Introduction: The method for purifying solids is done by observing the melting point. This is important because if there is an impure substance the melting point would be depression and the melting range would be broader. By finding the melting point of a known substance one can then observe an unknown substance’s melting point to see if the points are the same and try to figure out the unknown.
Experimental Section: The first known substance we used was Biphenyl. 68 degrees Celsius is the known melting point. We used the capillary method and observed the melting point using a Mel-temp device. The next substance whose melting point we observed was 90 % Naphthalene, 10 % Biphenyl. In the last part of the experiment I observed the
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Melting Point (Celsius) Melting Point Range (Celsius)
Trial One 112.1 102.1-112.1
Trial Two 114.7 106.-114.7
Trial Three 114.4 107.1-114.4
The next table shows the melting points of the mixtures made to determine the Unknown. Melting Point (Celsius) Melting Point Range (Celsius)
Trial One: 2-Chloracetamide and Unknown E 117.2 80.8-117.2
Trial Two: 2-Chloracetamide and Unknown E 118.1 81.8-118.1
Trial One: Acetanilide and Unknown E 115.1 106.7-115.1
Trial Two: Acetanilide and Unknown E 113.6 102.0-113.6
Discussion: In part A the melting points I observed were similar to those of my classmates. During the first trial the temperature was climbing quickly and the Biphenyl melted quickly. During the next two trials the Mel-temp was set at a lower setting and our melting point was closer to the known melting point.
Conclusion: I have determined that Unknown E is Acetanilide. The melting point of the mixtures was very close to the melting point of plain Unknown E. The 2-Chloracetamide and Unknown E’s mixture had to high of a melting point. Based on my results and observations I would conclude that Unknown E is Acetanilide.
References:
Fessenden, Fessenden, and Feist. Organic Laboratory Techniques. 3rd Edition. Brooks/Cole. Pacific Grove, CA. 2001. Pgs. 39-46.
Organic Chemistry Laboratory 1, CH
In order to fulfil the labs purpose, the lab was split into two parts. The first part consisted of measuring and determining the freezing point depression of the solution water. The second part consisted of measuring and determining the freezing point depression of a solution that consisted of water and an unknown solute.
No correction had to be made to the melting points because the standard melted in the range labeled on the bottle. The melted point observed is the correct melting point.
I would have liked to do one more trial on each mixture for melting point analysis to confirm that my results were consistent. Furthermore, I would go back and repeat the second experiment to avoid adding HCl to the organic layer in order to separate an accurate weight of the unknown solid and ensure that the purity of the unknown is unaffected by an accidental HCl addition. I am unsure if my results are truly accurate due to the HCl addition and other errors, which means that the experiment would need to be repeated multiple times in order to report a consistent result. In conclusion, this experiment covered the techniques of recrystallization and melting point analysis, both of which are based on understanding physical properties such as water solubility and melting point.
After each of the solids were completely dry, each was placed into a MelTemp device. The temperature at which each solid began to melt and completed melting was recorded.
Maleic acid has a melting point of C and Fumaric acid has a melting point of C. The substance that has a higher melting
Discussion: As seen in the melting point determination, the average melting point range of the product was 172.2-185.3ºC. The melting points of the possible products are listed as 101ºC for o-methoxybenzoic acid, 110ºC for m- methoxybenzoic acid, and 185ºC for p- methoxybenzoic acid. As the melting point of the sample
After the process of recrystallization was completed, the melting points and weights were taken for each solid. Some melting points recorded for the solids were very close to the values listed in the literature. However, others differed by sizeable margins from the values listed in the literature. The range observed for the melting point of naphthalene was 78-81°C. This coincides with
The fact that in both cases the experimentally determined melting point ranges were very similar to the expected melting point ranges indicates that the benzoic acid and benzocaine were purified quite
The experimental melting point was measured to be between 122.3oC and 132.1oC for an average of 127.2oC. The literature melting point is from 160-163oC for an average of 162oC.
The beaker was slowly heated on a hot plate with low stirring until most of the stilbene was dissolved. 0.4 g of pyridinium tribromide was measured and added to the beaker after 5 minutes of heating. Small amounts of ethanol were used to clean the sides of the beaker. The beaker was heated for an additional 10 minutes on low temperature. An ice bath was prepared. The beaker was removed from the hot plate and left to cool to room temperature. Once at room temperature, the beaker was placed in the ice bath for 15 minutes. The solid product was collected through vacuum filtration and the product was weighed and a melting point was taken. Waste was disposed of in the correct waste bins and lab bench was cleaned
The experimental Boiling Point value is 203°C, and the predicted value is 211.58°C by EPIsuite using Adapted Stein & Brown method. The estimate bp value is close to the experimental value, therefore it is accurate enough. The Melting Point is 11.30°C and was predicted by EPIsuite.
The objectives of this lab are, as follows; to understand what occurs at the molecular level when a substance melts; to understand the primary purpose of melting point data; to demonstrate the technique for obtaining the melting point of an organic substance; and to explain the effect of impurities on the melting point of a substance. Through the experimentation of three substances, tetracosane, 1-tetradecanol and a mixture of the two, observations can be made in reference to melting point concerning polarity, molecular weight and purity of the substance. When comparing the two substances, it is evident that heavy molecule weight of tetracosane allowed
To apply thermal analysis to the two-component system, naphthalene-biphenyl at atmospheric temperature. The analysis will be represented by a solid-liquid phase diagram (freezing point diagram).
We first, determined the percent recovery of both vanillin and unknown and then determined the melting range of both compounds. Determining the melting point range, verifies whether or not students purified the compounds properly. Pure compounds tend to have smaller and higher melting points than the original compound. Students worked individually when determining the melting range of vanillin—we were to determine the melting ranges of crude vanillin and the recrystallized vanillin made in the first lab. Moreover, students worked in pairs when determining the melting range of the unknown by using a commercial apparatus. For both solids, we watched the crystals melt. We recorded the temperature at which the solid first began melting and when the solid was completely
Brittain, C. G. (2009). Using Melting Point to Determine Purity of Crystalline Solids. Retrieved from http://www.chm.uri.edu/mmcgregor/chm228/use_of_melting_point_apparatus.pdf