Researcher

Stephanie Costa

Objective

To determine the solubility of cinnamic acid in DMSO and THF at 25C and 0C. The additivity of the volumes is assumptive .

Procedure


These are the initial reactants for the experiment
Sample 1- 7.1472 g cinnamic acid and DMSO at 25C
Sample 2- 7.1420 g cinnamic acid and THF at 25C
Sample 3- 7.1005 g cinnamic acid and DMSO at 0C
Sample 4- 7.0718 g cinnamic acid and THF at 0C

The solubility of cinnamic acid in DMSO and THF at room temperature and 0C was tested by first dissolving the cinnamic acid into the solvents with a 47-51C hot water bath. The supernatant of cinnamic acid and THF was poured off while the test tube was still hot. The supernatant was used for the remainder of the experiment. The solutions (test tubes 1 and 2) were cooled to room temperature (24C). The solutions (test tube 3 and 4) were cooled to 1C. The solubilities were found using the density method.

Results

Density Sheet

Calculation sheet

There was not precipitate in the test tubes of DMSO at either 24C or 1C. The solubility for cinnamic acid in THF at 1C was unable to be measured. There was not enough solution for a 1mL volumetric flask measurement.

The solubility of cinnamic acid in THF at 24C was 2.329M.

Because the solution of cinnamic acid and DMSO yielded no precipitate when a 3M was made, this solubility of this solution could not be determined.
[In the case of DMSO where you got no precipitate >5M you can report this as miscible - do you know how to do that? JCB]
[Also add both values to the solsum sheet JCB]

Picture 1
[Pics should go under results - add a brief caption and remove all white space around the image JCB]

243-1.png
All 4 samples in the hot water bath

Discussion

There are predicted solubilities of cinnamic acid in THF. The predicted value was 1.890 M. The solubility obtained from this experiment was 2.329M.

There was no precipitate in the DMSO solutions, therefore, no solubility measurements could be taken.
However, the predicted solubility of DMSO was 1.972M.
[You had the wrong CSID in that link - I fixed it JCB]
[How do your results compare with the predicted values?]

Upon looking at the recently updated version of the predicted solubilities sheet (2012-03-25), the solubility values changed. The predicted value of solubility for THF is 1.528M and DMSO is 6.339M.

The predicted solubility of DMSO is 1.972 M. However, no precipitate was formed when a 3M concentration was made; therefore, no solubility was able to be measured.

The predicted solubility of THF is 1.890M. Precipitate was not formed when a 3M concentration was made (EXP242 ). However, precipitate was formed when a 5M solution was made. Therefore, the actual solubility of cinnamic acid in THF, 2.329M, is higher than predicted by the Solvent Selector.

Conclusion

The objective of this experiment was to determine the solubility of cinnamic acid in DMSO and THF at 25C and 0C. The temperatures in reality was 24C and 1C. The two test tubes (1C and 24C) with cinnamic acid and DMSO did not show any visible precipitation. The test tube with cinnamic acid in THF at 1C did precipitate, however, there was not enough liquid available for measurement. The solubility of cinnamic acid with THF at 24C was measured to be 2.329M.

