Log in, log out, and parameter set up

Log in to lutz by entering your advisers’ last name (all lower case letters) at the user name prompt followed by a return. The password prompt will appear. Enter your password, these are the same as for the other NMR spectrometers, followed by a return. See an experienced NMR user in your lab or Jeff Ellena to obtain your password.

Move the cursor to the Main Menu button and click.

Click on the following buttons or text in order:
File
stds/  (after clicking the background will become blue)
Set Directory
Data
stdh1.fid/
Load Shims
 
Enter su followed by a return.
Wait for the Setup Complete message and beep.

Click on:
File
stdh1.fid/
Load

Enter su followed by a return.
Wait for the Setup complete message and beep.

When you wish to log out, move the cursor to the desktop background, hold down the right mouse button, drag to Log out... and release the mouse button.

Sample changing and locking

Activate the Acquisition window by clicking on it to bring it to the front.

Click on:
Connect
eject

Remove the standard sample and spinner from the magnet. Remove the standard sample from the spinner and make sure that the standard sample, the spinner, and your tube are clean. A gold colored cylinder is used for positioning a NMR tube in the spinner. Insert the small diameter end of the spinner into the gold cylinder as far as possible. Insert your tube into the spinner until the bottom of your tube meets the floor of the gold cylinder. Put the spinner and tube in the magnet and then click on:
insert
LOCK

Look at the words beneath the yellow line. If
SPIN OFF
appears, click
SPIN:on
If LOCKED appears, go to the next section on shimming the magnet.
If NOT LOCKED appears, click
LOCK: off
LOCK OFF will appear below the yellow line.
Set lockpower near 30
Set lockgain between 30 and 48
Set spin to 20
Adjust Z0 so that the yellow line has a non-zero amplitude and is flat. For a more complete description of locking see Optimizing System Lock in VNMR Basic Operation.
The proper setting for Z0 depends on the lock solvent.
Solvent      Z0
CDCL3      47
C6D6         16
Acetone    268
CD3CN    286

Click LOCK:on and LOCKED should appear the yellow line.

Shimming

Click SHIM
Click SHIM:manual  near the top of the screen and then
click on the triangle to the right of SHIM:  until fine z appears. Adjust Z1, Z2, Z3 for maximum lock level. Shims are adjusted by moving the cursor to one of the numbers to the right of the right of the shim name and clicking the left or right mouse button to decrease or increase respectively the shim DAC value by the number near the cursor. If the lock level reaches 100, move the cursor to the bottom of the window and decrease the lock gain. When you have finished shimming click on Disconnect.

Parameter adjustment and data acquisition

The acquistion parameters appear in the lower NMR window. If this window is partially hidden, click on Flip once or twice to see the entire window. nt is the number of scans that will be collected. d1 is the time (in seconds) between scans. If you wish to change parameters, put the cursor in the command window (near the top of the screen) and click any mouse button, then enter the parameter name followed by = and the new value for the parameter (ie. nt=4).
Click on the upper VNMR window and enter go followed by a return to collect a FID. The number of scans completed can be viewed in the Acquisition Status window. The words Acquisition complete will appear in the upper VNMR window when nt scans have been collected and stored in a temporary location.

Data storage and processing

After collecting your FID click on the following to save and process the FID.
Main Menu
File
Data
Save FID
Main Menu
Process
Weight, Transform
Enter aph for autophase. If further phase adjustment is necessary, click on Phase.
Move the cursor to the middle of a peak on one side of the spectrum, hold down the left mouse button and drag the mouse vertically to adjust the phase about the position where the cursor was located. If you wish to make fine phase adjustments, hold down the right mouse button and move the mouse. When the phase near the initial cursor position is set properly, move the cursor to a peak on the opposite side of the spectrum, hold down the left (for coarse adjustment) or right (for fine adjustment) mouse button, and drag the mouse to make phase changes. When you have completed phase adjustments, click on Phase to exit phase adjustment.
 
Zooming and chemical shift referencing

To zoom on a peak, click on:
Main Menu
Display
Interactive
Then move the cursor to the left zoom boundary and click the left mouse button. Move the cursor to the right zoom boundary and click the right mouse button. Click on Expand to view only the zoom region.
Spectral referencing is done by completing the following. Zoom on a peak that has a known chemical shift. Position the cursor in the middle of the peak with the mouse. Click on Ref. Enter the chemical shift of the peak followed by a return.

Integration

Adjust the intensity of the spectrum so that the tallest peak of interest fills the vertical dimension of the window. This is done by putting the cursor on a peak, holding down the middle mouse button and dragging the mouse to change peak amplitude. Also zoom to display the spectral width of interest as described in F.
Click on:
Return
Massage
Region
Return
Massage
BC
Return
Massage
Adj IS
Return

To see a list of integrals on the screen click on:
More
Integrals

To add integrals:
Put the cursor on the left edge of the desired region. Enter z. Put the cursor on the right edge. Enter z.

To set the value of an integral and view integral values near the spectrum:
Click on:
Main Menu
Display
Interactive.
Put the cursor inside an integral. Click Set Int. Enter a value for the integral followed by return. Enter dpir return to display the integral values below peaks.
 
Peak picking

Click on:
Main Menu
Display
Interactive
Th.
Hold down the left mouse button and drag the mouse to position the horizontal yellow line so that it is slightly lower than the lowest amplitude peak of interest. Click on Th again to exit threshold adjustment. Click on:
Main Menu
Display
Plot
Peaks
Enter dpf return to see the peak positions displayed above the peaks.
Enter axis? return to see current axis units.
To set axis units enter:
axis=h return for hertz
axis=p return for ppm

Plotting

Click on:
Main Menu
Display
Plot (to plot spectrum and integral if present)
Scale (to plot the frequency axis)
Peaks (to plot peak positions after doing peak picking)
Page (to send perviously selected plot commands to the printer)
If, after integration, you would like to plot the spectrum, integral, axis, and integral values, enter:
pl pscale pir page return