CHEMISTRY
ASSIGNMENT
NAME: GAYATHRI GADICHARLA
CLASS :11 B
ROLL NO. 17
METHODS OF PURIFICATION OF ORGANIC
COMPOUNDS
Distillation
Types: Simple distillation, Fractional distillation, Steam
distillation
Simple Distillation: This method is used to separate volatile
liquids from non-volatile impurities and the liquids having sufficient
differences in their boiling
points. Liquids having different
boiling points vaporize at
different temperatures. The
vapours are cooled and the
liquids so formed are
collected separately. The
liquid mixture is taken in a
round bottom flask and
heated carefully. On boiling,
the vapours of the lower boiling component are formed first. The
vapours are condensed by using a condenser and the liquid is
collected in a receiver. The vapours of higher boiling components
form later and the liquid can be collected separately.
Fractional Distillation: If the
difference in boiling points of two liquids
is not much, simple distillation cannot be
used to separate them. The vapours of
such liquids are formed within the same
temperature range and are condensed
simultaneously. In this technique, vapours
of a liquid mixture are passed through a
fractionating column before
condensation. The fractionating column is
fitted over the mouth of the round
bottom flask.
Fractionating columns are available in various sizes and designs. It provides
many surfaces for heat exchange between the ascending vapours and the
descending condensed liquid. Some of the condensing liquid in the
fractionating column obtains heat from the ascending vapours and vaporizes.
The vapours thus become richer in low boiling components. The vapours of low
boiling components ascend to the top of the column.
On reaching the top, the vapours become pure in low boiling component and
pass through the condenser, and the pure liquid is collected in a receiver. After
a series of successive distillations, the remaining liquid in the distillation flask
gets enriched in a high boiling component.
Each successive condensation and vaporization unit in the fractionating column is
called a theoretical plate.
One of the technological applications of fractional distillation is to separate
different fractions of crude oil in the petroleum industry.
Distillation under reduced pressure: This method is used to purify liquids
having very high boiling points and
those, which decompose at or below
their boiling points. Such liquids are
made to boil at a temperature lower
than their normal boiling points by
reducing the pressure on their surface.
A liquid boils at a temperature at
which its vapour pressure is equal to
the external pressure.
The pressure is reduced with the help of a water pump or vacuum pump.
Glycerol can be separated from spent-lye in the soap industry by using this
technique.
STEAM DISTILLATION: This technique is applied to separate substances
that are steam volatile and are immiscible with water. In steam distillation,
steam from a steam generator is passed through a heated flask containing the
liquid to be distilled.
The mixture of steam
and the volatile
organic compound is
condensed and
collected. The
compound is later
separated from water
using a separating
funnel.
In steam distillation,
the liquid boils when the sum of vapour pressures due to the organic liquid
(p1) and that due to water (p2) becomes equal to the atmospheric pressure
(p), i.e. p =p1+ p2. Since p1 is lower than p, the organic liquid vaporizes at
a lower temperature than its boiling point.
A mixture of water and the substance is obtained which can be
separated by using a separating funnel. Aniline is separated by this
technique from an aniline–water mixture.
Differential Extraction:
When an organic compound is present in an
aqueous medium, it is separated by shaking it
with an organic solvent in which it is more
soluble than in water. The organic solvent and
the aqueous solution should be immiscible with
each other so that they form two distinct
layers which can be separated by the
separatory funnel. The organic solvent is later
removed by distillation or by evaporation to get back the compound.
Differential extraction is carried out in a separatory funnel.
If the organic compound is less soluble in the organic solvent, a very large
quantity of solvent would be required to extract even a very small quantity
of the compound. The technique of continuous extraction is employed in such
cases. In this technique same solvent is repeatedly used for extraction of the
compound.
The solubilities of various substances in a liquid can also be used to separate
substances from one another. Consider the case of phenol extraction if it is
necessary to extract phenol, it can be preferentially extracted by using NaOH
solution as one of the liquids to be used.
# QUALITATIVE ANALYSIS OF ORGANIC COMPOUNDS
DETECTION OF CARBON AND HYDROGEN.
Carbon and hydrogen are detected by heating
the compound with copper(II) oxide. Carbon present in the compound is
oxidised to carbon
dioxide (tested with
lime-water, which
develops turbidity)
and hydrogen to
water(tested with
anhydrous copper
sulphate,
which turns blue).
C + 2CuO ---2Cu + CO2
2H + CuO --- Cu + H2O
CO2 + Ca(OH)2 ⎯→ CaCO3↓ + H2O
5H2O + CuSO4 ⎯→ CuSO4.5H2O
white Blue
TEST FOR HALOGEN
The sodium fusion extract is acidified with nitric acid and then treated with
silver nitrate.
A white precipitate, soluble in ammonium hydroxide shows the presence of
chlorine, a yellowish precipitate, sparingly soluble in ammonium hydroxide
shows the presence of bromine and a yellow precipitate, insoluble in
ammonium hydroxide shows the presence of iodine.
X– + Ag+ ⎯→ AgX
X represents a halogen – Cl, Br or I.
If nitrogen or sulphur is also present in the compound, the sodium fusion
extract is first boiled with concentrated nitric acid to decompose cyanide or
sulphide of sodium formed during Lassaigne’s test. These ions
would otherwise interfere with silver nitrate test for halogens.
#QUANTITATIVE ANALYSIS OF ORGANIC COMPOUNDS.
SULPHUR
A known mass of an organic compound is
heated in a Carius tube with sodium peroxide
or fuming nitric acid. Sulphur present in the
compound is oxidised to sulphuric acid. It is precipitated as barium sulphate by
adding excess of barium chloride solution in water.
The precipitate is filtered, washed, dried and
weighed. The percentage of sulphur can be calculated from the mass of barium
sulphate.
Let the mass of organic
compound taken = m g
and the mass of barium
sulphate formed = m1g.
1 mol of BaSO4 = 233 g BaSO4 = 32 g sulphur
m1 g BaSO4 contains 32 X m1 / 233 Percentage of
sulphur= 32 X m1 X 100/233 X m.
CARBON AND HYDROGEN
Both carbon and hydrogen are estimated in ammonium hydroxide shows the
presence of one experiment. A known mass of an organic compound is burnt in the
presence of excess of oxygen and copper(II) oxide. Carbon and hydrogen in the
compound are oxidised to carbon dioxide and water respectively.
CxHy + (x + y/4) O2 ⎯→ x CO2 + (y/2) H2O
The mass of water produced is determined by passing the mixture through a
weighed U-tube containing anhydrous calcium chloride. Carbon dioxide is
absorbed in another U-tube containing concentrated solution of potassium
hydroxide. These tubes are connected in series.
The increase in masses of calcium chloride and potassium hydroxide gives the
amounts of water and carbon dioxide from which the percentages of carbon and
hydrogen are calculated.
Let the mass of organic compound be m g, mass of water and carbon dioxide
produced be m1 and m2 g respectively;
Percentage of carbon= 12 X m2 X 100/ 44 X m
Percentage of hydrogen = 2 X m1 x 100/18
