UNIVERSITY OF WISCONSIN River Falls
Note: Where the instructions tell you to type a command, only type what is within the quote marks, do not type the quote marks.
REFERENCE 13C CARBON SPECTRUM
Follow the initial steps of sample preparation, logging on, locking and shimming, that are used for a routine carbon experiment. Record a routine 13C carbon spectrum. Calibrate it and record the values of sw and sfo1.
RUNNING THE EXPERIMENT
1. Pull down the "File" menu, move to "open" and release on "data set owners".
2. Click on "nmr".
3. Pull down the "file" menu, move to "open" and release on "data sets by name".
4. Click on "DEPT135". Old data may be displayed. Ignore it.
5. Pull down the "file" menu, move to "new" and release. Click in the box after "name" and type in a new name for your sample. Be sure to click in the box after "user" and to type in your owner name. Then click on "save".
6. Type sw and enter the value from your reference carbon spectrum. Do the same for sfo1. If you have not done this earlier with this same sample, type "rga" (return) and wait until the automatic receiver gain adjustment is complete.
7. Type "zg" (return).
8. Type "em" (return) and then type "ft" (return).
9. Click on the up arrow to move the spectrum to the middle of the page. Increase the amplitude as appropriate and then click on "phase".
10. Click on "biggest".
11. Click and hold down the mouse button on "PH0" and roll the mouse up or down as needed. Attempt to get the up peaks completely above the line and the down peaks completely below the line. Ignore the fact that the baseline may be curved. Release when the phasing looks good. Click on "return" and "save and return".
12. Type: "abs" (return) to even out the baseline.
13. Peak-picking, setting the title and plotting are similar to those actions for carbon spectra.
14. Log out in the usual manner. Be sure to leave a sample in the magnet.