Objective:

The objective of the experiment is to learn the equipment and operation of fractional distillation, and to
understand the principles of distillation.

Results and Discussion: Fractional Distillation:

Distillation is one of the oldest and still most common methods for both the purification
and the identification of organic liquids. It is a physical process used to separate chemicals from a
mixture by the difference in how easily they vaporize. As the mixture is heated, the temperature
rises until it reaches the temperature of the lowest boiling substance in the mixture, while the other
components of the mixture remain in their original phase in the mixture. The resultant hot vapor
passes into a condenser and is converted to the liquid, which is then collected in a receiver flask.
The other components of the mixture remain in their original phase until the most volatile
substance has all boiled off. Only then does the temperature of the gas phase rises again until it
reaches the boiling point of a second component in the mixture, and so on.
A fractional distillation of liquid mixture of acetone and n-buthyl alcohol
was carried out. A slight modification to the experiment was instead of each acetone of 15 mL and
n-buthyl alcohol of 20 mL was used. The temperature was noted every mL of sample was collected.
The data obtained from the experiment is presented in the following table

Volume of Liquid Temperature Volume of Liquid Temperature

Collected (mL) Observed (oC) Collected (mL) Observed (oC)

1 38 14 94
2 40 15 100
3 43 16 103
4 46 17 105
5 49 18 107
6 52 19 108
7 53 20 108
8 54 21 109
9 55 22 109
10 54 23 109
11 56 24 110
12 86 25 110
13 94 26 110
Table. 1. Data of Volume and Termperature Collected of Fractional Distillation Process

And then the experiment record the temperature of distillate as soon as the first drop is
collected and every several drops thereafter. Once the data is collected, a graph such as the
following is made:
 120

Temperature (oC) 100

80

60

40

20

0
0 5 10 15 20 25 30
Distillate Volume (mL)

Figure 1. Graph of Fractional Distillation of Acetone and N-Buthyl Alcohol

Based on fractional distillation experiments that has carried out on a mixture of acetone
and n-buthyl alcohol substances, the data obtained is that the longer the distillation process, the
more distillate is produced and it has a straight line with an increase in temperature from 1 ml of
sample collected at 38oC until last 26 ml of sample collected at 110oC, until the distillate volume
is 7 mL. temperature has increased, but at 8 to 11 ml of volume collected, the temperature tends to
be stable at 55oC. Then after11 ml of distillate volume, the distillate temperature again increases
highly to 86oC until stable at 110oC

Based on these data, boiling point values for component A and component B can be obtained
where component A in the form of acetone has a range boiling point of 55oC with first volume for
a mixture of acetone substances with a lower boiling point at 38oC, which the distillate obtained
from distillation processes is acetone which has a boiling point for 56oC.This clearly shows that
the first distillate droplet has a boiling point under its pure substance, which indicates that the
distillate is impure. The cause is the weak bond formed between molecules of pure substances with
solvents so that evaporation will occur more easily, in contrast to pure, stronger and more stable
bonds. The vapor pressure in the mixture is also lower due to the comparison of the amount of
substance in the mixture or called the fraction which corresponds to Raoult's law.
In equation form, this reads:

In this equation, Po is the vapour pressure of the pure solvent at a particular temperature.
xsolv is the mole fraction of the solvent. That is exactly what it says it is - the fraction of the total
number of moles present which is solvent.
Because there is a fraction in a mixture causing the pressure of the mixture to be lower and because
of the low vapor pressure (the pressure needed to evaporate the substance), the temperature needed
to evaporate the substance is also low, the temperature is directly proportional to the pressure (ideal
gas equation).

PV = Nrt

Where P is the pressure of the gas, V is the volume taken up by the gas, T is the temperature of the
gas, R is the gas constant, and nnn is the number of moles of the gas.

