Experiment No.

1 
MELTING POINT DETERMINATION

1.  Introduction
Melting point provides useful data for the characterization of organic compounds.  The melting
point of a compound is the temperature at which thermal motion of the molecules is sufficient to break
down the lattice structure of the crystal. This temperature for a given crystal would remain constant
until the solid phase changes to liquid.  Heat added during the process of melting does not bring about a
change in the solid unless it has disappeared.  The heat applied is converted to potential energy of the
molecules which have escaped from the solid to the liquid state.  A crystal which is bound by weak
forces will generally show a low melting point.  Crystals that are bound by strong forces will exhibit high
melting points.  During the process of melting of ionic compounds, much energy is required to rupture
the interatomic distances.  On the other hand, the interatomic attraction of covalent molecules is
generally weaker than the attraction in ionic or electrovalent molecules.  Hence, covalently bonded
substances have relatively lower melting points.  The common types of intermolecular attractive forces
in covalent molecules are those resulting from hydrogen bonding and Van der Waals forces.   

The technique of mixed melting point is based on the fact that  unlike compounds will
eventually act as impurities and cause a depression in the melting point.  The depression of the melting
point is the result of the weakening of the intermolecular forces.  There are instances, however, in which
the technique of melting point is not applicable like in the case of solids that form solid solutions.  In
such cases, the boiling point of a mixture will be higher than any of the compounds.  The increase in the
melting point is attributed to the strengthening of the intermolecular forces.    

The lowering of the melting point by the addition of a small amount of one substance to another
is used in the determination of the molecular weight.

II.  Objectives
1. Recognize melting point value as an index of purity.
2. Experimentally determine melting point using a simple apparatus.
3. Compare the melting point of a pure substance with that of an impure one.

III.  Procedure
1. Prepare 3 capillary tubes.  Seal one end of each by rotating it in a burner flame.

2.  Introduce powdered samples of benzoic acid, stearic acid, and a mixture (stearic acid and benzoic
acid) to each capillary tube, separately.  The samples must be finely ground using a mortar and a pestle
and this should occupy 1 cm in the capillary tube.  The powdered sample inside the capillary can be
pushed downward by dropping the tube with closed end first down a long piece of glass tubing which is
held upright on the table.  This procedure is repeated several times, if necessary.

3. Attach the capillary tube to a thermometer in such a way that the substance is at the level of the
mercury bulb.

4. Fill the Thiele tube (completely dry or free from water) with oil and insert the thermometer with the
sample into it.  Do not allow the thermometer to touch the side of the Thiele tube.  The tip of the
thermometer with the sample must be at the corner where the side of the arm bends.  (See to it that
there is an outlet for pressure in the melting point tube).

5. Heat the oil bath slowly.  A good rate is one where the temperature of the heated oil rises one degree
per minute until the melting point of the substance is approached.  Observe the capillary tube.  Record
the temperature at which the substance starts to liquefy and when the solid has completely
disappeared.  This is the melting point range.  

Note:  Let the temperature of the oil bath lower to about 50 C before using it for another  capillary
o

tube (o another sample).  Place the used oil in a separate container provided by the instructor.