See Acquisition and Processing of 1D H-1 Spectra, Acquisition and Processing of 1D C-13 Spectra, and/or More on Shimming lutz and burger if necessary.
Enter
pfgon='nny' su
to make sure the pulsed field gradient amplifier is on. Recheck the shim on Z1 to make sure it is (still) maximized.
Adjust the lock gain so that the lock level is at ~100.
Click the GLIDE button.
Under setup:
Expt: H1 and H1 Detected Experiment
Solvent: Select solvent
Autolock: No
Autoshim: No
Select a title for your experiment.
Click the SETUP button and then wait a second for the acquire button to appear.
Click the ACQUIRE button
Select a ppm range for the ¹H NMR spectrum (which is both axes for NOESY and COSY, one axis for H-C correlation). The H-C correlation ¹³C window is fixed, but can be changed. Select the number of scans (that makes your 1D spectrum look good). The relaxation time should be 1 second. Do not change the pulse angle. For COSY, select the gDQCOSY button. For H-C correlation, select the gHSQC button, for NOESY, select the NOESY button. Click DO and another window should appear. Select the scans per increment and number of increments (If you select 8 scans per increment and 256 increments, a COSY experiment will take 90 minutes. If you select 2 scans per increment and 128 increments a COSY experiment will take 11 minutes. The shorter acquisition time will usually be sufficient. Spectral signal to noise and artifact reduction will be better when the longer acquisition time is used.) Click the OK button. The experiment will start. The 1D spectrum will be printed after it is acquired. The machine will autophase it for you. After the experiment is over, your data will be located in the "vnmrsys/data" folder which can be accessed from the home directory. If the experiment is the first 2D experiment of the day, it will be in the folder with the name of the day. If it is the second, it will have the day and the time as well.
COSY and NOESY processing and plotting:
Enter
jexp1
Find the folder containing your data in the vnmrsys/data folder. Click the proton.fid file then click LOAD, then click PROCESS followed by WEIGHT, TRANSFORM (or type wft). Your processed proton spectrum is located in experiment 1. Enter
jexp2. Click File, then highlight the gDQCOSY.fid file from the open folder and click LOAD, PROCESS, then FULL TRANSFORM. Be patient as the machine works up your data. Your 2D spectrum will appear on the screen. Adjust the contours first by clicking the colors on the bar to the right of the spectrum. Then adjust the contours by using the vs±20% buttons on the top bar. If you so desire, you may zoom in by using the left and right mouse buttons to isolate a square you wish to zoom in on. Click on the EXPAND button. To plot your spectrum, enter
plcosy(10,2,1)
for the either the COSY or NOESY (plcosy is the command to plot 2D homonuclear correlation spectra). 10 is the maximum number of contours, 2 is the spacing between contours and 1 is the experiment where the proton spectrum is located. If
plcosy(10,2)
is typed, the COSY will be plotted but without the 1D spectrum on the axes. If you are using lutz enter
pfgon='nnn' to turn the field gradient amplifier off. Do not do this on burger.
HSQC processing and plotting:
Again, put the 1D ¹H NMR spectrum in experiment 1. If you have separately acquired the 1D ¹³C spectrum that has the same spectrometer frequency and sweep width as was used in the indirect dimension of the HSQC experiment, put the ¹³C spectrum in experiment 2. Work up the HSQC in experiment 3 in the same manner as above for NOESY or COSY. If the spectrometer indicates that the spectrum won't fit on the screen, enter
wc=200
wc2=200
Then replot the spectrum again (you can use the color map button). Use the color bar and the vs±20% buttons to adjust the contours. Enter
plhxcor(10,2,1,2)
where 10 and 2 have to do with the contours and spacing as described above; 1 is the experiment of the proton spectrum, and 2 is the experiment of the carbon spectrum. If you don't have the carbon spectrum acquired, clicking the AUTOPLOT button will plot the HSQC spectrum with the 1D proton spectrum and a ¹³C spectrum which will be extracted from the experiment, which is proton detected.