Duha Adnan Mahmood
2020
Experiment name 4/Distillation
– Introduction
Since organic compounds do not usually occur in pure condition in nature, and are
accompanied by impurities when synthesized, the purification of materials forms
.an important part of laboratory work in chemistry
Four general separation procedures are used frequently in organic work in the
laboratory and in industry: distillation, chromatography, crystallization, and
.extraction
The process used in any particular case depends upon the characteristics of the
substance to be purified and the impurities to be removed. In order to select the
most appropriate process and to employ it effectively it is important that the
student understand the principals involved as well as the correct methods of
manipulation. Simple distillation is one of the most commonly used purification
.methods
Distillation
It is a process of separation & purification of liquid organic compounds by selective
.evaporation & condensation
It may result in complete separation ( nearly pure ) , or, a partial separation that
increase the concentration of selected compound of the mixture
The temperatures at which a liquid distills is a definite value at a given pressure ,
for every pure organic compound called boiling point
:Aim of the Distillation
.Purification of liquid organic compound -1
.Determination of the boiling point -2
Separation of liquid organic substances from each other or from a non volatile -3
solid compounds
:Types of distillation
.Simple distillation -1
.Vacuum distillation -2
.Steam distillation -3
.Fractional distillation -4
.Reflex -5
Simple Distillation
A simple distillation apparatus is shown in Figure 1. This consists of a round-bottomed flask :
connected by means of a distillation adapter to a water-cooled condenser. A thermometer is
held in place in the vertical arm of the distillation adapter by a special rubber connector at a
height adjusted so that the top of the thermometer bulb is 5 – 10 mm below the opening of
the side-arm. A (vacuum) adapter is connected to the lower end of the condenser. The distilled
liquid is collected in a clean, dry receiver, commonly an Erlenmeyer flaks or small mouthed
bottle. To reduce vapor losses and minimize fire hazards, it is desirable to insert the lower end
of the adapter well into the mouth of the receiver. A distilling assembly must have an opening
to the atmosphere to avoid developing a dangerously high pressure within the system when
.heat is applied
vacuum Distillation
The vapors generated in the pot rise up the fractionating column and encounter cooler
.surfaces, upon which they condense (see Figure2)
Some compounds have very high boiling point or unstable to heat. To boil such
compounds it is better to lower the pressure at which such compounds are boiled
instead of increasing the temp. Once the pressure
is lowered to the vapor pressure of the compound , at a given temp., boiling & the rest of
the distillation process can commence. This technique is referred to as vacuum
.distillation
:Steam Distillation
This method is used for the separation of water immiscible compound of low
volatility from non- volatile tarry products which are formed as by-products in
.many reactions
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
: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
Name of experiment: Simple Distillation
Aim of experiment: Purification of Ethanol
:Procedure
.Put 100 ml of ethanol in a boiling flask -1
.Add 2-3 pieces of boiling chips -2
.Start the water running slowly through the condenser -3
.Heat until boiling -4
Adjust the temperature so that distillation proceeds at 2-3 drops -5
.per second. Discard the first 2-3 ml of the distillate
.Continue distillation until you collect 30-60 ml -6
Record the boiling point of your liquid, Ethanol -7
Notes *
.Pure compound's distill over a very narrow range of temp *
The boiling point is affected by impurities; some may increase the boiling *
.point, others may decrease it & some may not affect it
Usually the 1st few milliliters of the distillate contain water or volatile *
.impurities, 2nd portion contains the substance
porcelain chips are placed in the boiling flask withpieces of broken 3 – 2 *
be distilled to prevent bumping by producing a constantthe substance to
.stream of bubbles that keep the liquid in motion
If the liquid is volatile ( low boiling point ), the flask is heated by a water bath *
rather than by a flame
Questions
?Why is it necessary to add boiling chips to the round flask .1
Considering your results, which method is better for separating acetone from .2
ethanol, simple or fractional distillation? Justify your answer. 3.
?What is the purpose of the condenser
In this lab you will separate a mixture of organic liquids by two methods; .4
simple and fractional distillation. In theory, which method should give the better
.separation? Briefly explain why
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