Lab Manual
Lab Manual
Lab Manual
AIM
Construction of the phase diagram of simple eutectic like cinnamic
acid – benzoic acid using cooling curves method.
APPARATUS REQUIRED
Thermometer, test tubes, clamp, stand, stirrer, conical flask, spatula,
test tube holder, 50 mL titration flask, Bunsen burner.
CHEMICALS REQUIRED
THEORY
Phase rule is a qualitative treatment of systems in equilibrium. It
enables us to predict in general the conditions that must be satisfied
to a given system to be in equilibrium and the variation that may be
expected among the variables defining its state.
PHASE RULE-
It states that for systems in complete equilibrium in which the
phases can exchange material, heat and pressure-volume work the
following relation holds good
F+P= C+2
P= number of phases
C= number of components
F= degrees of freedom
2 is included to account for the fact that the two intensive variables-
temperature and pressure must be specified to describe the state of
equilibrium.
THERMAL ANALYSIS-
It is a convenient method to study solid- liquid equilibrium. In this
method solid mixture of different components are melted above
their melting point. The resulting liquid melt is cooled slowly and the
cooling curve is constructed by plotting temperature(y-axis) against
time(x-axis). A break in cooling curve indicates crystallization of the
solid whereas a horizontal portion in the curve represents separation
of a second solid and temperature remains constant at this point
indicating the presence of three phases that is- two solids and one
liquid and at this point, F=0 that is the degrees of freedom of the
components is zero. Once the solidification is complete, the
temperature falls gradually giving a smooth curve again.
NOTE: Place the lower melting component at the bottom of the test
tube and above it the higher melting component.
Table 2
0 20 40 60 100
0
20
40
60
-
-
-
-
Table 3
Composition of
cinnamic acid-benzoic Break/°C Halt/°C
acid system (% of
urea)
0
20
40
60
80
100
RESULT
Eutectic temperature = °C
PRECAUTIONS
1. Place the lower melting component at the bottom of the test
tube.
2. Stir the contents in the test tube generously while observing
the temperature.