Group 4 Date Performed: 28 JULY 2017

No.
Section: A06 Date Submitted: 11 AUGUST 2017
Name: ABENOJAR, EUBERT ALFRED L. Professor: ENGR. BENNY MARIE B.
ENSANO
DELA CRUZ, JEFFERSON
GOMEZ, MARY ROSE M.
PEREIRA, CHRISTA LYND A.

Experiment 5
DISTILLATION OF ESSENTIAL OIL FROM LEMON GRASS

I. INTRODUCTION

On heating, the temperature of the liquid increases until the boiling point is reached. Additional heating
causes the liquid to vaporize accompanied by vigorous bubbling of the liquid. The boiling point of a
substance is a physical property of a substance and can be useful for characterizing that substance. The
fact that different substances have different boiling points allows us to separate them. The process of
heating a substance until it is vaporized, cooling the vapors, and collecting the condensed liquid is the
basis of a commonly used purification technique called distillation (Fieser and Williamson, 1993).

Distillation is a commonly used method for purifying liquids and separating mixtures of liquids into their
individual components. Familiar examples include the distillation of crude fermentation broths into
alcoholic spirits such as gin and vodka, and the fractionation of crude oil into useful products such as
gasoline and heating oil. In the organic lab, distillation is used for purifying solvents and liquid reaction
products (Williamson and Masters, 2011).

The most common methods of distillation are simple distillation and fractional distillation. Simple
distillation can be used when the liquids to be separated have boiling points that are quite different.
Fractional distillation should be used when the boiling points are similar.

To understand distillation, consider what happens upon heating a liquid. At any temperature, some
molecules of a liquid possess enough kinetic energy to escape into the vapor phase (evaporation) and
some of the molecules in the vapor phase return to the liquid (condensation). An equilibrium is set up,
with molecules going back and forth between liquid and vapor. At higher temperatures, more molecules
possess enough kinetic energy to escape, which results in a greater number of molecules being present
in the vapor phase (Monson, 2001).
The diagram shows that at lower temperature, there is less molecules present in vapor, while in higher
temperature, more molecules are in vapor.

In this exercise, students should be able

1. To experience in assembling a simple distillation setup
2. To understand simple distillation as a separation method

II. MATERIALS
A. LIST OF CHEMICALS

Finely cut Lemon grass

NaCl
Distilled water

B. EXPERIMENTAL SET-UP

Figure 5.1 Simple Distillation Setup

III. SCHEMATIC DIAGRAM

A. STEAM DISTILLATION
 Weigh in an analytical balance
Fill the beaker with finely cut lemon grass
Weigh again

B. SEPARATION OF THE ESSENTIAL OIL FROM HE STEAM DISTILLATE

IV. DATA AND RESULTS

Table 5.1 Percent Oil in lemon grass

mass beaker + lemon grass
mass beaker
mass lemon grass
mass test tube + stopper + beaker + oil
mass test tube + stopper + beaker
mass oil
% oil in lemon grass

Table 5.2 Steam Distillation of lemon grass

Step Observation
 Lemon grass

During distillation

Liquid Exraction of Oil

Oil

V. POST-LAB QUESTIONS:

1. Site and describe four basic distillation methods.

a. Simple Distillation
This simple distillation may be used when the boiling points of two liquids are significantly
different from each other, this may be used also to separate liquids from solids or nonvolatile
components. In this method of distillation, a mixture is heated to change the most volatile
component from a liquid into vapor. The vapor rises and passes into a condenser which is
usually cooled, like for example, by running cold water around it, to promote condensation of
the vapor, which is collected.
b. Steam Distillation
Steam distillation is used to separate heat-sensitive components. Steam is added to the mixture,
causing some of it to vaporize. This vapor is cooled and condensed into two liquid fractions.
Sometimes the fractions are collected separately, or they may have different density values, so
they separate on their own. An example of this is the steam distillation of flowers to yield the
essential oil and water-based distillate.
c. Fractional Distillation
As determined using Raoult's law, this fractional distillation is used when the boiling points of
the components of a mixture are close to each other. A fractionating column is used to separate
the components used in a series of distillations called rectification. In fractional distillation, a
mixture is heated, so vapor rises and enters the fractionating column, it condenses on the
packing material of the column as the vapor cools. The heat of rising vapor causes this liquid to
vaporize again, moving it along the column and eventually yielding a higher purity sample of the
more volatile component of the mixture.
d. Vacuum Distillation
This Vacuum distillation is particularly useful when the normal boiling point exceeds the
decomposition temperature of a compound. Vacuum distillation is used to separate
components that have high boiling points. Lowering the pressure of the apparatus also lowers
boiling points. Otherwise, the process is similar to other forms of distillation.

2. Explain how a phase diagram of a liquid mixture of two components works.

Phase diagrams are a systematic way of discussing the physical changes mixtures undergo when they are
heated or cooled and when their compositions are changed.

If we are interested in distillation, both the vapor and the liquid compositions are of equal interest and
the two preceding diagrams can be combined into one: The point a indicates the vapor pressure of a
mixture of composition xA, and the point b indicates the composition of the vapor that is in quilibrium
with the liquid at that pressure. If the composition is specified, the pressure at which the two phases are
in equilibrium is fixed.

A richer interpretation of the phase diagram: the horizontal axis shows the overall composition of
the mixture, zA. All points above the solid diagonal line correspond to a system that is under such
high pressure that it contains only a liquid phase (the applied pressure is higher than the vapor
pressure), so zA = xA, the composition of the liquid. All points below the lower curve correspond to a
system that is under such low pressure that it contains only a vapor phase (the applied pressure is
lower than the vapor pressure), so zA = yA.

Points between the two lines: two phases are present, liquid and vapor.

