Basra University College of science and Technology

Pharmacy department

ORGANIC CHEMISTRY LABORATORY

Title of Report :-

Distillation

Students Names :

‫علي مكي عبد الحسن‬

Supervised by:

Dr: Ahmed makki

THEORY:

Distillation: It is a process of separation & purification of liquid organic cpd.s by

selective evaporation & condensation. It may result in complete separation (nearly
pure), or, a partial separation that increase the concentration of selected cpd. of the
mixture.
The purpose of Distillation is:

1. Purification of liquid organic cpd.

2. Determination of the boiling point.
3. Separation of liquid organic substances from each other or from a non-volatile
solid cpd.s

Types of distillation:

1. Simple distillation: A method of separating mixtures based on differences

in their volatilities in a boiling liquid mixture. The components in a sample
mixture are vaporized by the application of heat and then immediately cooled
by the action of cold water in a condenser. so, the distillate is identical to the
composition of the vapors at the given temp. & pressure. That concentration
follows Raoult's law. This proses only happen when The liquid bp.s differ
greatly ( 25 ⁰C ), Separating liquids from non-volatile solids or oils
2. Vacuum Distillation: It is the process of lowering the pressure in the
column above the solvent to less than the vapor pressure of the mixture,
creating a vacuum, and causing the elements with lower vapor pressures to
evaporate off. Lowering the pressure below atmospheric results in

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 lower temperature requirements to achieve evaporation for elements of the
distillate, lowering overall heating requirements for the system.
3. Steam Distillation: is a separation technique that harnesses the low boiling
point property of immiscible mixtures. It is predominately used to separate
temperature-sensitive organic molecules from a non-volatile contaminant. The
organic molecule must be immiscible in
4. Fractional Distillation: It is used to separate mixtures in which the
components have boiling points that differ by only a few degrees, by
employing a fractionating column in the distillation apparatus. So, fractional
distillation is a process of collecting separate fractions according to controlled
boiling ranges during the distillation of a mixture of substances.
5. Reflex Distillation: Reflex is a distillation technique involves the
condensation of vapors & the return of this condensate to the system from
which it originated. This method is used to keep or prevent the reactants from
loss by evaporation during a reaction.

Difference Between Fractional Distillation and Simple Distillation:

1. Boiling Point:  Fractional distillation is used to separate liquids with closer

boiling points while Simple distillation is used to separate liquids with
boiling point gaps of at least 25 degrees.
2. Apparatus: Fractional distillation uses a complex apparatus with a
fractionating column while the simple apparatus with a flask to contain the
mixture, a condenser and a flask to collect purified components is used.

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 3. Repetition: The process has to be repeated several times to get the pure
components in the Fractional distillation but the simple distillation is a one
run process.
4. Separation of a Solvent from a Solute: Fractional Distillation cannot be
used to separate a solvent from a solute but Simple Distillation can be used
to separate a solvent from a solute.

Factors affecting distillation

1. The boiling point increases with increase in pressure.
2. Strength of intermolecular forces strong boiling point high.
3. Boiling points increase as the number of carbons is increased.
4. Branching decreases boiling point.
5. Boiling point increases with addition of impurities in it.
6. Polarity of the molecule. the greater Polarity, the higher is the boiling point.
7. The higher molecular weight has the higher boiling.

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Tools and Material:

 boiling flask.
 100 ml of ethanol
 2-3 pieces of boiling chips.
 cold Water
 Thermometer
 Burner
 Distillation flask
 receiving flask
 simple distillation device

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procedure:

1- Put 100 ml of ethanol in a boiling flask

2- Add 2-3 pieces of boiling chips.

3- Start the water running slowly through the condenser.

4- Heat until boiling.

5- Adjust the temperature so that distillation proceeds at 2-3 drops per second.

Discard the first 2-3 ml of the distillate.

6- Continue distillation until you collect 30-60 ml.

7- Record the boiling point of your liquid, Ethanol

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Data:

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Discussion:

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Distillation is one of the most popular separation methods. used industrially. This
operation allows the separation and purification of mixtures of constituents whose
boiling temperatures are different, in taking advantage of the difference in
volatility (ability to evaporate depending on the temperature) of the constituents
then in performing a succession of condensations and sprays to finish with the
recovery of one of the constituents.

Things that should be considered when working on distillation:

 Feed rate: Feed rate to the column should be constant and the Amount of feed
into column= sum of the overhead and bottom products, A feed rate that is too
high or too low can lead to inefficient liquid-vapor contact on the trays, affect
the effectiveness of the separation. Changes in feed rate also has an effect on
column temperatures and pressure at different points.
 Heat input: The latent heat energy added in the reboiler creates vapor flow
from tray to tray up the length of the column. By controlling the amount of
heat added to the reboiler, the amount of liquid vaporized and the vapor rate
up the column can be controlled.
 Pressure: An increase in pressure increases the boiling point of the liquids,
therefore the overall operating temperature of a column goes up as pressure
increased. A decrease in pressure lowers the boiling point and causes overall
operating temperature drops. Pressure increases or decreases vapor density,
which has an effect on vapor liquid contact.
 Reflux: The vapor velocity is stabilized at different feed rates by recycling a
portion of overhead condensate. Reflux increase low boiler concentration
overhead by sending high boilers back down the column.

Total reflux=all the condensate returned to the top of column.

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Zero reflux=all the condensate is drawn off and none is returned.

Slowly heat the distillation flask until the liquid begins to boil. Vapors
will begin to rise through the neck of the distillation flask. As the vapors pass
through the condenser, they will condense and drip into the specified receiver. The
appropriate distillation rate is about 20 drops per minute. Distillation must occur
slowly enough that all vapors condense into a liquid in the condenser.

Many organic compounds are flammable and if the vapors pass through the
condenser without condensing, they may ignite on contact with the heat source.

Pressure relief devices are installed and set below the design pressure. A
distillation column (like many other equipment) needs to be protected from
damage caused by excessive pressure beyond what the column is designed for.
Column can be protected against overpressure by means of pressure relief devices,
such as pressure relief valves, bursting discs or vents.

boiling chips are added to both simple and fractional distillation flask because they
create a more even and controlled boil. In addition, when a liquid becomes
superheated, a speck of dust or a stirring rod can cause violent flash boiling.
Boiling chips provide nucleation sites so the liquid boils smoothly without
becoming superheated or bumping.

The boiling point. is affected by impurities; some may increase the boiling point
others may decrease it & some may not affect it.

Usually, the first few milliliters of the distillate are ignored because it contains
water or volatile impurities. If the liquid is volatile low boiling point the flask is
heated by a water bath rather than by a flame.

References:

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[1] Zubrick, J. W. (1997). Chapter 20:Distillation For Dummies (fromThe

Organic Chem Lab SurvivalManual, 4th Ed.)

[2] Explain the difference in the usage of Raoult’s Law and Dalton’ s Law SMK

Pusat Bandar Puchong 1 -Form 6 (n.d.). Retrieved from

[3] Mujtaba, I. M. (2004). Batchdistillation: Design and operation

[4]  2019. Distillation: The Historical Symbol of Chemical Engineering. The

University of Toledo.

[5] Othmer, D. F. (1982) "Distillation – Some Steps in its Development", in W.

F. Furter (ed) A Century of Chemical Engineering.

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