Experiment 1

Melting Point Determination of

chemical solids
Objective:

Determination the melting point for pure

substances and mixture of these substances.
 Definition:

Melting Point (m.p.) of a solid: is the temp. range at which it changes state
from solid to liquid.

Melting range: the difference between the temp. at which the sample begins to
melt and the temp. at which the sample is completely melted.

M.P. can give an indication of degree for the substances purity. (useful for
identification).
 Pure crystalline solids have a sharp melting point,
(melting range lower than 2 C).

Impure samples normally have melting range larger than 2 C.

Impure samples melt with a broad temperature range and have lower
m.p. than the pure samples. (WHY???)
Crystalline structure for:

Pure solid Impure solid (mixture)

 Mixed Melting Point - used to determine identity of compound:

Have unknown compound (X)

that melts at 132-134.
What is the unknown?

How could you tell?

(A) Urea (B) Cinnamic acid
MP 131-133 MP 133-134
 Mix unknown compound with a little urea and measure melting point
 Mix X with A, and take resulting melting point

Observed mp = 131-133 Observed mp < 131

Conclusion: (X) = Urea Conclusion: (X) Urea

Mix X with B, and take resulting melting point

Observed mp = 133-134 Observed mp < 131

Conclusion: (X) = Cinammaic acid Conclusion: (X) Cinammaic
acid
Eutectic Mixture
It should be noted, however, that there is one unique mixture
of two compounds, A and B, that has a lower melting point
than any other mixture of the two compounds. This particular
mixture is called the eutectic mixture. The melting point of
the eutectic mixture is called the eutectic point. A mixture
whose composition corresponds exactly to its eutectic
mixture will have a relatively sharp melting point.
Eutectic point diagram
 To generate a eutectic point diagram, it is more
relevant to convert the % composition (% w/w) of
samples into mole fraction for each sample. The mole
fraction ci is defined as (mole of i)/ (total moles). The
mole fraction for a pure substance is 1.00
Example:
Assume you have 100 g of the mixture; let's say 30% urea-70% cinnamic
acid, then,
mole urea = (30 g urea)/ (MW urea)
mole cinnamic acid = (70 g cinnamic acid)/(MW cinnamic acid)
total moles = mole urea + mole cinnamic acid
X urea = (mole urea)/(total moles).
X cinn.acid = (mole cinnamic acid)/(total moles)= 1.00- Xurea
 Experimentally:
1. Take about 50-100 mg of thin, finely powdered samples (if not, then crush the samples
further with spatula against the walls of a small dry beaker) and fill a capillary melting point
tube with the sample by thrusting the open end of the tube into the powder several times.

2. Vigorously tap the seal end of the tube on the table or drop the melting tube, closed end
down, through the length of a glass tubing onto the bench top.

3. Repeat the procedure until the tube contains a 1-2 mm column of densely packed powder
at the bottom.

4. Insert the tube into the melting point apparatus and set up the melting temperature for the
heating apparatus.
Best amount to fill the capillary tube ( 1-2 mm)
THERE IS A SLUSHY MIXTURE

OF CRYSTALS AND LIQUID.

ALL OF THE SOLID HAS MELTED

AND A CLEAR LIQUID REMAINS.

Results & Discussion:
All Questions under the table are required in the report
Final Melting Temp.
Substance Initial Melting Temp. C Melting Range
C

1. Pure Urea

2. Pure Cinnamic Acaid

3. 75Urea-25C.A%

4. 50Urea-50C.A%

5. 25Urea-75C.A %