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Solubility book (3rd Edn)
To test the solubility of n-[(e)-(4-chlorophenyl)methylene]aniline in ethanol, acetonitrile, benzene, hexane, and THF by the SAMS NMR method.
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.
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.
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.
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.
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