Boiling point and distillation

A Purification Technique of Liquids

Murooj Abudabaat MPH PCR
Faculty of Pharmacy and medical science
Hebron University
PURPOSE
 1- To learn how to obtain boiling point using
distillation
 2- To differentiate between types of

distillation
 3- To separate two miscible liquids using

simple and fractional distillation

 4- To compare the efficiencies of simple and

fractional distillation.
Introduction :-
 Boiling Point :- The temperature at which the vapor pressure of
the liquid equals the pressure of the atmosphere above the
liquid.

 At the boiling point, bubbles of vapor form within the liquid

and rise unimpeded to the top of the liquid, breaking the
surface tension and releasing the vapor into the atmosphere
above.

 If the pressure of the atmosphere above the liquid is exactly 1

atmosphere, then the temperature at the boiling point is called
the normal boiling point.

 Increasing the Molecule weight will increase the boiling point

 Distillation:-
 Distillation is used for
separation and purification
of liquids. It is perhaps the
oldest separation technique
known. It is most commonly
used to purify a liquid from
either liquid or solid
contaminants by exploiting
differences in their boiling
points.
Type of Distillation
1- Simple distillation can separate compounds cleanly if the difference in
boiling points between the compounds is greater than 70 °C. The process
is useful to further
1- purify relatively pure liquids
2- to get rid of volatile organic solvents
3- to separate the liquid from polymerization products and mineral
impurities.
(( (( ‫ درجه سيليسيوس‬70‫الفرق بيندرجه الغليان للمادتين كبيييير اكثر من‬

2- Fractional distillation is a separation technique that is used when the

boiling point differences of the compounds in a mixture to be separated
are not large enough to employ the simple distillation technique ( Less
than 70 °C) . The components to be separated are collected in different
fractions, whose identity are usually then confirmed via spectroscopy or
TLC (thin layer chromatography).
(( (( ‫الفرق بيندرجه الغليان للمادتين صغير حيث يمكن ان تتبخر المادتينمع بعض‬
Type of Distillation cont.
3- Vacuum distillation is used to purify compounds that can
decompose (‫ ( تتحلل‬before reaching their boiling point at
atmospheric pressure. By lowering the gas pressure above a
liquid, that liquid can be encouraged to boil at a lower
temperature. This is important if it would break down at a
higher one.

4- Steam distillation is also used for high boiling point

substances that decompose before the boiling point is reached.
In this case, instead of using a vacuum, the liquid in question is
mixed with another, immiscible liquid. The presence of the
second liquid causes both to boil at a temperature lower than
the regular boiling points of either liquid.
Example of Steam distillation :-
Naphthalene, a solid at room temperature
that boils at 218°C, can be melted and mixed
with water. Because the two are immiscible,
they will steam distill at a temperature
around 90°C, less than 100°C (the boiling
point of water) and well below 218 °C. In all
steam distillations, the distillate collected will
be a mixture of both liquids, but since they
are immiscible, they can generally be
separated easily via extraction.
Distillation Apparatus
 1- The distillation flask
 2- The distilling adapter
 3- The condenser
 4- The receiving flask

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The distillation flask
1- It is a round-bottom flask and is often referred to
as the pot.

2- The liquid to be distilled should fill the distillation

flask to 1/2 to 2/3 of its capacity.

3- If the flask is too small, the liquid is likely to bump

or foam over into the receiving flask without
vaporizing.

4- If the flask is too large, a substantial amount of the

liquid may be lost as vapor filling the flask. This
residual volume is called the take-up volume.
The distillation flask cont.
((‫)) كيف بدنا نسرع عمليه التبخر خالل التجربه ؟؟؟‬

