Instructions for Using 300 MHz NMR

ICON-NMR

Susan J. Kohler

June 1, 1998

Modified Sept. 22, 1998

Modified August 24, 2004

How to Reserve Time: There is a daily schedule in the NMR room. If you come in and time is free, just sign up on the daily schedule and use it.

How to Use the Spectrometer:

General Comment: All mouse clicks are done with the Left Mouse Button unless otherwise specified.

First, please sign the log book so we can keep track of how the instrument is being used. This is necessary for bookkeeping for the funding agencies. They like to know things like how many students use the spectrometer per month, etc.

To log on, click on the appropriate user icon and hit Return, or type your user name in the box and hit Return. Enter the password followed by Return. If it gets rejected, make sure Caps Lock is not on! Wait for the big green screen to appear. This takes a little while.

Normally your data will be saved on the hard drive ("u" drive) and you will not need to use the zip drive. But if you are using the zip drive, insert your cartridge in the drive. If a previous user has left a cartridge in the drive, you can eject it by clicking on the Zip icon on the screen with the Left Mouse Button (icon will get yellow highlights), then clicking with the Right Mouse Button to get a menu, and choosing Eject Zip.

Click on the Routine Spectroscopy icon. Then click on the Identify User icon. Choose the appropriate user name with the mouse (it will underline the choice) and click on it. Enter the password again.

Now follow the flow chart.

• Click on Insert/Eject. REMOVE THE COVER ON THE MAGNET BORE, then choose Insert Sample from the box on the screen. Leave the cap off until you are finished for the session. You don’t need to have it in place when you are doing a series of samples. The current sample will slowly and quietly float to the top of the magnet. Remove it, insert the new sample in the holder, check the positioning with the depth gauge, and insert the sample. Click on the Okay button in the Insert Sample dialog box. The sample will go down.

• Click on Filename. Enter a file name. Start the name with your initials. Only use letters, numbers, dashes and underscores. Do not use any other characters or spaces. If you see a choice, choose drive u for normal work and zip if you need to use the zip drive. The experiment number will default to 10, which is a fine place to start. It will get automatically incremented with each spectrum. Then click Okay.

• Click on Set Solvent, then choose the proper solvent from the list with the mouse. Click Okay.

• Click on Set Experiment, and then choose the specific experiment you want to run. Then click Okay. You must then click on Set Plot Title. A new window will pop up and allow you to enter a title which will appear on your plots. Enter a title, then click Save.

• (OPTIONAL) If you need to change any of the acquisition parameters (like number of scans, NS) you may click the Parameters heading. If you hold down the left mouse button when you click, you will get a menu of parameter classes. Choose the appropriate class (i.e. Edit Acquisition Parameters) and then edit the necessary parameters. Click Save (effective for ONLY the current spectrum) and return.

• Click on Start. Watch the flashing icons to see the progress of the experiment. If the Lock window is not open, click on the Lock button to open the window so that you can confirm that the spectrometer is properly locked. If you want to, after Acquire Data starts you can click on the FID button to watch the acquisition. Wait a couple of seconds before you do this, since it hangs up if you start too soon. You can adjust the vertical scale with the *2 and /2 buttons.

After the plots are done, choose EXIT and you will be ready for the next sample. If you need another spectrum of the same sample, you will see that there is a choice to use the same sample rather than Inject a new one.

When you are finished with your experiments, please put s sample back in the magnet.

When you are all done , go the File menu at the top of the screen and choose Exit to Icon NMR. Then choose Exit to Unix from the IconNMR File menu. Eject your cartridge by clicking on the Zip icon on the screen with the Left Mouse Button (icon will get yellow highlights), then clicking with the Right Mouse Button to get a menu, and choosing Eject Zip. Finally log out by pressing the Right Mouse Button to get a menu, and choosing the Logout option. You will be asked to confirm your choice.

Finally, put the cap back on the magnet bore.

How to Use XWINPLOT for Pretty Plots: You can start XWINPLOT by opening a window (usually by clicking on a window icon at the bottom of the screen) and typing xwinplot at the %prompt sign. You use the Data button to identify the data sets you want to work with, and the buttons on the left to compose your plots (I will give you more help in person). When you want to go back to ICONNMR, you can make the plot window small by clicking on the little dot in the upper right corner of the window. This will make it into an icon in the window at the bottom of the page. To reopen it later, just double click on the icon.