Experiment 3
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Experiment 3 - 9/27
1
Experiment 3 - 9/27
Katen Gulati
Organic Chemistry Lab
Post-lab discussion and questions:
(1) Calculate the yield of recrystallization and then calculate the “theoretical yield of
recovery after recrystallization”, i.e. yield you should obtain knowing the solubility
unknown in water, weigh of unknown and volume of the solvent you use. Compare your
recovery yield with the theoretical one, and comment if you get markedly lower of higher
yield.
Experiment 3 - 9/27
2
I got a much lower recovery yield compared to my actual yield. This could be
because of the substance being lost during filtration, or because of human error.
(2) Identify your unknown based on the melting point of the pure sample, and
melting points of the mixture of your sample with acetanilide or phenacetin. How much
different was melting point temperature of your pure unknown from the value given in
the manual for the authentic sample? Discuss briefly, what the reason could be for that
difference.
My unknown was phenacetin. The melting of a pure sample of phenacetin is 135
degrees celsius, the melting point of Acetanilide is 114 degrees celsius. The
melting points of my unknown with acetanilide was 94 degrees celsius, and my
unknown and phenacetin was 118 degrees celsius. The melting point of the
mixture with acetanilide melted first at 94 degrees, leaving the pure substances of
the unknown and phenacetin + unknown to be left and to both melt at 118
degrees celsius. This means the unknown had to be phenacetin because of the
same melting point. The melting point was significantly lower than the authentic
sample because of the impurities that were in my sample. There could have been
filtering issues or impure substances which alters the melting point. Regardless,
it was observed that phenacetin was the unknown substance.
(3) Describe briefly what effect on the measured melting point temperature will have
the following:
(a) your sample is contaminated with small amount of material with higher melting point
than your sample.
The melting point will be higher since the small amount of material melts at a
higher point, it will cause the overall substance to melt at a higher point. For
instance, if there was a little bit of phenacetin mixed in with a sample of
acetanilide, there would be some phenacetin properties which cause a higher
melting point.
(b) your sample is not dry.
If the sample is not dry, there can be a lower melting points since the liquid
makes it easier for it to change from a solid to liquid. When a substance is fully
dry, it is a solid and has to melt to a liquid phase.
(c) you heated the sample too fast in the melting point apparatus.
Experiment 3 - 9/27
3
The equillibrium is not fully reached which creates to much variety in melting
points. If the equillibirum is not reached, then there will be a low melting point to
recorded. This is because the system as not fully converted, and has many
impurities.
(4) Suppose you have three test tubes with three substances, A, B, and C with
nearly the same melting point. Describe how would you proof experimentally (having
only melting point apparatus in hand) that these are not the same substances.
Using the Same method we used for the acetanilide, the phenacetin, and the unknown,
we can take two of the substances (B and C) and mix them with A in two tubes. We then
have a test tube with A and B and one with A and C. We test the melting points of these
and if one does not follow the theoretical melting point, then it they are not the same
substances. For example, if A and B have the same melting point as A, then they are
the same substance, and if they do not, they are different substances.
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[A]
Units of Molarity
.00125
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[B]
Units of Molarity
00125
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