Note: Where the instructions tell you to type a command, only type what is within the quote marks, do not type the quote marks.
1. Follow the initial steps of initial steps of sample preparation, logging on, locking and shimming, that are used for a routine proton experiment.
2. Be sure that the probe is tuned to 1H and the broad band probe is tuned to 13C.
1H REFERENCE SPECTRUM
3. Run a normal 1D proton spectrum. Examine the spectral width. If desired, reset sw and sfo1 and run again. Write down the name of the data set.
4. When finished, type sw and sfo1 and write down these displayed values.
5. Use the cursor to identify a reference peak and write down the value of this peak.
6. Pull down "output", move to "show-define..." and release on "retain cx".
13C REFERENCE SPECTRUM
7. Run a normal 1D carbon spectrum. Examine the spectral width. If desired, reset sw and sfo1 and run again. Write down the name of the data set.
8. When finished, type sw and sfo1 and write down these displayed values.
9. Use the cursor to identify a reference peak and write down the value of this peak.
10. Pull down "output", move to "show-define..." and release on "retain cx".
RUNNING THE 2D EXPERIMENT
11. Turn the spinner off.
12. Pull down the "File" menu, move to "open" and release on "data set owners". Click on "nmr". Pull down the "file" menu, move to "open" and release on "data sets by name". Click on "HETCOR515". Old data may be displayed. Ignore it.
13. 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".
14. Type "eda" (return). Find SW and click in the box for F2 and enter the sw value for your 13C spectrum.
Click in the box for F1 and enter the sw value for your 1H spectrum.
Click on "save".
15. Type "sfo1". Enter the sfo1 for your 13C spectrum. (return).
16. Type "sfo2". Enter the sfo1 for your 1H spectrum. (return).
17. Type "rga" (return)
18. Type "zg" (return).
PROCESSING
19. Type "xfb" (return). The 2D spectrum will be displayed.
20. Click on "calibrate" and obtain cross hairs on the screen. Move the cross point so that the vertical line lies directly on the reference peak for the 13C spectrum and the horizontal line lies on the reference peak for the 1H spectrum. Click the center mouse button and enter the values for these peaks that you recorded earlier. For F2, enter the 13C reference value, for F1, enter the 1H reference value.
21. Type "edg". Click on "EDPROJ1". Find PF1NAME and enter the name of the 1H dataset that you recorded earlier. Click on "save".
Click on "EDPROJ2". Find PF2NAME and enter the name of the 13C dataset that you recorded earlier. Click on "save" and again on "save" to return.
22. Pull down from "output", move to "define-show..." and release on "current screen limits". Respond to the displayed values with three returns.
23. Type "view" to obtain a preview of the plot.
24. You can type "setti" in order to put a title on the spectrum, but the title may get written on top of the 13C spectrum projection.
LOGGING OUT
Log out in the usual manner.
IMPORTANT: Put a standard sample back into the spinner and release the lift button on the keypad. You may also turn on the spinner. Do not leave the magnet with the lift air on and no sample in.
Created by: d.b.rusterholz@uwrf.edu