Department of Chemistry NMR Facility
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Acquiring a Spectrum Using ICON-NMR
Correct Login Procedure and Restarting Information---On the Bruker 300: Make sure XWIN is running under the user called advanced. Look at the top bar and you should see the words "started by Advanced" If you do see these words Exit out of the program and go to the blue UNIX window. Type login advanced and the return. Enter the password for advanced. At the prompt type xwinnmr. In the pink text field type iconnmr and then login into icon with your account.
On the Bruker 500: See these specific directions
Signing Up for Use---In the orange notebook near the workstation sign the login/logout sheet. This system is used so the previous user can reach you when they are finished. Limit your experiment to 15 minutes. Experiments requiring more time need to run after 5:00pm or scheduled with the NMR Lab Manager. There are after hours scheduling sheets in the back of the orange notebook.
STARTING ICON-NMR---If only XWIN-NMR is open type iconnmr in the pink text field (there is a menu option under Window in the main menu if you prefer menus). If only the desktop is displayed then follow this sequence:
1) Open a shell by going to the Tool Chest on the desktop and choosing Desktop-->Open UNIX Shell.You will be prompted by icons during this process.
2) At the prompt type in xwinnmr
3) In the command line of xwinnmr type iconnmr1. ROUTINE SPECTROSCOPY---Obtain a login ID and password from the NMR Lab Manager. Click on Routine Spectroscopy and scroll down to your login ID and double click. nEXT, Enter your password and press enter.
2. INJECT/EJECT---Three important reminders for this operation:
The first window you are presented with allows you to eject the sample currently in the machine and allows you to insert your sample. Click on Insert New Sample and wait till you hear air escaping from the top of the magnet. Remove the tube and spinner assembly that is lifted up and replace with your tube and spinner assembly. Fist you must insert your sample into the spinner and set the correct height using the depth gauge on the cabinet above the sample preparation area. Clean your tube and spinner with a Kimwipe and insert into the magnet. There are pictures detailing this process in the lab. Once your sample is being held at the top of the magnet by air click OK in the pop up window.THERE IS A HIGH POTENTIAL FOR DAMAGING THE NMR IN THIS PROCEDURE SO YOU MUST SEEK TRAINING FROM AN AUTHORIZED USER BEFORE INSERTING YOU SAMPLE INTO THE MAGNET. NEVER TOUCH THE TUBE AND SPINNER WITH BARE FINGERS. MAKE SURE THE YOU HEAR AIR COMING FROM THE MAGNET BEFORE YOU INSERT YOUR SAMPLE. 3. EXPERIMENT---Click on the Data Set Filename icon. Type in or choose from the pull down menu a file name then click OK
4. SET SOLVENT---Choose you solvent from the list and click OK.
5. SET EXPERIMENT---Choose the experiment you wish to execute. A normal proton is named PROTON. See the NMR lab manager or someone with experience if you wish to try a new a different sequence. You can enter a plot title here if you wish.
Before starting you can investigate the acquisition and processing parameters. Go to the Parameters menu option and choose which parameters you wish to edit. A few acquisition parameters that are routinely changed are:a. NS – number of scans. Typically:
PROTON 16b. SW – size of window in ppm
COSY90 1 to 4
C13CPD 1k to 20k depending upon probe and concentration
C13APT 1k to 20k depending upon probe and concentrationPROTON to encompass all peaks of interest (sw = max ppm - min ppm)c. TD – number of points the FID is sample with.
COSY90 The F1 and F2 columns need to be identical to the value used in the 1D proton experiment.
C13CPD 250
C13APT 250PROTON 64k for a 20 ppm window and 32k for a 10ppm windowd. O1P or O2P – center of SW in ppm
COSY90 The F1 column needs to be 2K The F2 column need to be 128, 256 or 512 depending upon desired resolution.
C13CPD use default
C13APT use defaultPROTON calculate using o1p = sw/2 + min ppm. sw determined by: sw = max ppm - min ppme. If TD is changed for any experiment then the processing parameter SI needs to be set to ½ of the TD value.
COSY90 The O1P needs to be identical to the value used in the proton experiment
C13CPD 110
C13APT 110You can also choose Show approximate experiment time to see what effects your changes made.
6. START---Click on start to initiate the experiment.7. PROCESSING---To look at the spectra in detail in XWIN-NMR go to File-->Exit ICON-NMR then File-->XWIN-NMR. To process go to step 11 in the XWIN-NMR instructions.
8. EJECTING SAMPLE---The easiest way to eject your sample is to open XWIN-NMR by the steps outlined in step 7 and type ej to eject you sample and type ij to insert the standard sample. If you are running another sample then just type ej and remove your sample and then type ij and insert NO sample. Your sample will be inserted in step 2 above.