Solutions to Problems

RESET communication between computer and console

Reset communication between computer and nmr console. Symptoms that indicate the need to reset communication:

1. "STATUS Inactive" - In the upper left corner of the ACQUISITION STATUS window (usually in the upper right corner of the screen).

2. "acquisition in progress" error message after typing "su", "ga", or "go". First abort all acquisitions with "aa"; then repeat command (e.g. "ga"). If error message persists then reset communication..

3. "acquisition interface is locked by "xxxxx"" message when you type "su" or "ga". The previous user "xxxxx" left an active acquisition when they logged out. Reset of communication is necessary to regain control of the nmr console.

Procedure for resetting communication.

1. Exit from nmr program. Type: exit

2. Open Unix TERMINAL window, click with right mouse button over background, scroll down to PROGRAMS, then scroll down to TERMINAL.

3. In terminal window type: su acqproc you should see the response "CLOSING EXPPROC"

4. Go to the nmr console and press the red reset button. On Unity Inova 400 and 500 open left door. The reset button is on the left edge halfway down above the ethernet transceiver. On Mercury 300 open Plexiglas door. The reset button is on the right side halfway down.

5. Wait 45 seconds - then type: su acqproc you should see the response "STARTING EXPPROC"

6. Restart VNMR program.

7. Occasionally you may need to repeat this procedure a second time (and even a third time), until the symptom disappears.




Some Experimental Handouts

NOESY1D a 1d NOE difference experiment for the INOVA consoles

NOESY1D ##A 1d NOE difference experiment for use on the Inova 400 and 500 consoles##

Begin by acquiring in experiment 1 a proton spectrum for your compound. N.B. Phase the spectrum well.

Turn off the spinner and make sure the lock level with the spinner off is > 70.

a.) [probe?] Check the value of "probe". It should be 'quad' on the 400, or 'id' on the 500. If incorrect, set value (e.g. [probe='quad'].

b.) [pfgon='nny'] Set the value of "pfgon".

c.) [jexp2] Join experiment 2. (If you don't have an experiment 2, create it. Click on the menu button "Workspace", then click on "Create New", finally click "Exp 2".)

{CHORUS}

1.) [mf(1,2)] Copy the control spectrum from experiment 1 to experiment 2,

2.) [wft] and process the spectrum.

3.) Expand around the peak that you want to irradiate.

4.) [NOESY1D] Wait for the NOESY1D macro to finish (several seconds).

5.) Place the cursors around the peak to irradiate. If the expected NOE is with a nearby peak, place the cursors as close to the irradiated peak as possible.

6.) Click on the menu button "select"

7.) Click on the menu button "Proceed".
7a.) [nt=##] If you have a low sample concentration change the number of transients to collect.
7b.) [time} Shows how long the experiment will run.

8.) [ga] Begin the acquisition and displays the resulting spectrum. The lock level should start bouncing up and down if the experiment is working. Check with the staff if problem.
8a.) [text] Enter description of experiment.
8b.) [svf] Save the data to a file.

9.) Plot the spectrum as desired.

10.) Repeat the CHORUS as needed to irradiate additional peaks.

{INTERPRETATION}
If the phasing was done correctly at the beginning the irradiated peak should be the large upside down signal. Then, any upright signals represent NOEs to the corresponding peaks. Dispersive signals indicate a peak with strong coupling to the irradiated peak, which virtually always is an indication of a strong NOE.


 


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