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Experiment 1: Melting Point Determination
Isiah Brown
Lab Partners: Christian Trevino, Ricardo Amaya, Kiana Flores, Ezekiel Salazar
TA: Seetham Naidu Mudila
February 6
th
, 2024
Introduction:
Melting point is the temperature at which a solid melt and becomes a liquid is the melting
point. At the particulate level, the equilibrium temperature corresponds to the unique vibrational energy level which is just sufficient to shake loose the surface layer of solid molecules from the attraction of the underlying solid layer, allowing them to enter the contacting liquid layer (Young, 2013). Melting point determination identify compounds or to check the purity of the compound. It is a standard practice to carry out a rapid melting point determination initially to establish an approximate melting point and the carry out at least two determination. By heating more gently temperature changing only about 2°C/min until two consistent values is obtained
Melting point is the temperature at which a solid melt and becomes a liquid is the melting point. At the particulate level, the equilibrium temperature corresponds to the unique vibrational energy
level which is just sufficient to shake loose the surface layer of solid molecules from the attraction of the underlying solid layer, allowing them to enter the contacting liquid layer. Melting point determination identify compounds or to check the purity of the compound. It is a standard practice to carry out a rapid melting point determination initially to establish an approximate melting point and the carry out at least two determination. By heating more gently temperature changing only about 2°C/min until two consistent values is obtained.
Pre-Lab Questions:
1.
What is the definition of the melting point range? Use figure 2 to describe which temperature would you note for the melting point range.
-Whenever the meniscus forms is when it starts melting
2.
Benzoic acid has a m.p. of 121-122. If you have a sample of benzoic acid contaminated with some ethanol. What melting point would you expect for this sample?
-I would expect the melting point to drop in degrees, maybe about 10-15 degrees
3.
If you heat too fast, will your observed melting point be higher or lower than the true value?
-It is often higher than the actual melting point
4.
Why do you need to calibrate your melting point apparatus?
-If not calibrated correctly then your melting points will be off by a certain temperature difference
5.
Explain why do you need to grind the sample before filling in the capillary tube?
-If not grinded down to a fine enough powder then it may get stuck in the middle of the capillary
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Materials:
MEL-TEMP
Melting point capillaries
Watch Glass
Stirring Rod
Glass Tube
Spatula
Mortar and Pestle Procedure:
First we set up the MEL-TEMP apparatus and calibrated it to reduce as much error as we could. We then obtained 3 capillaries of the same chemical and placed them in the melting point apparatus to observe their melting point ranges. Each substance was observed in order to minimize any errors that may have occurred. The experimental values were used to calculate the correction factor compared to the actual melting points of each substance. Next an unknown organic substance was obtained. Using two trials of obtaining melting point, the identity of the organic compound was obtained by comparing the experimental values to the actual melting point values of organic substances. Then a vial of an unknown substance and benzoic acid was obtained. They were mixed together and melted to obtain the melting point of the mixture. The range would be benzoic acid if it was consistent with the original melting point range of the experimental benzoic acid. If the melting point range was lower for the mixture, it is deemed naphthol.
Data and Calculations:
Chemical
Actual Melting Point
Observed Melting Point Range
Error
Middle Acetanilide
113 ºC
113-114 ºC
-1 ºC
Left Acetanilide
117 ºC
113-114 ºC
-1 ºC
Right Acetanilide
117 ºC
113-114 ºC
-1 ºC
Unknown
122 ºC
121-122 ºC
-1 ºC
-
Middle Acetanilide started showing changes at 111ºC. -
Left Acetanilide started melting at 115ºC.
-
Right Acetanilide started melting at 115ºC.
-
Temperature increased by 1ºC every minute.
-
Average starting melting temperature – 115+111+115/3=113.66ºC
-
Average end melting temperature – 117+113+117/3=115.66ºC
-
Unknown started at 110ºC and increased 1ºC every minute
-
At 122ºC the unknown started to melt
-
Unknown substance ended melting at 122ºC
Observation and Discussion:
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Observation: We observed 3 different samples of the same chemical at the same time. While two
of the samples resulted in the same results, one of the samples did not. The reason for this could
be that two of the samples had impurities causing the melting point to be different. The unknown
compound melted at 122ºC so with those results we concluded that we had either benzoic acid or
2-naphthol. We mixed the unknown with benzoic acid and naphthol, after this we placed them in
the apparatus. We observed the one mixed with naphthol melted faster so the right unknown
compound was benzoic acid.
Discussion: The melting point range is the range of points at which a solid will melt into a liquid (a phase
change). The melting point of a substance can help identify an organic compound and determine
this substance’s purity. Calibrating the apparatus because it can become inaccurate at different
temperatures if not calibrated. Calibration is important because it will ensure that accurate results
are obtained and errors are minimized.
Conclusion:
The experiment was successful because we were able to understand how the melting point of a substance can be measured. The unknown substance in part two was correctly identified as m-dinitrobenzene. The correction factors for all of the substances were relatively low and this difference could have been due to the apparatus not peaking or an impurity developing in the substances due to exposure
Post-Lab Questions:
1.
Did your measured m.p. of acetanilide match with literature value? Yes
If yes, what is the temperature difference = 0ºC
2.
Report the following data of your measurements:
Unknown sample #1
m.p. of pure unknown: observed 122 ºC, calibrated
m.p. of mixture(A), unknown with Benzoic Acid=122 ºC
m.p. of mixture(B), unknown with 2-naphthol-122 ºC
Conclusion: Unknown sample#1 is Benzoic Acid
3.
You and your partner measured melting points of the same sample. You observed a melting pointof 115-118 ºC, while your partner observed a melting point at 121-123 ºC. Explain how you can obtain two different values of the same sample.
-Impurities can cause the melting points to be different 4. Draw the structures of naphthalene and sulfanilamide, and provide their literature melting points. What factors influence their respective melting points?
80 ºC 165 ºC Since sulfanilamide can form H-Bonding and also is more polar than Naphthalene hence its melting point is higher
5 In case you have no advanced melting point apparatus such as the MEL-TEMP available, how would you determine the melting point. Suggest a simple method
-A thermometer could be an alternative, having it in the mixture and keeping an eye on it.
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