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3 Simple Distillation 1

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34 views9 pages

3 Simple Distillation 1

Uploaded by

kareemadel
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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‫وزارة التعليم العالي والبحث العلمي‬

‫جامعة المعقل‬
‫قسم هندسة النفط‬
‫مختبر الكيمياء العامة‬
‫)‪EXPERIMENT (3‬‬
‫‪simple distillation‬‬

‫‪M.sc. Saja abdulhussein‬‬


Introduction
Distillation is the method of separating the components of a solution which
depends upon the distribution of the substances between a gas and a liquid
phase .Distillation may be done in two ways :

1. Production of vapor by boiling the liquid mixture to be separated and


condensing the vapor without allowing any to return to the still ,there is no
reflux.

2. Returning a part of condensate to the still under such conditions that this
returning liquid is brought into intimate contact with on their way to
condenser..
There are several types of distillation technologies:
Class 1: Simple distillation. Separating liquids boiling below 150°C at one atmosphere
(1 atm) from :
a. Nonvolatile impurities.
b. Another liquid that boils at least 25°C higher than the first. The liquids should dissolve in each
other.
Class 2: Vacuum distillation. Separating liquids that boil above 150°C at 1 atm from:
a. Nonvolatile impurities.
b. Another liquid boiling at least 25°C higher than the first. They should dissolve in one another.
Class 3: Fractional distillation. Separating liquid mixtures, soluble in each other,
that boil at less than 25°C from each other at 1 atm.
Class 4: Steam distillation. Isolating tars, oils, and other liquid compounds that are
insoluble, or slightly soluble, in water at all temperatures. Usually, natural products are steam
distilled. They do not have to be liquids at room temperatures. (For example, caffeine, a solid,
can be isolated from green tea.
Simple distillation
This technique is used when the impurity dissolved in the liquid to be purified is a
substance Non-volatile (i.e., a solid or other liquid with a high boiling point), the
presence of these impurities leads to a decrease in the vapor pressure of the
liquid, and figure (1) illustrates this effect, in this curved (figure 1) represents the
relationship between the liquid vapor pressure and the temperature of the pure
liquid under atmospheric pressure The normal (760mm / Hg), and
from this salt it can be seen that the boiling point is 60 ° C. Curve 2
represents the same relationship for the same liquid that contains
non-volatile impurities, and it is clear that the vapor pressure at any
temperature is lower than the vapor pressure of the pure liquid at the
same temperature. Therefore, we find that the clearance of the liquid
through the marrow is higher than the pure liquid under any
pressure. For example, under a pressure of 760mm / Hg, the boiling
point of the impure liquid is 69 ° C, while it is 60 ° C for the pure
liquid.
Figure 1 The relationship between vapor pressure Figure 2 The relationship between vapor pressure
and temperature of a pure liquid 1 and a liquid and temperature
containing impurities
To perform the simple distillation process, the device shown in Figure (3) is used.
It consists of a distillation flask (round-bottom flask) that is filled in the middle
with the liquid to be purified and a distillation head is fixed on it by passing
through a thermometer so that its connection is at the level of the collateral arm
Distillation. A condenser is connected to this arm, and an adapter link is fixed at its
end to reach a receiving flask in which the distillate is collected. A conical flask or a
graduated cylinder can be used to receive the distillate. The process begins with
adding 2-4 boiling chips to the liquid to be purified (boiling stone works to regulate
the boiling process), then the beaker is heated with a suitable heating method
(preferably electric) until the liquid inside boils (the liquid vapor pressure is equal
to the external pressure),Then the vapor rises from the distillation head and when
it passes by the side arm meets the cold inner surface of the condenser, the vapor
condenses and exits from the other end of the condenser in the form of droplets
that collect in the receiving flask.
Figure 3 A complete, entire simple distillation setup
The process of simple distillation should be carried out so
that it is modified the droplets come out about 3-4 drops
every minute. We notice a drop of the condensed liquid
attached to the thermometer bulb constantly and here
the liquid and its vapor are in equilibrium, the recorded
temperature is the true boiling point and when the
amount of heat increases, the vapors are in a state above
the boiling point (super heating) The drop in the
thermometer bulb disappears and the temperature rises
above the boiling point.
Procedure
Place a 50ml round beaker of pure methanol and add two pieces of
boiling stone. Place the distillation head on top of the beaker and
attach it to the condenser.
And make sure that all connections are tight (set up the device as in
figure (3). Start by gently heating the beaker until the liquid inside
it begins to boil, then adjust the heating rate so that the vapor
condensation ring moves around the thermometer bulb and the
vapors begin to enter the condenser. Liquid droplets coming out 3 -
4 drops per minute, record the temperature when 5, 10, 15, 20 ml
of the droplet have accumulated. When the volume of the collected
droplet reaches 20 ml, stop the distillation process by removing the
heat source. Relationship between boiling point and volume of the
distillate.

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