(IV) General procedure to run NMR experiments
A. Step-by-step instruction on running experiments on AV-400
- Click “Change user” and login to IconNMR with your username and password.
- Identify an empty sample holder in the IconNMR menu and make sure this position is also available in the autosampler. Insert your sample into the blue spinner.
- Press “Add” then “Go to position” on the autosampler control panel, put your sample into your desired holder.
- In the IconNMR menu, double-click on your sample holder to add an experiment. You can select your experiment type, solvent and set a title here.
- If desired, hit the equals button to edit standard acquisition parameters including number of scans, spectral width, acquisition time, offset frequency, etc.
- If you would like to also collect another experiment on this sample, you can highlight the current experiment and then hit the Add button. Another experiment will appear below with an empty experiment type. Select the appropriate experiment and edit acquisition parameters if necessary.
- Highlight the appropriate holder directory, and hit the Submit icon.
- After all your experiments are finished, press “Remove” then “Go to position” on the autosampler control panel and take your sample out. Login to IconNMR again, select your finished holder and hit delete. This will make this position available again.
B. Step-by-step instruction on running experiments on UI-500
- Login and open VNMRJ software by left double click the VNMRJ icon on the screen. Click “Eject” and put your sample on the top of the magnet, and click “Insert”.
- Click the “New study” button (left bottom corner of the screen) below “Study Queue”. Then double-click the experiment you’d like to run (for example, “PROTON” in the “Common” family) in the “Experiment Selection Tree” window.
- Choose your solvent. Type your sample name in the “Sample name” field. This name is not your file name. It is not important and for your reference only.
- Below “New study”, a “Submit” button will show up after you set up your experiments. To the right of the “submit” button, make sure it is “Foreground”. If you see “Background”, change it to “Foreground”.
- If you want to change some parameters for your experiment, double-click on your selected experiment (for example, “PROTON”) and make changes under “Acquire”.
- Click “Submit” to start your experiments. Wait for a couple of minutes for the experiment to finish. You will see “DONE” on the screen when it finishes. Type “wft” if you want to see the spectrum now.
- Save your data in your desired folder now by clicking “File” then “Save as” at top left. Please remember no spaces or other special characters allowed in your file name. But underscore and dash (- and _ ) are OK.
- After everything is done, eject your sample and insert again, then close VNMRJ.
- To logout, click on your login name at top-right and choose “Quit”, then select “Logout”.
– WARNING –
You need to be very careful when you insert your sample. This is the moment when you can do great damage to the spectrometer, so pay attention!!! The sample is ejected and inserted slowly by compressed air from the upper barrel of the magnet. You should be able to hear a loud sound of air pressure when the sample is in “eject” position. Gently put your sample on the air cushion at the top of the magnet. DO NOT let go of the sample until you feel the air cushion is supporting it. Once the sample is resting on the air cushion, deactivate the eject air (“insert”) and the sample will gradually descend into the magnet. Never insert a spinner without a sample tube. Make sure your tube is not cracked, damaged or leaking before introducing it into the magnet. Any carelessness at this moment (for example, letting the sample go without the supporting air) will cause the sample to crash in the magnet and lead to thousands of dollars of damage.
C. Run long carbon and any other more complicated experiments on 500
Now you’ve finished your first 1D proton on 500. Your sample has been shimmed and locked. You are ready to run (other) longer experiments manually. Please DO NOT click “New Study” and “submit” again to run your second experiment on this sample, because you do not need to shim and lock again. Just select the experiment you like to run from the top “Experiments” menu, change the parameters if you want to, and type “go” to start. I recommend using this way to run your long carbon experiments (rather than clicking “new study” and “submit” a long carbon), since you won’t waste a lot time in cases when the shimming and locking procedures fail.
D. Some Useful Commands on 500
The following are some of the common commands you can type in the command window. Please note all commands are followed by the “enter” key.
- e: eject
- i: insert
- go: start acquisition
- aa: abort acquisition
- wft: Fourier transformation with window function
- ga: = go + wft, start acquisition and process data automatically after acquisition
- aph: automatic phasing
- time: show experiment time
- fixit: load a saved shim file. If you have problems to shim, use this home-made macro to load a good shim file to start.
- jexp1, jexp2…: join experiment #1, #2, etc. If you wish to open two or more data files at the same time, use this command to switch between different spectra. {Note: “experiments” are like different “windows”; each has its own data set in it}