovery Percent
Dichloromethane
Initial: 8ml Distilled~ 8ml

(8/8)x100% = 100%

Cyclohexane
Initial: 8ml Distilled~6.5ml (6.5/8)x100% = 81.25%
P-Xylene
Initial 8ml Distilled 3.5ml (3.5/8)x100% = 43.7%

Conclusion
A fractional distillation of a 24ml mixture of Cyclohexane, Dichloromethane and Pxylene was performed. The distillate was collected in three fractions with head
temperatures of 46o (~8ml), 84o (~6.5ml) and 106o (~3.5ml) Based on the liquid vapor
curve for the compounds it was concluded that the first fraction contained mostly
Dichloromethane, the second fraction contains mainly Cyclohexane and the third fraction
contains mainly P-xylene based on this results, it appears that the distillation proceeded
fairly efficiently.
Based on theses results and comparing them with the simple distillation results it seems
that the fractional distillation was more efficient.