Then, the mixture compounds are stable at temperature 55oC for evaporation process because
many acetone compound evaporate at that temperature.
Component B has a boiling point range of 110oC. This is almost in accordance with the Safety data
sheet literature which shows that the boiling point of acetone (TA) is 56oC and the boiling point
of n-Buthyl Alcohol (TB) is 117.7oC. This is because when in the mixed phase the second has a
boiling point under its pure substance, which indicates that the distillate is impure. The cause is
the weak bond that forms between molecules of pure substances with solvents so that evaporation
will be easier to occur, in contrast to pure substances that are stronger and more stable. The vapor
pressure in the mixture is also lower due to the comparison of the amount of substance in the
mixture or called the fraction which corresponds to Raoult's law. Because there is a fraction in a
mixture causing the pressure of the mixture to be lower and because of the low vapor pressure (the
pressure needed to evaporate the substance), the temperature needed to evaporate the substance is
also low, the temperature is directly proportional to the pressure (ideal gas equation).
The composition of the vapor formed from a two-phase liquid mixture depends on the
partial vapor pressure of the pure constituents. Thus, if the vapor pressure of component A is high
and that of B low, the mixed vapor will consist very largely of component A. The ratio between
the weights of component A and B will be given by ratio of their vapor pressure multiplied by the
ratio of their molecular weights. As pointed out, boiling will take place only when the sum of the
partial pressures exerted by the components is equal to the pressure maintained in the vapor space,
therefore, a heterogeneous (two-phase) liquid boils or distills at a temperature which at the same
total pressure, always lies below the boiling point of the lowest boiling constituent, so long as the
latter remains in the mixture. that is the reason that the boiling point of the acetone and n-butanol
below the boiling point initially on fractional distillation process
A fractionating column can be insulated to provide a smooth temperature gradient. Maintaining a
uniform temperature gradient within a fractionating column is important because the whole process of
distillation heavily relies on the concept of temperature: it is necessary for proper separation of the
components. As the vapor moves up the column, temperature will decrease away from the heat source; this
will result in the compound with the higher boiling point converting back to liquid and condensing at the
lower area. The temperature gradient uses various condensation-vaporization cycles throughout the process
to separate the different compounds: in the end we then have a maximized amount of the lower boiling
point component in the receiving flask

Conclusion:

Based on fractional distillation experiment on the mixture of acetone and n-butanol substances
that has done, it can be concluded:
1. The point range boiling value for the substance A (Acetone) component obtained by TA at
55oC with the first volume of the acetone compound occurring at a temperature for 38oC.
This result differs little from the literature of boiling point temperature for acetone for 56oC
due to being in the condition of a mixture of substances which affects the vapor pressure
so that the boiling point is slightly below its normal boiling point.
2. The point range boiling value for the substance component B (N-Buthyl Alcohol) is
obtained by TB at 110oC. This result is slightly different from the literature boiling point
temperature for acetone of 117.7oC caused by being in the condition of a mixture of
substances that affect the vapor pressure so that the boiling point is slightly below its
normal boiling point.

Question and Discussion:

1. Please define azeotrope and list one example. What are effects of azeotrope on distillation?

Azeotrope is a mixture of two or more liquids whose proportions cannot be altered or changed by
fractional distillation. This happens because when an azeotrope is boiled, the vapour has the same
proportions of constituents as the unboiled mixture. Because their composition is unchanged by
distillation, azeotropes are also called (especially in older texts) constant boiling point mixtures.

Many azeotropic mixtures of pairs of compounds are known, and many azeotropes of three or more
compounds are also known. In such a case it is not possible to separate the components by fractional
distillation. There are two types of azeotropes: minimum boiling azeotrope and maximum boiling
azeotrope. A solution that shows greater positive deviation from Raoult's law forms a minimum boiling
azeotrope at a specific composition. For example, an ethanol-water mixture (obtained by fermentation of
sugars) on fractional
distillation yields a solution
containing approximately 95% by
volume of ethanol. Once this
composition has been achieved,
the liquid and vapour have the
same composition, and no further
separation occurs. A solution that
shows large negative deviation
from Raoult's law forms a
maximum boiling azeotrope at a
specific composition. Nitric
acid and water is an example of
this class of azeotrope. This
azeotrope has an approximate
composition of 68% nitric acid and
 32% water by mass, with a boiling point of 393.5 K (120.4 °C).
2. For distillation of acetone-n-butyl alcohol mixture, please draw figures of your results and
discuss the differences.
120

100
Temperature (oC)

80

60
Fractional Distillation
40 Simple Distillation

20

0
0 5 10 15 20 25 30
Distilled (mL)

