Short Instructions for basic operation
                          of nmr500-3 spectrometer.

*   Take out the plastic cap of the top of the sample insertion port.
*   Put your sample into the spinner turbine. Make sure that NMR tube is clean and  
     dry. Do not touch the turbine’s shaft by fingers. Use the insert gauge to find out  
     the proper sample depth. To achieve a good shimming, the length of a sample
     should be larger than the length of corresponding coil. We are using 5mm coils on
     all spectrometers.
*   Log into your account on spectrometer’s workstation.
     Double click on "Topspin"  icon. You may also open  the Linux  shell window
    “Red Hat->System Tools->Terminal” and type in command line “topspin”.
    Click the "BSMS" icon on upper “Top Spin” menu or type in command line   “bsmsdisp”.
     The bsms interface will appear. Click the  “Lift ” button. After you
     hear whistling gas coming from the top of the magnet and checked the flow of gas
     with hand place sample on air cushion and push the “Lift"  button again. The
     sample will descend softly into the NMR  magnet.
*   After you seen the green  “sample down” light lit, press “Spin”  button.
     The  light will be read till the sample is at the set speed and will turn green.
*  In the Top Spin under file menu select “New”
     Make sure that under “user” in this menu is your login name and under “DIR” is
     /opt/topspin. Put the file name, experiment # and processing data # and click “OK”
     button.
     At the prompt at the bottom of the “Tops Spin”,  type “rpar” and choose the
     /opt/topspin/exp/stan/nmr/par/user
    For a proton experiment select “stdh1.QNP ”, and choose all option click
    “Read” and “OK” in the   in the next window. Click “Close” as the next.  For any other nucleus
    select appropriate one.
* At the prompt, type “rsh” and select the default shims. nmr500-3 is
   equipped with quattro nucleus probe and the default shims files has extension
   “QNP”   default.QNP. If different probe is installed the message will be posted.
   If there is no “lockdisplay” on the screen, at the prompt type “lockdisp”
   or choose proper icon from the “Top Spin” menu and        resize it according to your needs.
* At the prompt type “lock” and select your solvent from the list provided.
   Perform the magnet shimming.
   Click BSMS icon.
* Select “Z” on the keypad, and change it value to maximize the signal
   Select “Z2”, and repeat maximization. Normally, you do not need to shim higher orders.
   Repeat above steps until the signal is maximized.
   You may also try automatic shimming instead, by typing “topshim gui”. After shimming showed
   “finished” message close the menu. Come back to bsms menu
* Select “lockgain”, adjust until the signal is within second line from the top.
* If the lock signal becomes saturated lower the lock power. Most often the good
   working lock power can be found in the range of –25 to –35 DB.
* If the lock fluctuates decrease the lock power until is stable.
   Select “Standby”
   At the prompt type “atma” and wait for the message “atma finished” Do not type any other
    command except “stop” while “atma” is in progress. This might results in freezing spectrometer.
* At the prompt, type “rga”, wait for the message “rga finished” before proceeding to next command.
   You can run experiment using icons or typing commands.
*At the prompt type “ns #”, where # is the number of scans. (To see other acquisition
  parameters it is helpful click “AcquPars” or type “eda”
*At the prompt, type “zg”, after spectrum is acquired, choose  "Processing -> Data
   Processing Guide". Click “Window Function and choose proper one to your
   molecule   “Window function type” and "Size of the line broadening”
  Go to the next menu and click “Fourier transform” and choose proper size “SI” for
  your spectrum. Click “OK”
  Click “Phase Correction” Choose “manual” and do it manually (recommended) or “automatic” (not always works).
* Click on “Axis Calibration”, select solvent peak or TMS with the left mouse button,
   and type in the solvent chemical shift (reference table is on the bulletin board)
   Click “Baseline Corr.” button and chose proper for your molecule way to get good
    baseline (very important for accurate integration)
   Click “Pick Picking” button and generate the peak list of the spectrum.
* Click the “Integration button” and perform integration.
   When spectrum ready for plotting click the “Plot/Print” button. Choose print with layout and
    start the plotting editor. Click on spectra icon and put your spectrum into the window. Select “1D/2D-Edit”
    and customize spectrum according to your needs. Select the “File->Print” and you will see the preview.
    If you are satisfy click print and spectrum will be plotted.
* After experiment is completed:  Click BSMS icon again.  “Click lock OFF” and
   “spin OFF” buttons
    Quit the lock window.
    Retrieve the sample, Press “LIFT” button.
* Make sure the none of button “lock”, “spin” or “lift” lit when you leave.
   Quit BSM menu
   Exit Top Spin
 * From the Linux window choose “Action->logout”
 * Insert the plastic cap on top of the sample insertion port.
 * Record your time in the logbook


There is a more extensive version of this manual. Contact lab manager if you are interested.