University of California, Riverside

NMR Facility



Avance NEO 400 Help


Basic 1D || Console Reboot

Basic Operation Guide: Bruker Avance NEO 400  

I   Logging in and Starting TopSpin 

  1. Sign in in the logbook before you start.
  2. If the screen is black, move the mouse.
  3. Type in your user name <return>, type in your password <return>.
  4. Click on the TopSpin 1.3 icon with the middle mouse button.

II  Ejecting and inserting samples

  1. On the BSMS unit, make sure both [SPIN ON-OFF] and [LOCK ON-OFF] are turned off. Press the [LIFT ON-OFF] button to eject the reference sample.
  2. Remove the sample from the spinner and position your sample properly in the spinner using the depth gauge. Wilmad 506PP or equivalent NMR tubes are required for this instrument. The sample height should be 4.5 cm or more (approx. 0.7 ml).
  3. With the eject air still on, place the sample and the spinner into the top of the magnet. Press the [LIFT ON-OFF] button to insert the sample. Press the [SPIN ON-OFF] button to spin the sample.

III  Setting up and running a 1H NMR experiment

1. Create a new dataset

a)   Click the a300 new experiment button in the upper toolbar.
b)      Specify the dataset NAME, EXPNO, PROCNO, DIR, and USERin the dialog box.  If one or more datasets are open, the fields are initialized with the current dataset.
c)   Click the down-arrow of the Solventbox and choose a solvent from the list, or type a solvent name.
d)      Click the down-arrow of the Experimentbox and choose a parameter set from the list (e.g. H1-STD for proton NMR).
e)   Type the dataset title in the TITLEbox.  Click OK. An empty dataset will be created and initialized with the parameters of the chosen experiment.

2. Lock and shim*

a)Type lockdisp <return> to bring up lock display window.  Type lock <return> to get the solvent list, click to select the solvent you are using and click OK.  Auto locking starts.
b)After auto locking finishes, press the [ONAXIS] and [FINE] buttons on the BSMS unit if not lit, press the [Z1] button and shim Z1 with the wheel on the BSMS unit to maximize the lock level, press [Z2] and maxmize the lock level.  Continue to iterate in this manner until you can no longer increase the lock level.  If the lock level goes off the top of the lock display window, then use the [LOCK POWER] or [LOCK GAIN] button then use the wheel to bring the lock level down and start shimming again.
c)Press the [STBY] button to deactivate the wheel.

 *If you are using a Non-deuterated solvent, make sure the [LOCK] and [SWEEP] button LEDs   are off .  Skip section III. 2 and proceed to section III. 3.

3. Type ased <return> to edit the acquisition parameters. Edit the parameters as needed.

4. Type rga <return> to set the receiver gain. Click the a300 start acq button to begin acquiring. To stop the acquisition early, click the a300 stop acq button. The  button a300 stop sign will also stop the acquisition but will not update the data.

 If you want to view the spectrum before the acquisition has finished, type tr<return>, then follow the instruction in section IV to do Fourier transform and phasing.    

IV  Processing 1D data

1. Fourier transform and phasing the spectrum: Type ef <return> to process, apk <return> to phase the spectrum automatically.  Fine phase adjustment can be performed by clicking the indicated button in the upper toolbar:

a300 phase

After clicking the phase button, the TopSpin program automatically places the red cursor on the biggest peak.  Click-hold on the a300 0 order phase adj button and move the mouse up and down for zero order correction (spectral region around the biggest peak), then click-hold on the a300 1st order phase button and move the mouse for the first-order correction (spectral region distant from the biggest peak).  Click the a300 save par  button to save and execute the phase correction.

2. Zooming – In/Out using the mouse: Click the mouse button to put the black cursor line at one edge of a peak or multiplet. Click-hold and drag the cursor line to the other edge of the peak or multiplet and release the button.  You should now see the expanded region on the screen.  To reset zooming (horizontal scaling) to full spectrum, click the a300 full spectrum button.

3. Calibrate the chemical shift: First, zoom-in on the reference peak. Click the indicated button in the upper toolbar:

a300 reference shift

Position the red cursor line on the reference peak and click the mouse button. A dialog box will pop-up. Enter the correct ppm value for the reference peak and click OK. The spectrum will be calibrated and re-displayed. TopSpin will automatically leave calibration mode.

