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Chemy 221-1

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16 views5 pages

Chemy 221-1

Uploaded by

nabaa2004.h
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© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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Experiment 1

Melting Point Determination.

Aim
* To determine the melting point of two different pure compounds, urea and cinnamic
acid that have approximately the same melting point range.
* To determine the melting point range of the different mixtures of urea and cinnamic
acid.
* To identify the unknown compound using mixture melting point method.

Introduction
The melting point of a compound is the temperature at which it changes from a solid to
a liquid. This is a physical property often used to identify compounds or to check the
purity of the compound.
Most pure solids typically melt at a sharply defined, single temperature value. It is
difficult, though, to find a melting point because very small amounts of impurity can
cause the melting point to spread out over a range of several degrees. Impurities also
lower the melting point of a substance; this explains why we put salt on icy sidewalks
and roadways. Usually, chemists can only obtain a melting range of 2-3 °C. Melting
begins when the crystal structure of the sample begins to “slump,” or form liquid drops,
and ends when the entire sample is liquid. This is usually sufficient for most uses of the
melting point. For example, if a sharp-melting unknown substance X is suspected of
being identical with some known substance A, the two should have the same melting
points. If A is reported to have a melting point rather different from that observed for X,
the two substances may be identical (the small differences being due to variations in
technique of determining the melting points). Whether they are indeed identical can
often be deduced quickly if a sample of A is available, by determining a mixture melting
point. A mixture of X and A should have the same melting point as that of either
substance alone, provided the two substances are identical.If X and A are not the same
substance (even though they separately have the same melting point), then a mixture of
the two will usually show a lower melting point and a broader melting point range than
either substance alone. This is because each substance acts as an impurity in the other.
Miscible or partially miscible impurities, even when present in small amounts, usually
lower the melting point and broaden its range. A wide melting point range usually
indicates that a substance is impure, but it may also result from the fact that the pure
substance undergoes some decomposition prior to reaching its melting point. In some
cases, the material undergoes a slight liquefaction and contraction at a temperature
below the true melting point; in others, the material may decompose and discolor so
badly that a definite melting point cannot be observed.
Observations and calculations:

An indication of purity can be found with a small melting point range. Impurities
broaden and lower the melting point range of a compound, whereas pure
compounds usually have a sharp, narrow melting point range (1-2°C).

The melting point typically rises with increasing molecular weight. This is because
intermolecular forces (such as van der Waals forces) are often greater in larger
molecules and take more energy (higher temperature) to overcome.
This trend can be seen, for instance, when comparing the melting points of octane
(C₈H₁₈), which has a much greater molecular weight and a proportionally higher
melting point, and methane (CH₄), which has a low molecular weight and a very low
melting point.
-Naphthalene: 80-82°C (observed: 79-80°C, close to the expected value, likely pure)
- Benzophenone: 48-49°C (observed: 45-47°C, slightly lower, suggesting possible impurity)
- p-Anisic acid: 184-186°C (observed: 178-182°C, slightly lower but within reasonable range, likely pure)
- Salicylic acid acetate (acetylsalicylic acid): 135°C (observed: 135°C, matches perfectly, pure)
- 3-Chlorobenzoic acid: 155-157°C (observed: 157-158°C, slightly above, but likely pure)
- Sulfanilamide: 164-166°C (observed: 165-166°C, matches expected values, pure)
-Ferrocene: 173-174°C (observed: 157.5-161.5°C, significantly lower, suggesting impurity)

- Pure compounds based on melting point ranges: Naphthalene, p-Anisic acid,


Salicylic acid acetate, 3- Chlorobenzoic acid, Sulfanilamide
. - Impure compounds: Benzophenone, Ferrocene (as their melting points are
significantly lower than expected).
Discussion
Finding the melting points of two distinct pure solids, urea and cinnamic acid, as well as
urea and cinnamic acid mixes and an unknown chemical, was the aim of this
experiment. First, each sample was made in modest amounts:
100% cinnamic acid,
100% urea,
50% cinnamic acid, 50% urea,
75% cinnamic acid, 25% urea,
25% cinnamic acid, 75% urea,
and an unknown sample.
Each was pounded into a fine powder and set individually on a little piece of permeable
tile. For each powdered sample, a tiny amount was placed into a clean melting point
capillary tube, and the melting points were determined with an appropriate instrument.
It was found that each sample had a different melting point; some melted more fast
than others.

Cinnamic acid melted at 138°C and ended at 151.3°C, while urea melted at 144.2°C and
146°C, respectively. Melting of the mixture of 50% urea and 50% cinnamic acid started
at 116.4°C and ended at 118.5°C. While the 25% urea and 75% cinnamic acid mixture
melted at 117.2°C and ended at 119.4°C, the mixture including 75% urea and 25%
cinnamic acid started melting at 126.8°C and finished at 132.8°C.The unknown
substance was examined based on these findings, and it was found to melt between
145.9°C and 146.7°C. Cinnamic acid was determined to be the mystery substance.

CONCLUSION
There are differences between the melting and boiling points of different compounds. A
material's melting point is the point at which its temperature transitions from solid to
liquid. There is an equilibrium between solids and liquids.

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