To promote even boiling of the liquid, pieces of porous clay

plate or silicon carbide chips are added to the liquid before
starting to heat the liquid.
The irregular chips provide sites for bubbles of vapor to
form.
An alternative method for promoting even boiling is to
agitate the liquid with a magnetic stirrer as it is being
heated.
CAUTION: Never add boiling chips or a stir bar to a hot
liquid. This can cause a seemingly calm liquid to boil
suddenly and violently.
 The distilling adapter
 The adapter connects the distillation flask, the
condenser, and the thermometer.
 This type of adapter is often referred to as a
distillation head. The ground glass joints must be
lined up and mated tightly to avoid leakage of the
vaporized liquid.
 Leakage will result in loss of some of the liquid and
will pollute the laboratory environment.
 The position of the thermometer is adjusted so the
bulb is below the adapter sidearm connected 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.
 The condenser
 The condenser cools the vapor causing it to reliquify and directs this
condensate to the receiving flask.
 The most common type of condenser is the water jacketed type shown.
 The water supply is connected to the condenser with rubber hoses. The water
flows in the lower hose connection (most remote from the distillation flask) and
out the upper hose connection. Before turning the water flow on, check the
hose connections carefully to ensure that they are secure and will not pop off.
 An extra margin of security can be gained by twisting wire around the hose
connections.
 The water flow is adjusted so there is a slow, constant flow of cold water to the
condenser.
 During the distillation of very high boiling liquids, it is common practice to cool
the condenser with air instead of water. The thermal shock to glassware from a
large temperature difference between cold water and hot vapor can crack the
glassware.
The Receiving Flask
 The container to collect the liquefied vapor is called the receiver.
 It may be a round-bottom flask, an Erlenmeyer flask, a bottle, or a
graduated cylinder.

 the receiver is connected to the condenser with an adapter. The sole

purpose of the adapter in this case is to direct the condensate from the
condenser to the receiver.
 One important feature of the setup should be noted at this point—the
system is open to the atmosphere. If the liquid being collected has a low
boiling point, it is good practice to cool the receiving flask with a cold water
bath.
 Fractional distillation
 It is similar to the apparatus for a simple distillation
with an extension added to increase the path the vapor
has to travel.
 This extension is called a fractionating column. There
are many types of fractionating columns that are used
in fractional distillation.
 They are all similar in that the surface area, which
contacts the distilling vapor, is increased. The larger
the surface area contacted by the vapor, the more
efficient the column is in separating the components.
 Fractional distillation cont.
There are columns which are open,
columns with glass indentations called
Vigruex columns, and columns which are
loosely packed with glass, metal or
ceramic material

The fractionating column is often

insulated to keep the temperature of the
column nearly constant. If the temperature
of the column fluctuates widely, it is
difficult to maintain a slow, constant
distillation rate. Sophisticated
fractionating columns have regulated
heating coils built into them.
Procedure Simple Distillation.
1) Assemble a simple distillation apparatus as shown in Figure1, using a 50 mL
roundbottom flask as the distillation flask and a 25 mL graduated cylinder as the
receiver.
2) 2) Place a few boiling chips into the distillation flask
3) 3) Add 15 mL of acetone and 15 mL of water into the pot using a glass funnel, taking
care not to spill the chemicals onto the flask heater.
4) 4) Start the flow of water through the condenser. Ask for approval from your
instructor before proceeding to the next step.
5) 5) Heat the mixture to boiling. Adjust the heater to produce distillate at a rate of
about 1-2 drops per 1 second.
6) 6) Record the temperature when you collect the first drop of distillate and again after
every 1 mL of distillate. Continue the distillation until fewer than 5 mL of liquid
remains in the distillation flask.
7) 7) Turn off the heater and lower it from the pot. Allow the pot to cool for a few
minutes. Then turn off the water to the condenser.
8) 8) Make a plot between the temperature (Y axis) and the volume of the distillate (X
axis).
Procedure Fractional Distillation.
 1) Assemble the fractional distillation apparatus shown in Figure 2, using the 50 mL round bottom flask
from part A as the pot and a 25 mL graduated cylinder as the receiver. Use a Vigreux column instead of a
fractionating column.
 2) Place a few boiling chips into the distillation flask.
 3) Add 15 mL of acetone and 15 mL of water into the pot using a glass funnel, taking care not to spill the
chemicals onto the flask heater
 4) Start the flow of water through the condenser. Ask for approval from your instructor before proceeding
to the next step.
 5) Heat the mixture in the pot to boiling. Observe the condensation line as it moves up the Vigreux column.
 6) When the vapors reach the top of the column, reduce the heating rate so the vapor condensation line
remains just above the column and below the side arm of the distillation head.
 7) Maintain the vapor condensation line in this position for 5 minutes to allow the vapor and liquid in the
column to reach equilibrium
 8) Wrap the fractionating column and distillation head with aluminum foil to minimize the temperature
fluctuations.
 9) Adjust the heating rate to produce distillate at a rate of about 1-2 drops per 5 seconds.
 10)Record the temperature when you collect the first drop of distillate and again after every 1 mL of
distillate. Continue the distillation until the temperature reaches 110 °C or until fewer than 5 mL of liquid
remains in the distillation flask
 11)Turn off the heater and lower it from the pot. Allow the pot to cool for a few minutes, then turn off the
water to the condenser.
 12)Make a plot between the temperature (Y axis) and the volume of the distillate (X axis)
 Done
Thank you so much