The melting point of a compound is a reproducible, easily measured property of a solid. So a melting point determination is a convenient way to confirm the identity of a compound. Furthermore, because impurities both lower the melting point and broaden the melting point range, taking the melting point of a compound can tell you about the compound's purity. A sample with a broad melting point, if done correctly, would be impure. A sharp melting sample is pure (unless it is a eutectic mixture - optional discussion here).
Melting point and
freezing
point are essentially two aspects of the same phenomenon. Cool a
liquid, it will freeze to a solid; heat a solid, it will melt into a
liquid.
The temperature at which these two processes occur should be the same
(except
if there is supercooling, which we won't need to go into.)
If you think back to
General
Chemistry lab, probably second semester (on this campus it's CHM 112)
you'll
recall a lab called "Freezing Point Depression" aka F.P.
Lowering.
If a solute is added to a solvent, the solvent's freezing point is
lowered.
Typically in these labs you melt (there's that word again) a pure
solid,
or a mixture of two solids, and then let them cool and watch them
freeze.
If the pure solid freezes at 80 degrees, then the mixture will freeze
at,
say, 76 degrees.
In CHM 112, a pure solvent
has a higher freezing point than a solvent mixed with a solute.
Rephrase
& update:
In CHM 245, a pure
solid
has a higher melting point than a solid mixed
with
an impurity.
If the sample you are using is made of large crystals, use a mortar and pestle to grind it into a fine powder. place the sample on a watch glass, and put a small amount of your compound into a melting point capillary. These 4 items are shown here. You can pack the crystals in the capillary by tapping it on the benchtop, or by dropping it through the long tube as described in the "Lab Manual". The crystals should occupy no more than about two millimeters of the capillary.
Here is a picture of the simplest type of melting point apparatus we use, the "Meltemp".
The "Electrothermal" is the other melting point machine we use in Organic Lab I. We have two illustrations of this one, a wide shot and a close-up. You can even look into the melting point apparatus to see the compounds melt. As you can see from the illustration, the tube contents on the left are beginning to melt, the middle one is already melted, and the right one is still solid (also there's a little too much in the tube on the right).
In the first part of
the
lab, you will calibrate the melting point apparatus. The "Lab
Manual"
describes how to take the melting point of a substance that has an
unkown
melting point. FOR THIS LAB, you know the approximate melting
points
of all your samples. You do not have to do a fast
preliminary
determination.
For the calibration,
carefully
take the melting point of three solids. You won't need to label
the
little tubes, because you'll know their contents' melting points.
Please remember that each apparatus has three slots to accomodate
capillaries
- so the melting points can be done side by side by side
sequentially.
The rate of heating should be ~ 1 or 2 degrees per minute near the
melting
point. Between melting points please heat faster - otherwise
the determination of something with a 145o melting point
will
take one to two hours!!
Be sure to record the
m.p.'s
as a range. Compare the highest number in the observed
m.p.
range to the literature values (make sure you've looked these up and
written
them into your bound lab notebook before class.) Apply any
corrections
to subsequent measurements. In future labs, to calibrate the
instrument,
you will measure the m.p. of a known whenever you determine the melting
point of a solid.
In the second part of
the
lab you will be given an unknown. It will be one of three
compounds
which do not differ by much in melting point (all around 130 -
133).
The idea here is to take mixed melting points: mix each
of
the possible compounds with your unknown (a 20/80 unknown to known
ratio
is a good place to start).
If the resulting m.p. is
sharp and up near the expected temperature, then the unknown is
identical
to the compound you mixed it with. If the unknown is different
from
the other compound, it (the unknown) will act as an impurity - a broad
range and a low melting point are expected.
Again you have only three
samples to run. (You don't really need to do the melting point of
the unknown by itself). Again please use the three slots in the
melting
point apparatus. As you heat the tubes, watch for melting.
After two samples melt ... you're finished. Think about it.