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list of experiments
Solubility book (3rd Edn)
This experiment had been aborted/postponed. The samples that were left to equilibrate were lost. Therefore, the experiment needs to be restarted.
To ascertain the solubility of
by NMR spectroscopy.
Saturated solutions of 2-phenylbutyric acid were prepared in
DMSO, THF, and toluene. The solutions were prepared by mixing together the solute and 200
of the solvent
into a vial. With each subsequent addition of solute, there were bouts of vortexing. Once the solutions showed an excess of solute, the vials were sonicated, using a Branson 1510 instrument, for 30 minutes.
Solutions were then left to equilibriate. 100
of the supernatants were micropipetted out and then dissolved into NMR tubes containing 900
deuterated chloroform (CDCl3)
. Proton NMR readings of the solutions are obtained with the use of a 500MHz instrument.
17:10 Ambient temperature in the lab was observed to be 26°C.
17:15 Made a solution
[You didn't based on your later comments JCB]
of 2-phenylbutyric acid by adding the solute to 200
μL of DMSO solvent in a vial labeled "DMSO". Vortexed the vial briefly inbetween the additions of solute until solute was visibly seen collecting at the bottom of the vial.
17:22 A solution of 2-phenylbutyric acid in THF was made by adding the solute to 200μL of THF in a vial labeled "THF". The vial was vortexed briefly inbetween additions of solute till solute was seen to collect at the bottom of the vial.
Made a solution of 2-phenylbutyric acid by adding the solute to 200
μL of toluene solvent in a vial labeled "Toluene". Vortexed the vial briefly inbetween the additions of solute until solute was visibly seen collecting at the bottom of the vial was reached.
[You didn't reach saturation - nor could you tell at this point - based on your later comments JCB]
17:35 Sonicated all 3 vials of solutions for 30 minutes.
[Don't record what you plan to do but rather what you did - 17:35 Added vials to sonicator - record temperature of bath; 18:05 removed vials from sonicator - record temperature JCB]
18:11 After the sonication, it was observed that all collected solute had gone into solution in each vial. Therefore, more solute was added to
all vials. Volume of the solution in each vial was seen to greatly increase.
18:18 Sonicated all vials for another 30 minutes.
18:48 Vials were left to equilibriate.
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