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Melting Point Range Averages


Discussion: This experiment gave me (the experimenter) great practice for a

procedure used very often in Organic Chemistry. Purification technique is very
import for the practicing chemist, as it allows one to rid their product of impurities.
The first step in the procedure was to find a solvent that would dissolve the
unknown crystals. This is important, as a chemist may not always know what they
are presented with, and trying a number of various solvents to dissolve a compound
is a common procedure in chemistry as well as good practice for dissolving crystals
(i.e. needing to dissolve it at the boiling point, and it recrystallizing when cooled).
After finding the right solvent, the unknown compound was dissolved in the
minimum amount of diethyl ether (the correct solvent), as to not make it difficult to
separate out the crystals from the diethyl ether without losing crystals. After doing
this, I performed a hot gravity filtration of my saturated solution. The reason hot
gravity filtration is used is to avoid recrystallization during the transfer (the energy
from the heated solvent keeps the crystals dissolved). However, an almost
negligible, but unmeasured amount may have been lost during gravity filtration,
and I tried to brush the crystals off the filter paper into the flask (which may have
caused experimental error, discussed later). The purpose of the gravity filtration is
to remove impurities while the dissolved crystals pass through the filter. After this,
the solution was cooled slowly to avoid losing any desired solute, and was then put
into an ice bath and allowed to recrystallize for 2 nights before pouring the solution
onto a vacuum filtration apparatus. This was done to separate the crystals from the
solvent (if not entirely evaporated). Then, I washed the crystals that were stuck to
the flask out with about 30 mL ice water in order to get the maximum amount of
crystal from the recrystallization flask onto the vacuum filtration apparatus. After
transferring all of the crystals onto the apparatus, I washed the crystals on the filter
with ice water (in order to avoid dissolving the crystals). I then weighed the crystals
to see how much made it through recrystallization. Then, three trials of finding
melting point ranges identified the unknown as mandelic acid, however, equivocally.
(this is assuming minimal or no experimental/observational error). The initial weight
was 0.999 g and the final weight was 0.901, meaning (show math above) 9.81% of
the original product was lost during recrystallization. This loss of mass could have
been from the 30 mL of ice water. If the crystal were to be slightly soluble in water,
it could potentially make sense that the 30 mL of ice water caused this small
disparity, and that not much was lost during transfer. The corrected melting point
range averages are 120.5*C, 120.4*C, and 120.5*C. These values give the identity
of mandelic acid, with the possibility of the compound being benzoic acid due to
how close the melting point range is, and acknowledgment of experimental error.
When I brushed the crystals off the filter paper during hot gravity filtration, there is

a possibility that I added impurities from my hands, thus causing a melting point
depression. The amount of impurity would be very small, though, due to the crystals
still having a tight melting point range, and being so ambiguously close to the
melting points of both mandelic and benzoic acid. Referring back to the idea of a
slightly soluble compound; if the identity of the crystal is mandelic acid, it would be
very soluble in water, and likely a significant amount could have been lost. I would
have also seen the crystals dissolve in the flask, which I did not observe. According
to YALKOWSKY,SH & DANNENFELSER, RM (1992), the solubility of mandelic acid at room temp is
181,000 mg/L. (show math above) This means that 30 mL of water would dissolve 5.43 grams. I only lost
0.098 grams of crystal. Even though it was washed with ice water, the crystals would have dissolved when
I washed them out with all that water, and they hardly did. Additionally, benzoic acids solubility in freezing
water is 1.7g/L (show math above) which means that 0.051 g would have been lost, which is much closer
to the 0.098 grams that I lost. The remainder could have been from when I brushed crystals off the filter
paperI could have lost a small amount. This leads me to believe that I simply made an observational
error during the melting point portion of the experiment, and that the identity of the crystal is benzoic acid.