Lab 5_ Melting Point
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Lab 5: Melting Point
Goal: To understand the melting point lab skill while using melting point techniques to identify
the given unknown compound.
Background: The physical properties of a compound are not simply numbers that are associated
with it, but rather, very important attributes that can identify what an unknown substance may be.
The melting point is important in identifying a compound as well as determining its purity. A
compound's melting point is usually determined by heating a small amount of compound in a
special melting point apparatus. We have learned that when identifying purity it is helpful to note
that the higher the melting point of the tested compound the purer it is. This was proven to us in
the aspirin lab when the last step was to test the melting point of aspirin which is about 135C, so
the closer we were to that number the purer the aspirin came out to be.
Structures and their melting point:
L-tartaric acid
Chemicals and Equipment Used:
●
Melting point apparatus
●
Aspirin sample
●
Unknown sample
●
Standard sample
Procedure:
1.
3 samples of the recrystallized aspirin and the unknown sample were run separately to
determine their melting point.
2.
In the 2nd run, the unknown was mixed with the standard, and the melting point was
determined
3.
In the 3rd run, a sample of the unknown which has already been identified as urea was
mixed with another standard which has a close melting point, and inserted into the
melting point apparatus.
Results:
Unknown #
19 mp
Aspirin melting point
112C
M.p of unknown sample
134C
M.p of mix (unknown + standard)
132C
M.p of the mix ( unknown + D-ribose
(another STD))
121C
Conclusion:
Based on the results above as well as the given table of melting points, I was able to
come to the conclusion that the melting point of 134C closely resembles that of Urea. Then, once
the unknown was identified as urea, a mix of the unknown was placed with the standard urea
compound to test the resemebelance in melting point. It came out to be 132C which is very close
to the first melting point. A sample of urea was mixed with the standard that I chose to be
D-ribose since its melting point is pretty close to urea ranging between 88-92. A mix of three
compounds was put in the apparatus which was set at 120C and almost immediately the
compounds melted at 121C.
Changes:
●
No significant changes were noted in this lab
Discussion:
As previously discussed, the melting point of a compound is far more than just a number.
This lab demonstrated that by identifying the melting point of a substance that was given to us,
we were pretty accurately able to identify an unknown compound. Some errors that may have
occurred in the process of this lab which could have led to false interpretations is that too much
of one compound could have been added to the the tube when doing the last few steps. For
example, since D-ribose has a much lower melting point than urea, in the last mixture, too much
of D-ribose could have gone into the tube with the unknown and standard causing the mixture to
melt almost immediately. Although this might be a minor error, it is something to be cautious
about the next time this lab is performed.
Questions:
1.
Two substances, A and B, have the same melting point. How can you determine if they
are the same without using any form of spectroscopy? Explain in detail.
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-
To determine if substances A and B are the same, we could mix them and identify the
melting point of the mixture. If the melting point comes back identical to the one of A
and B then it would determine that the mixtures are the same.
2.
Using Figure 9.5, determine which heating curve would be most appropriate for a
substance with a melting point of about 150°C.
-
Based on the given figure, I believe curve number 2 would be most appropriate
for a substance with m.p of 150C
3.
What steps can you take to determine the melting point of a substance that sublimes
before it melts?
-
In order to prevent a substance from sublimation ( turning into gas), the tube in
which the substance is could be sealed so the gaseous phase does not have a way
of escaping. This way it could be easier to note any physical changes.
4.
A compound melting at 134°C was suspected to be either aspirin (mp 135°C) or urea (mp
133°C). Explain how you could determine whether one of these two suspected
compounds was identical to the unknown compound without using any form of
spectroscopy
-
In order to determine this, the mixed melting point technique from question 1
could be completed. Meaning that the two mixtures should be combined with the
standard to determine if the melting point changes or not.
5.
An unknown compound gave a melting point of 230°C. When the molten liquid
solidified, the melting point was redetermined and found to be 131°C. Give a possible
explanation for this discrepancy.
-
During the heating process, the physical property of the compound completely
shifts thus changing its structure and altering the melting point. Once a compound
is resolidified after melting once, it changes.
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