Figure. 2. Comparison of Fractional Distillation and Fractional Distillation

The fractional distillation although faster, is not as effective as the fractional distillation. We can
see by looking at the graphs at figure 2 above that there is no evident separation of the compounds in the
mixture: absence of an immediate spike, but instead we have a steady slope increase. The rise that
we observe from both the experimental data occurs at approximately 11-15 mL. Looking at the 2
compounds in our mixture and for us to determine the boiling points of each, we must look at their
molecular size as both. Acetone evaporates first: its fewer number of atoms results in much more smaller
molecules, and thereby the overall compound displays less intermolecular forces (induced dipoles from
Van der Waals forces) when compared to the n-buthyl alcohol. It will therefore take less energy to
change the acetone state from liquid to gas: we observe on figure 2 the evaporation of acetone at a
temperature of approximately 55⁰C. n-buthyl alcohol evaporates second and last: its higher number of
atoms results in much bigger molecules, and thereby shows a compound that has a greater amount of
intermolecular forces: it has the highest boiling point of the two compounds approximately 110⁰C.
Fractional distillation is a process that can be described as the separation of a mixtureinto
its components parts, and doing so by separating chemical compounds by their boilingpoint. By adding
a fractioning column in Fractional Distillation, we have the ability to create a pure mixture. The texture
of the column and its packing material will make place for a series of condensations and evaporations
to happen in order to enrich the vapor in the lower boiling component. Each condensation-vaporization
cycle enriches the vapor in acetone and return ssome condensate, enriched in n-buthyl alcohol, to the
distilling flask. Enough cycles will result in an effective separation of the vapors. As viewed earlier, the
acetone with the lowest boiling point (approximately 55⁰C) will evaporate first and the n-buthyl alcohol
with the highest boiling point of the two compounds (approximately 110⁰C) will evaporate last. The
peak in temperature that begins at approximately 12 mL shows the evident separation between the two
compounds boiling points
A fractionating column can be insulated to provide a smooth temperature gradient. Maintaining a
uniform temperature gradient within a fractionating column is important because the whole process of
distillation heavily relies on the concept of temperature: it is necessary for proper separation of the
components. As the vapor moves up the column, temperature will decrease away from the heat source;
 this will result in the compound with the higher boiling point converting back to liquid and condensing
at the lower area. The temperature gradient uses various condensation-vaporization cycles throughout
the process to separate the different compounds: in the end we then have a maximized amount of the
lower boiling point component in the receiving flask

3. What are the consequences if temperature is not properly controlled?

The basis function of distillation column is to separate a feedstream into two r more
product streams. The separation may be into accuratively separated individual components or
alternatively into each containing many components and characterized by a range of boiling point.
Its typical that the distillation column will have lower temperatures at the lower part of the column,
assuming that the pressure remains essentially constant throughout. The temperatures reflect
compositions in the column, so the typical measurement, if not control, of temperature at various
points throughout the column and its associated facilities
Temperature isn’t a true measurement of composition for multicomponent mixture but is
a truemeasurement for binary mixture. Determining the best location for temperature measure ng
points is very complex in multicomponent distillation. Product qualities must be maintained in
spite of operating changes and upsets. The temperatures which indicate composition of the product
are those at the top ant the bottom of the column. However, small changes in product impurity
levels, which are usually important in distillations, aren’t indicated by a change of temperature at
the top and the bottom. Small quantitied of impurities have a very small influence on the product
temperature and any changes are completely masked by other variations and the inaccuracy ehich
is inherent in temperature measurements. Thus temperatures at the top and bottom aren’t usually
used for control of a distillation column. If temperature measurements are to be used at all reflect
product purities, they must be made at points in the column at which the amounts of the imputirities
are at relatively high levels, and the product qualities inferred therefrom.
A method and system for controlling distillation columns to minimize the effect of process upsets
uses the sum of temperature measurements from two or more points to control key process
variables. Measurement of more than one temperature point and the adding of temperatures within
the column provides a method of detecting changes in product qualities which may be used to
change the heat input as required to adjust the product qualities. Advantages are gained over
conven tional single point control which does not accurately reflect composition changes,
particularly in multicom ponent distillation and differential temperature con trol, which may be
unstable. Typically, a properly se lected temperature point in the upper section of the column is
combined with a corresponding temperature measurement in the lower section of the column. The
two temperatures are added and the combined signal is used to adjust heat input to the reboiler,
thus varying the vapor and liquid rates throughout the column and thereby controlling the product
qualities.