H-H NOESY
GN/Tecmag-300

 

(These instructions assume you are familiar with basic Macintosh procedures, if you are not, see a Macintosh manual or the tutorial which is on most Macintosh computers. Throughout the following, MB means mouse button.)

Basic Acquisition

Collect a 1D H-1 spectrum (see Acquisition and Processing of 1D H-1 Spectra). Record the RCVR gain value; it can be found among the parameters listed in the Dashboard. Go to the Console AIR window and set the Spinner air flow to 0. Go to the LOCK window and increase the RX gain value so the the lock level is near 90. Close the currently active file and open the noesysetup file located in the setup files folder. Open the Dashboard window and set the RCVR gain to the value that you used when collecting the 1D H-1 spectrum. Hold down the Apple key and enter z to begin spectrum acquisition. A dialog box will appear that is used to enter the name of the file which will contain the data and the folder in which the file will be saved. The spectrum will have 256 t1 increments and will take about 2.9 hours to collect.

Potential Adjustments of Acquisition Parameters

Acquisition time may be reduced by decreasing the Last Delay value and/or the number of t1 increments. If you use a Last delay value of 0.7s and collect 128 t1 increments your acquisition time will be near 51 minutes. Open the Dashboard to change the Last delay value. Move the cursor to the Pulse Sequence button and click the MB to open the pulse sequence window. Move the cursor to the Acquisition Settings (fourth icon from the left on the upper right) button and click the MB to open the acquisition settings dialog box. Change the Scans 2D value to 128. Go to the 2D section and change the SW +/- to 6600. Move the cursor to the OK button and click the MB. Move the cursor to the first T2 icon in the pulse sequence; hold down the option key and click the MB. Move the cursor to the box below First Tau:, click the MB, and enter 1u. Move the cursor inside the Calculate button and click the MB. The number next to Total Items: at the bottom right area of the window should now be equal to the number of Scans 2D that you set in the Acquisition Settings window. Move the cursor to OK and click the MB. Go back to the Acquisitions Settings window and change the SW +/- back to 1650.

Spectrum Processing and Plotting

Move the cursor to the Commands menu item at the top of the screen. Hold down the option key, hold down the MB and drag to nDFT, release the MB. The Multi-dimensional Filter and Transform Settings dialog box should now be on the screen. Move the cursor to the Load button at the bottom of the dialog box. Click the MB and then go to the setup filesgn folder and open the noesyprocess file. If you changed the Scans 2D value before collecting your spectrum, you should go to the 2D area of the Multi-dimensional Filter and Transform Settings dialog box and set the Width value equal to the Scans 2D value. Move the cursor to the Apply settings button and click the MB to process the data. See Chapter 9 of the MacNMR manual for instructions on viewing and printing the processed data. When in the 2D display mode, move the cursor to Edit at the top of the MacNMR window, drag to Preferences and then drag left and down to 2D. Move the cursor to the circle between Vertical: and Invert and click the MB to put a dot in the circle. This will fix the orientation of the displayed noesy spectrum in the vertical dimension. Make you use the Symmetrize right to left option before plotting and analyzing the data, symmetrization often removes substantial unwanted spectral intensity.


Return to GN/Tecmag-300 Instructions