Log

2011-12-8

9:35- the hot plate was turned on to 100C.
9:52- the hot water bath was 33C
9:53- cinnamic acid for sample 1 was weighed out (7.1472g) and added to test tube 1
10:05- The hot water bath was 39C. Cinnamic acid for sample 2 was weighed out (7.1420g) and added to test tube 2.
10:12- the hot water bath was 41C. Cinnamic acid for sample 3 was weighed (7.005g) and added to test tube 3.
10:20- the hot water bath was 43C. Cinnamic acid for sample 4 was weighed (7.0718g) and added to test tube 4.
10:29- the hot water bath was 45C.
10:36- the hot water bath was 46C. DMSO was added to test tubes 1 and 3 to the 3/4th mark.
10:39- the hot water bath was 46C. Test tubes 1 and 3 were inverted and parafilm was added around the cap.
10:43- the hot water bath was 47C. THF was added to test tubes 2 and 4 to the 3/4ths mark. Test tubes with DMSO (test tubes 1 and 3) contracted, the volume was less than 3/4th in those tubes.
10:50- the hot water bath was 48C.
10:51- all of the test tubes were added into the hot water bath. The temperature of the hot water bath was 47C.
11:02- the temperature of the hot water was was 47C. Solute was seen in all test tubes. The test tubes were inverted and replaced into the hot water bath.
11:03- the ice bath was started. The initial temperature of the ice bath was 5C.
11:07- the room temperature bath was started. The intitial temperature was 22C.
11:08- the hot water bath was 47C. Solute was seen in all four test tubes.
11:09- the hot water bath was 48C. All four test tubes were inverted and replaced in the hot water bath.
11:11- picture 1 was taken. The room temperature bath was 22C. The temperature of the ice bath was 3C.
11:14- Solute was seen in all test tubes. The temperature of the hot water bath was 47C. the temperature of the hot plate was increased to 105C. All test tubes were inverted and replace into the hot water bath.
11:16- the room temperature bath was 22C. the ice bath was 3C.
11:17- all four tubes were sonicated for 5 seconds.
11:18- the test tubes were inverted and replaced into the hot water bath (48C). The room temperature bath was 22C and adjusted with warm water.
11:19- the hot water bath was 48C. No solute was seen in test tubes 1 and 3. Solute was seen in test tubes 2 and 4.
11:24- the hot water bath was 48C. solute was seen in test tubes 2 and 4. Test tubes 2 and 4 were sonicated for 10 seconds.
11:25- the hot water bath was increased to 110C. The room temperature bath was 29C and was adjusted with ice. The ice water bath was 3C and adjusted with ice.
11:28- The hot water bath was 49C. Solute was not seen in test tubes 1 and 3. Solute was seen in test tubes 2 and 4. The room temperature bath was 25C. The ice water bath was 2C.
11:29- test tubes 2 and 4 were sonicated for 10 seconds and placed back into the hot water bath.
11:32- the hot water bath was 49C. Solute was still seen in test tubes 2 and 4. The room temperature bath was 25C. The ice bath was 1.5C.
11:35- the hot water baht was 49C. Test tubes 2 and 4 were sonicated for 10 seconds and replaced into the hot water bath.
11:39- the hot water bath was 50C. Solute was seen in test tubes 2 and 4. Solute was not seen in test tubes 1 and 3. The room temperature bath was 25C. The ice bath was 1C. Ice was added to the ice bath.
11:42- The hot water bath was 50C. Solute was still visible in test tubes 2 and 4. The room temperature bath was 25C. The ice bath was 1C.
11:46- the hot water bath was 51C. Solute was seen in test tubes 2 and 4. The room temperature bath was 26C. The ice bath was 1C.
11:51- The hot water bath was 51C. The hot plate was turned off. Solute was still seen in test tubes 2 and 4. The room temperature bath was 26C. A small amount of ice was added to the room temperature bath. The ice bath was 1C and was adjusted with ice.
11:53- the solutions in test tubes 2 and 4 were poured off into new test tubes (labeled with the same numbers). The original solute and test tubes were discarded.
12:00- Test tubes 1 and 2 were placed into the room temperature bath (24C).
12:02- The ice bath was 1C. Ice was added to the ice bath.
12:03- The ice bath was 1C. Test tubes 3 and 4 were added to the ice bath.
12:07- The room temperature bath was 24C. Precipitate was visible in test tube 2. No precipitate was visible in test tube 1. The ice bath was 1C. Precipitate was seen in test tube 4. No precipitate was seen in test tube 3.
12:11- the room temperature bath was 24C. test tube 1 had not precipitate. Test tube 2 had visible precipitate. The ice bath was 1C. No precipitate was seen in test tube 3. Precipitate was seen in test tube 4. In test tube 4, very little solution is seen, this will need to be strained in order to obtain a sample for the density measurement.
12:13- The density of room temperature of test tube 1 was measured (*after the measurements were taken, I remembered that I could not use the density method because test tube 1 had no precipitate). The 2 mL volumetric flask was cleaned and dried and weighed (8.4055g). The mass of pure DMSO was 10.6103g. The mass of the same empty volumetric (after cleaning and drying) was 8.4096g.The mass of the solution was 10.6634g.
12:25- the room temperature bath was 25C. Precipitate was seen in test tube 2. The ice bath was 1C. Precipitate was seen in test tube 4.
12:26- Density of test tube 2 (room temperature) was taken. The 2mL volumetric flask was cleaned, dried and weighed (8.4037g). The mass of pure THF was 10.1708g. The mass of the same 2mL volumetric flask (after cleaning and drying) was 8.4037g. The mass of the solution was 10.3769g.
12:38- the room temperature bath was 24C. Precipitate was seen in test tube 2.
12:40- The ice bath was 1C. Precipitate was seen in test tube 4. No precipitate was seen in test tube 3. The room temperature bath was 24C. Precipitate was seen in test tube 2. No precipitate was seen in test tube 1.
12:45- The ice bath was 1C. Precipitate was seen in test tube 4. No precipitate was seen in test tube 3. The room temperature bath was 24C. Precipitate was seen in test tube 2. No precipitate was seen in test tube 1.
12:50- The density of test tube 2 was taken first in a 2 mL volumetric flask, however, there was not enough solution at that size. A 1 mL volumetric flask was instead used. The empty 1mL volumetric flask, after cleaning and drying, had a mass of 20.4627g. The solution had a mass of 21.4418g. The 1mL volumetric flask, after cleaning and drying, had a mass of 20.4627g. The mass of the pure THF was 21.3394g.
13:10- The density of test tube 4 was taken. The mass of the 1mL volumetric flask, after cleaning and drying, was 20.4631g. The mass of pure THF was 21.3334g. The mass of the empty 1mL volumetric flask, after cleaning and drying, was 20.4632g. The mass of the solution was unobtainable due to the sample being too small.


[Please update the log before any other parts of the experiment JCB]