HETCOR Instructions

Typical aquisition time = 2 hours 30 minutes

This routine takes over two hours, so it should only be used when no other users will be using the instrument (early morning or late afternoon).

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. If you wish to change the scale, reset sw and sfo1 (the spectral width and center frequency of the spectrum) using the sw-sfo1 button and run again. Write down the name of the data set. The resulting file should be saved in your directory on the D: disk.

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. Select Output --> show-define --> retain CX.

13C REFERENCE SPECTRUM

7. Run a normal 1D 13C spectrum. If you wish to change the scale, reset sw and sfo1 (the spectral width and center frequency of the spectrum) using the sw-sfo1 button and run again. Write down the name of the data set. The resulting file should be saved in your directory on the D: disk.

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. This reference peak should be one you expect to be bonded to a proton; a 13C in a methyl group (large 1H signal) would be ideal.

10. Select Output --> show-define --> retain CX.

RUNNING THE 2D EXPERIMENT

11. Turn the spinner off.

12. Select File --> New and open a new file in your directory.

13. At the command line type "rpar hetcor". This will load standard HETCOR parameters.

14. Type "eda" (Edit Acquisition). 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" (edit graphics). Click on "EDPROJ1"(Edit Projection 1). Find PF1NAME and enter the name of the 1H dataset that you recorded earlier. Be sure that the data set owner and disk unit (D:) are set correctly. Click on "save".

Click on "EDPROJ2"(Edit Projection 2). Find PF2NAME and enter the name of the 13C dataset that you recorded earlier. Be sure that the data set owner and disk unit (D:) are set correctly. Click on "save" and again on "save" to return.

22. Select Output --> define-show --> 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.