NMR Processing (TopSpin 3.2)
September 23, 2013
TopSpin 3.2 NMR processing software is installed on all of the computers in the Computer Lab (room 1312), the two stand alone computers in the NMR room (3184) and on many of the research lab computers in the Department. Log-in is typically done with the “chemstud” username and “studen” password.
Open TopSpin by clicking on the Topspin 3.2 desktop icon.
A directory should appear on the left-hand side of the window.
Click on the appropriate directory for your data.
Click on the data file name and drag it into the spectrum window. Use the scaling buttons to adjust the spectral display. You may also use these buttons during the use of any of the options listed below.
If your data has not already been converted from the time domain (fid) to the frequency domain (spectrum), click on the Process option on the Top level toolbar and then select from the following options. Note: If you hold the cursor over any buttons on the toolbars, an explanation of what function is performed should appear.
Proc. Spectra - This will auto process and autophase your fid to produce a spectrum.
Adjust Phase - If required proceed as follows:
Click on the Adjust Phase button. Note the spectrum window tool bar will display a new set of buttons, and the largest peak in the spectrum will be marked with a red line
Click and hold the 0 button while scrolling the mouse up and down to achieve a flat baseline on both sides of the largest peak.
Click and hold the 1 button and scroll the mouse up and down to achieve a flat baseline on the other peaks in the spectrum.
When you are satisfied with the phasing click the save and return button. If you want to start over, just click on the return button.
Calib. Axis - Before selecting this option, blow up the region for your calibration peak. Normally this is the TMS peak which should come at 0 ppm. If your calibration peak is not at the correct position then:
Click on the Calib. Axis tab. Note the spectrum window tool bar will display a new set of buttons.
Click on the button with peak that has a 0 under it.
(OVER)
Click on the center of the calibration peak for your spectrum and this should bring up a calibrate box.
Enter the correct position of the calibration peak in ppm, which is zero for
TMS.
Press enter and this should complete your calibration, giving you the correct position and take you out of the calibration mode.
Pick Peaks - Click on the Pick Peaks button. Note the spectrum window tool bar will display a new set of buttons.
Click on the define peak picking range button. (This button turns orange when it is active.)
Use the mouse to draw a box around the peaks to be marked.
After you have picked all of your peaks, click the save and return button. If you want to start over, just click on the return button.
Integrate- Click on the Integrate button. Note the spectrum window tool bar will display a new set of buttons. It is usually helpful to blow up the regions that you integrate, in order to get reasonable baseline area before and after the peak.
Click on define new region button. (This button turns orange when it is active.)
Use the mouse to scroll across regions of the spectrum to be integrated.
If you want to modify the reference value for your integrations, right click on the region you want to use to calibrate the integrated area and enter the value that you want that peak to have. (Frequently people will chose the smallest peak in the spectrum for their compound and set that value to 1.00 to have all other peaks compared to that peak.)
Click the save and return button
To print the spectrum click on File at the top of the screen and then click on print.
When the print window comes up, leave the option for print active window and click
on OK. Your plot should print to the default printer for the computer. This will only
print the spectrum and title. If you want to print a more comprehensive report, you
will need to go to the Publish option on the top level toolbar and then into the plot
tab for the spectrum.
If you have other ways that you want to use your data or want to print a more comprehensive report, you may go to the Publish option on the Top level toolbar. This option gives you alternatives for copying (for placement in a word document, PowerPoint, etc), printing, changing your plot layout, making a PDF file of your spectrum, or e-mailing your data to someone else. Details on this option will be covered in another instruction set.
