Exp272

= = =Researcher= Mark Mangir =Objective= To test the solubility of n-[(e)-(4-chlorophenyl)methylene]aniline in ethanol, acetonitrile, benzene, hexane, and THF by the SAMS NMR method. =Procedure= =Results= [|SAMS Sheet] =Conclusion=

=Log=

2012-03-16
13:04 Added about 0.072g of solute to 1 dram screw cap vial. (Vial 1) 13:08 Added about 0.079g of solute to a second screw top vial. (Vial 2) 13:12 Added about 0.075g of solute to a third screw top vial. (Vial 3) 13:16 Added about 0.070g of solute to a fourth screw top vial. (Vial 4) 13:20 Added about 0.076g of solute to a fifth screw top vial. (Vial 5) 13:24 Added 40 drops of ethanol to Vial 1. Crystals were still visible. 13:25 Added 40 drops of Acetonitrile to Vial 2- all went in 13:26 Added 0.056g of solute to vial 2. Crystals were visible. 13:28 Added 15 drops of Benzene to Vial 3- all went in 13:29 Added 0.045g of solute to vial 3. Crystals were visible. 13:31 Added 40 drops of hexane to Vial 4. Crystals were still visible. 13:32 Added 10 drops of THF to Vial 5- all went in 13:33 Added 0.020g of solute to vial 5. Crystals were visible. 13:40 Parafilmed each vial and placed them in a 50C water bath. 13:55 Removed all the vials. No precipitate was visible in any of them.

2012-04-09
12:30 Checked vials after spring break. Vials 2,3, and 5 had dried out. Vials 1+4 had solvent and visible crystals. 12:32 Added 30 drops of acetonitrile to vial 2, crystals were still visible. 12:35 Added 10 drops of Benzene to vial 3. Crystals were still visible. 12:38 Added 10 drops of THF to vial 5, no crystals were visible so added 0.064g of imine to the vial, and crystals were visible again. 12:40 started heating water bath. 12:55 Placed all the vials in the water bath at 47.5C. 13:10 Took all vials out of the water bath, at 53C. Let sit on counter to cool. 13:40 Prpeared NMR samples by taking 200uL of each sample and putting it into an NMR tube. Sample 2 solidified upon addition. 13:45 Added 1mL of CDCl3 to each tube. 13:50 Went to take an NMR, but the machine was under maintanence.

2012-04-16
13:00 Took NMR of samples 1-3, but the NMR computer stopped receiving signal from the instrument during my 4th sample, so the last to samples were aborted. The files were mim_imine_ONSEXP_1_Acetonitrile.dx, and mim_imine_ONSEXP_1_Benzene.dx.

2012-04-23
13:20 Took an NMR of sample 5, sample 4 was never returned after the NMR was fixed. It was named mim_imine_ONSEXP_1_THF.dx.