Exp219

=Researcher= Mark Mangir =Objective= To test the solubility of trans-cinnamic acid in ethanol and methanol by the SAMS NMR method. =Procedure= =Results= =Conclusion= Experiment aborted due to NMR problems. =Log=

2011-09-30
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]**

2011-10-03
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.

2011-10-14
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.