3. In the distilling flask, why is it that we don’t fill it more than two-thirds full?

It is to allow the liquid that is being heated to expand as it evaporates. If a distilling flask is filled more
than two-thirds full, there is a chance of the liquid boiling (or bumping) over into the condenser without
vaporizing that will result in an impure distillate. Also, if the flask were too full, there would be too little
surface area for rapid evaporation and therefore the distillation would be very slow.
 4. It is said that the surface area of the boiling liquid should be kept as large as possible.
However, why is it that too large of a distilling flask should also be avoided?

The reason why a large distilling flask is not recommended in distillation is because it will take time to
distribute the heat within the flask making the process slower. It is true that a higher surface area if the
boiling liquid should be kept as large as possible but in return, using a bigger flask is not recommended
because of the distribution of heat in a small sample in the experiment.

5. If no boiling stone is available, suggest alternative ways to prevent bumping.

As an alternative to boiling chips, many researchers use magnetic stirrers to prevent bumping. For
solutions of low viscosity, this method is quite effective mostly when the round bottom flask is full of the
dalandan sample to prevent the bumping.

6. If you forgot to put a boiling stone in the distillation mixture, would it be wise to put the
boiling stone to a hot superheated liquid?

It would not be wise to put the boiling stones into a hot superheated liquid because the mixture will
react to the immediate temperature changes in the liquid. If boiling stones are placed, the expected
result would be a sudden gush of the liquid and the worst case scenario would result into breaking the
distillery. To prevent this, make sure to place the boiling stones in the mixture before heated.

7. What is the reason for why we position the thermometer below the sidearm of the distilling
head?

The entire mercury bulb must be positioned below the bottom of the sidearm leading to the condenser.
In order to get reliable readings on the thermometer during the distillation, the vapors of the heated
liquid must totally surround and contact the thermometer bulb. Placing the thermometer too high will
lead to a low value for boiling point.

8. Suggest a way for us to know if the flow rate of the water inside the condenser is just right.

Water should always enter from the bottom of a condenser (the end closest to the flask) and exit from
the top of the condenser. Doing it this way always ensures that your condenser will be full of cooling
water. If you set it up the opposite way, and if for some reason the rate of water flow into the
condenser decreased and became slower than the rate of water exiting the condenser, then the
condenser would not remain filled with water. If the reaction were unattended, this could cause
problems.

9. How can we prevent the popping out of rubber tubing from the condenser?

Attach the rubber tubing from the lower end of the condenser to an adapter on the water faucet. Place
the end of the upper outlet tubing from the condenser in the sink or drainage trough. Turn on the water
cautiously; after it fills the condenser and flows out, adjust the flow. Water should flow, not drip, from
the outlet tubing; however, a forceful flow of water is likely to cause the tubing to pop off the
condenser.

10. What do we mean by a forerun in a distillation?

The first material that distills before the temperature stabilizes is called the forerun. The forerun will
contain any low boiling impurities and is usually discarded after checking its purity. The material
collected after the temperature stabilizes is the purified substance. Usually the temperature stabilizes
slightly below the literature value for the boiling point and then slowly creeps up. When the
temperature begins to drop, the distillation is halted by removing the heat from the distillation flask.

11. In a steam distillation, why is it that the distillate collected is either cloudy or milky in
appearance?

The presence of the oil in the condensate will cause the drops forming in the condensor to be cloudy.
Thus, you can estimate when the condensate no longer contains oil by noting the absence a cloudy
appearance. Also, the cloudy or milky appearance is due to the mixture of oil and water in a steam
distillation.

12. How many grams of water must be distilled to steam distill 1.55g of 1-octanol from an
aqueous solution? What will be the composition (w%) of the distillate? The mixture distills at
99.4°C. (Vapor Pressure of H2O at 99=4C is 744 mm Hg) Molar mass 1-octanol = 130g/mol,
molar mass of H2O = 18.02 g/mol [answers: 10g water, 13.4% 1-octanol and 86.6% water]

Since it is an aqueous solution, solvent = H2O ; solute = 1-octanol

Psoln = Χsolvent P°solvent

744 mm Hg = Χsolvent (760 mm Hg)
744 mm Hg
Χsolvent =
760 mm Hg
Χsolvent = ΧH2O = 0.9789
Χsolute = Χ1-octanol = 1 – 0.9789 = 0.0211
Mole fractions: ΧH2O = 0.9789; Χ1-octanol = 0.0211
(1) Calculate moles of 1-octanol and water in sample:

1.55 g 1-octanol x 1 mol = 0.0119 mol

130 g of 1-octanol

0.0119 is 2.11% of what number? Answer: 0.5651  total number of moles

Since mole of water + mole of 1-octanol = 0.5651 and mole of 1-octanol is 0.0119, therefore mole
of water is 0.5532 mole.

(2) Calculate mass of water, given number of moles of water:

0.5532 mol H2O x 18.02 g = 9.9687 g
1 mol of water

Mass of water is 9.9687 g, approximately 10 g.

(3) Calculate percent composition (%)

 Since there is 1.55 g of octanol and 9.9687 g of water in the sample, percent weight of each
component can be calculated as follows:

For water: 9.9687

x 100 = 86.54%
1.55 + 9.9687

For 1-
1.55
octanol x 100 = 13.46%
1.55 + 9.9687

VI. CONCLUSION

Distillation is a process for purifying liquids and separating mixture of liquids into their individual
components. In this experiment, oil was distilled from lemon grass. Steam distillation was the method
used. The oil recovered was very minimal compared to the water collected. In this experiment, it was
found out that lemon grass contains a small amount of oil. This indicates that to collect a huge amount
of oil, a very large quantity of lemon grass must be used.