Mark Mangir


To test the solubility of trans-cinnamic acid in ethanol and methanol by the SAMS NMR method.




Experiment aborted due to NMR problems.



3:04 Added about 1mL of methanol to 1 dram screw cap vial. (Vial 1)
3:05 Added about 1mL of ethanol to a second screw top vial. (Vial 2)
3:09 Weighted 388 mg of Cinnamic acid (TCA) (99+%, Aldrich) on weigh paper.
3:12 Added TCA to vial with methanol (Vial 1)
3:15 Weighed 377 mg of TCA on weigh paper.
3:18 Added second sample of TCA to vial containing ethanol (Vial 2)
3:20 Added 2400mL of water to roto-vap water bath.
3:22 Took 2 40mL beakers, added water to the 40mL mark and placed them in in the water bath.
3:27 Placed each vial in one beaker after parafilming them.
3:28 Turned heat up on roto-vap bath to 45C.
3:33 While heating vials, prepared vials to decant into.
3:40 Since bath did not heat, plavced vial 1 in 41C tap water.
3:42 Placed sample 2 in same beaker.
3:45 Temp of bath decreased to 37C.
3:47 Temp decreased to 35C.
3:50 Temp at 34C- removed vial 1.
3:52 Temp at 33.5C- removed vial 2.
[You should have decanted supernatant at this point JCB]


Room Temperature was 18.5C.
12:15 Checked samples for precipitate.
-ethanol had precipitate, methanol did not.[because you did not decant supernatant day before while hot you cannot be sure you reached saturation JCB]
12:15 Blew small amount of vial 1 with air, precipitate quickly formed.
12:17 Cleaned NMR tubes.
12:22 Added an equal amount of Duterated Chloroform to each vial.[You should have decanted supernatant at this point also before adding CDCl3 JCB]
12:25 Used glass Pipette to decant solutions 1 and 2.
12:30 Transferred each solution into NMR tubes.
12:40 Both NMR were busy, will remake the samples and run them another day.


Room Temp was 21C
12:15 Checked Samples for precipitate, ethanol had some, methanol did not.
12:15 Blew the methanol with a small amount of air, and precipitate quickly formed.
12:16 Decanted both solutions.
12:17 Cleaned NMR tubes.
12:25 Used a glass pipette to transfer the solutions to the tubes.
12:30 Tried to take an NMR of the Samples, but the instrument kept producing errors.