Name: Rate:

Course & Section: Date:

Experiment No.8
Physical Properties of Organic Compounds
Determination of Melting Points

Discussion:
As a means of identification of organic compounds and as criteria of the compound we must
rely upon certain physical properties and analytic data. Such properties as melting point, boiling
point, density, refractive index, color, optical rotation, surface tension, and conductivity are among
the determinations usually applied to organic compounds. The most important data are melting
points and boiling points.
The melting points may be defined as the temperature at which the compound changes from
the solid to the liquid state. The range of temperature change required to effect this change is the
melting-point range of the compound, and it gives a definite indication of the purity of the
compound. In general, pure compounds show a sharp melting point (range of 0.5 to 1.0deg.). An
impure substance or a mixture of substances has a considerable range of melting point, unless the
two substance are in the correct proportion and form a molecular complex, and then the mixture is
in reality as pure compound.
The melting point of mixtures will be lower than expected mean of the melting points of the two
components. We may use this effect to prove the identity of an unknown which has the same
melting point as the known compound. If the compounds are identical there will be no lowering of
the melting point of the mixture, but if they are not identical there will be a distinct lowering of the
melting point.
The lowering of the melting point by the addition of a small amount of one substance to
another is proportional to the relative molecular amounts of the two components in the mixture and
a function of the major constituent. It is thus possible to determine the molecular weight of an
unknown substance since this "freezing-point-lowering constant" can be determined easily and the
amounts of the components (in grams) and the gram-molecular weight of the major component are
known.

Reagents and Materials:

Napthalene
Benzoic acid bunsen burner
Urea iron stand
Salicylic acid iron ring
Glycerol iron clamp with extension
Cork capillary tubings - 7 pcs.
Thermometer cork borer stirring rod
Experimental Procedure:
(A.)Prepare a melting-point apparatus using a 150-ml beaker. Fill the beaker with about
two-thirds full of anhydrous glycerol or mineral oil, as advised by the instructor.
Note; after the experiment is finished, the glycerol should be allowed to cool and should be poured
back into the bottle rather than left in the open beaker in your desk. Glycerol is very hygroscopic
and will absorb moisture from the air. Care should be exercised to avoid spilling glycerol in you
desk. Do not heat the glycerol melting-point bath above 200°, if compounds do not melt at this
temperature, record point as "above 200°."
The melting-point tube should be prepared by using the capillaries. Close one end of the
capillary by heating in a burner. Have the capillaries checked by your instructor before putting the
sample inside. The amount of material introduced into the tube should not exceed 1 cm in the tube
length. The material should be pulverized before being introduced into the capillary tube. The tube
should be attached to the thermometer with a small rubber band so that the compound is adjacent to
the thermometer bulb.
Determine the melting point of the following substances: naphthalene, benzoic acid, urea, and
salicylic acid. The bath should be heated slowly with stirring, and the melting points of these
compounds should be in the order given below. If the compound does not melt sharply, record the
temperature range over which it melts, and take the average of the range as the melting point. This
correction is obtained from the mean value of the melting-point, range. This correction is really a
"stem correction" since the contraction of the column of mercury in the thermometer tube becomes
greater as the temperature is raised. Complete the table by looking up in a handbook the correct
melting points of the compounds.
 Compounds: M.Pt. (obs.) Thermometer
M.Pt. (lit.) Correction

Range Ave.

Napthalene

Benzoic acid

Urea

Salicylic acid

On the basis of the thermometer correction data from the above melting points, plot a correction
curve for your thermometer.

+4

-4 50° 75° 100° 125° 150° 175° 200°