Characterisation and Purificationof

3
Chapter
Chemical Substances
Introduction..
To identify a compound, it must be obtained in the pure form. Compounds obtained
from the natural sources or prepared in the laboratory may contain impurities. So
they need to be purified first. Filtration, recrystallisation, sublimation, distillation,
chromatography, etc. are some of the most common methods used for purification
while the most convenient and commonly used physical properties to test the purity of
a substance in the lab are melting points for solids and boiling points for liquids.

Expériment -r3
AIM:
To determine the melting point of a given substance.
THEORY:
Meting point of a substance is the temperature at which asolid changes into liquid at atmospheric pressure.
When a solid is heated, the kinetic energy of the molecules increases and exceeds a limit that results in
melting of the solid. The liquid thus formed can move freely.

MATERIALS BEROIRED:
Sample, the melting point of which is to be determined liquid paraffin, thermometer, 100 or 150 ml beaker,
stirrer, iron stand, wire gauze, capillary tube 8 to 10cm longand 1 to 2 mm diameter, spatula andtripod stand.
METHOD:
1. Take acapillary tube and seal one end of the capillary by rotating that endof the tube while heating in
the flame of burner. Abulb is formed and the capillary gets sealed.See figure-3.4

Post Inverted
porous
Heap of plate Tap
sample
fense
Push

Sealed capillary

Figure 3.1: Sealing one end of the capillary tube Figure 3.2: Charging the capillary tube
2. Grind the crystalline substance to a fine power. For fillingthe substance make a heap of the powdered
substance on the watch glass. Push the open end of the capillary tube into the heap. Some powdered
substance enters into it. Now gently tap the sealed end of the capillary on the working table. By this
method, you fillthe capillary tube upto 2-3 mm. {Geefigure 3.2]
Chemistry Lab Manual - XI 25
phthalene Acetamide
acid
Choral Benzoic
Benzophenone The
CONOLUSION:
26 hydrate OBSerMelting
VATION: 4. 3.
melting
try Substance errors. 30°C Ifandallow thermometer.
about
substance Heat Surface and (if Fill
pointexperimental it the
is th e a
point again the beaker
of andmore, the 10° m.pt.
the temperature tension outer
Lab Raslt of by when below beaker in is
the substance using the 2/3rd
the Hang above
part
ual given solid the capillary the slowly of
Table: a the the of of
newly wholeexpected to 100°C). th e
Melting substance is Reading is thermometer
- Reading1t°C = is not rise by
bath the volume
Substance Capilary Thermometer
XI Melting filled and capillary
Mean = of continuously
slowly. liquid
pure. the Attach
80.0 57.0 46.0 122.4 82.0 melting also
point 2 capillary. with Figure
points = You solid The iswith
the through enough thewater
in t,t,°C point
°C may
substance
temperature mercury paraffincapillary3.3/Taking
of
t,°C+2°C The stirring
(if
Some repeat (if th e to t he
hloracetic acidPhenol
acid UreaOxalic average its
a-Naphthol =

level the iron hold expected oil tube the

has m.pt. or
Organic the is
Substance
liquidstand thewater to melting
experiment ofmelted. to is in the
°C. the be the capillary
known), melting
inintothermometer point
Compounds two noted
thermometer the (whichever
The the
readings when beaker. tube point
by
rangedecrease beaker.
letting in is is
°C the by
may of While position, taken below Burner
(See Paraffin
Liquid Beaker
Melting substance the when
melting wetting
the
be
rate heatingthe figtre in100"C)
takenliquid attached the the
57.0 132.0101.0 42.0 54.0
Point may temperature
starts of
bath
to heating observe 3.3) thermometer beaker). or
minimise be paraffin
in cool 1-2°Cmelting with
°C
and the The
by is the oi
tri TE M