4. Integration:

a) Type abs <return> to straighten the baseline.
b) Click the indicated button in the upper toolbar:

a300 integrate

To define integral regions, click the a300 integral regions button.  Put the red cursor line at one edge of a peak or multiplet, click-hold and drag the cursor line to the other edge of the peak or multiplet.
c)Repeat step b for all regions to be defined.
d)To calibrate a given integral, click inside the integral region with the right mouse button, choose Calibrate from the popup menu, a dialog box will appear.  Enter the desired integral value and click OK.
e)To save the integrals and exit integration mode, click the a300 save par button.
f) To print the integral list, click the Integrals tab of the data window to show the list, then click the a300 print  button in the upper toolbar to open the Print dialog box.  Select Print active window, Click OK and Print.

5. Peak picking: Click the indicated button in the upper toolbar:

a300 peak pick

With the mouse click-hold and drag to draw a green box.  The box should cover the top of the peak(s) to be picked.  To print the peak list, click the Peaks tab of the data window to show the list, then click the a300 print button in the upper toolbar to open the Print dialog box.  Select Print active window, click OK and Print.

V  Plotting a 1D spectrum

Click the Spectrum tab in the data window.  Click the a300 print button in the upper toolbar to open the Print dialog box.  Select Print active window, click OK and Print,then click OK.

VI  Setting up and running an X nucleus NMR experiment

1. Create a new dataset

a)Click the a300 new experiment button in the upper toolbar.
b)Specify the dataset NAME, EXPNO, PROCNO, DIR, and USERin the dialog box. If one or more datasets are open, the fields are initialized with the current dataset.
c)Click the down-arrow of the Solventbox and choose a solvent from the list, or type a solvent name.
d)Click the down-arrow of the Experimentbox and choose a parameter set from the list (e.g. B11-STD for boron-11 NMR).
e)Type the dataset title in the TITLEbox.  Click OK.

2. Type atma <return> to begin tuning the probe for both observation and decoupling channel. The tuning will take about 2 minutes.

3. After the tuning is finished, Type ased <return> to edit the acquisition parameters, make any desired change.  Type rga <return> to set the receiver gain.  Click the  button to begin acquiring.  To stop acquiring early, click the   button.

VII  Logging out

  1. On the BSMS unit, press the [SPIN ON-OFF] button and the [LOCK ON-OFF] button to stop sample spinning and turn off the lock respectively.  Press the [LIFT ON-OFF] to eject your sample.
  2. Remove your sample from the spinner and position the reference sample properly in the spinner using the depth gauge.
  3. With the eject air still on, place the sample and the spinner into the top of the magnet. Press the [LIFT ON-OFF] button to insert the sample.
  4. Go to File and choose Exit.Click on the screen background with the right mouse button and select logoutxxxx”, then click Logout. Sign the logbook with time out.

The Figure below shows the TopSpin window with two data windows in the data area and the browser:

a300 TopSpin Window

Avance 300 Console Reboot

Step 1. Exit TopSpin.  Open the console door; press the red reset button (upper left side). Close the door, wait one minute. Start TopSpin and type ii<return> on the command line.  If error messages are displayed click OK/Close then run the ii routine again. You should see no error messages the second time through.  If Step 1 does not work proceed to Step 2

Step 2. Exit TopSpin.  With the right mouse button pressed, select “Open terminal”. Within the terminal window type the bold entries below.

[user@chem2126b dir]$ telnet spect<return>
login: root<return>
spect> init  5<return>

Note: If you do not get the login prompt go ahead and do 2B and 2C. Then repeat Step 2 starting from 2A.

B.  Open the console door, turn off the BSMS/2 unit (lower part), turn off the AQS unit (upper part).  Close the door and press the red button to turn off the console power.

C.  Press the green button to turn on the console power.  Open the console door, turn on the AQS unit (upper part), wait 20 – 30 seconds, then turn on the BSMS/2 unit (lower part).

  1. Close the door.  Start TopSpin and type ii<return> on the command line. If error messages are displayed click OK/Close. Type ii<return> on the command line again. You should see no error messages the second time through. Type lockdisp<return>, type rsh<return>.  Select the latest default shim file and click the Read button.  Type rsh<return> and select the latest default shim file again, then click the Read button again to retrieve default shim setting. It is important that you read in the shims twice as they will not be properly read the first time.

 

If you encounter any problems, please contact Dan Borchardt (phone 2-3628, e-mail dan.borchardt@ucr.edu).

More Information

General Campus Information

University of California, Riverside
900 University Ave.
Riverside, CA 92521
Tel: (951) 827-1012

UCR LibrariesCampus Status
Career OpportunitiesDiversity
Visit UCRMaps and Directions

Facility Information

Nuclear Magnetic Resonance Facility
Chemical Sciences Bldg.

Tel: (951) 827-3628
Fax: (951) 827-4713
E-mail: danb@ucr.edu

Footer