Previous - 5.1 General approach (ANALYSIS)

 

5.2 NMR

5.2.1 Overview (Theoretics)

5.2.2 Preparing Sample

1. Take your sample from the frige and let it stay at room temperature for a few minutes.
2. Get a NMR tube and be sure that the opening end of the tube is not broken, because it should be plane in order not to damage the tube or the NMR machine. Label it with your sample name identification and with the number of tubes of the column chromatography fraction that the NMR you're about to realize represents (e.g. JR02F20_23).
3. Retrieve from the sample about 3 mg of your product with a spatule into a small tube.
4. Dissolve the product in 0.8 ml of deuterated solvent (e.g. Chloroform) from the dispenser, to dissolve completely all the organic compounds of your product.
5. With the pipette improve the dissolution even further.
6. After filling the NMR tube, the ideal height should be about 98 milimeters and now we have finished preparing our sample.

 

5.2.3 Running Sample

1. Then you have to go on the bottom floor to the room of the Nuclear Magnetic Ressonance. Here, you need a card to get inside and read thoroughly the warning instructions/precautions, to avoid any possible accident.
2. When you get to the computer, you should pass the card again on the device, in order to update the user.
3. The "Current Status" board, points out the available location (in this case number 9) to insert the tube in the NMR machine.
4. Place the NMR tube inside the spiner (greenish object) and with the measurer, you can know the perfect location (in terms of depth) of the tube inside the NMR, this should be done very carefully.
5. Then insert the tube (with the spinner) inside the NMR machine on the right location.
6. In "Eaddr", you should insert your email and also update the "Sample Name" and SAVE.
7. Don't forget to check the "Autoplot" box to automatically print.
8. Select "PROTON" (in this case for 1H NMR).

9. Double-click the new left bottom line that appeared and change the following configurations:

"Spectral Width": -1.0 to 11.0 ppm

"Number of scans": 16

And click "SAVE" button to update the new info and then "SUBMIT".

11. Don't forget to write in the register your use of the machine.
12. And finally, click "QUIT SESSION" when the NMR has ended, as you can see from the info in the screen, all the tubes appear as green (finished) otherwise it would be blue (if not finished).

 

Next- 5.3 Mass Spectrometry