Exp265

=media type="custom" key="9944241"= =Researcher= Evan Curtin =Objective= To determine the melting point of benzylamine to clarify [|inconsistent data] =Procedure= A sample of benzylamine is sealed in a screw-cap half-dram vial with parafilm then cooled in an acetone bath with dry ice. =Results=

NMR 1
media type="custom" key="9539656" =Discussion= The sample did not solidify even at -78 C. This is likely due to the impurity of the sample from the H NMR, estimated at only about 84% based on the integration of peaks at 3.8 and 4.8 ppm. Judging from the peaks at 4.84, 7.81 and 8.39 the impurity has an aromatic ring with a benzylic carbon. The impurity is more than likely a derivative of benzylamine, but the exact identity is not clear. **[What is the impurity? How did it get there? AL]** =Conclusion= The measurement of the freezing point of benzylamine must be redone with a sample of much higher purity. =Log= 10:57 - Added benzylamine to 1/2 dram screw cap vial, sealed with parafilm. Made a bath of acetone in a 250mL beaker. Added some dry ice to the bath. 11:02 - Bath temperature is -13C, added sample. 11:22 - Sample is still liquid, added more dry ice to cool further. Cooled to -30C **[What is the limit to how low your thermometer can measure? AL][The thermometer can measure to -100C - EC]** 11:32 - Added excess dry ice to the acetone. Solid pieces of dry ice were in the liquid. The sample did not freeze, but became viscous. 11:40 - Took pic1 showing the sample still liquid at -78C 11:40 - Prepared solution of benzylamine and CDCl3 11:45 - Took HNMR-1 of benzylamine using 500MHz varian NMR.