NMR spectrometer


Procedure for Obtaining an NMR Spectrum

1. Sign log book.
2. Turn on power to the oscilloscope.
3. Turn on spinner air by turning on the toggle switch in the front panel above the R-1200 logo.
4. Wipe off the TMS sample, place in the spinner (white plastic), adjust height and lower it into the probe.
5. Press RESET button ontop control panel of the NMR.
6. Adjust Field Shift knob (or Wide Shift knob if necessary) to get TMS signal at 0.  The chloroform signal will be at 7.5 .
7. Press AUTO RES button or turn resolution knob until the TMS peak has ringing. 
You will hear a beep when ready.
8. Remove the TMS sample and place the spinner on your sample.  Lower the sample into the probe.
9. If the signal is weak, increase the amplitude from 8 to 10.  (press AMPLITUDE, enter the number, and press ENTER.)
10. Set the number of scans to 5.  (press No. of Scans, 5, ENTER.)
11. Hold the ACQ. key in and press ACQ. START/STOP, and then press CORR.
12. To plot and integrate your spectrum - Use the Procedure to plot NMR spectra  (listed below line) using the ink jet printer on the computer using GRAMS Version 1.01 - written by Dr. Mike Panigot (June 28, 2000).
13. When finished with the NMR (including spectrum), push RESET button to remove acquired spectrum from the screen of the oscilloscope.
14. Remove sample from the probe.  Remove spinner and placed it in the sample compartment. Close the sample compartment door.  Turn off spinner air
15. Turn off the oscilloscope.

Procedure to plot NMR spectra using the ink jet printer on the computer using GRAMS Version 1.01 - written by Dr. Mike Panigot (June 28, 2000).
1. Open the R-1200 1.0a transfer program by double clicking on its icon.
2. On menu bar go to Operations and select Transfer File (this opens a dialog box).
3. In the dialog box, enter your filename (you may use as many letters as deisred, recommended is 8 letters or fewer as letters beyond 8 are truncated) and path (usually C:\NMR\DATA\ or C:\NMRDATA) in the Filename box.
(NOTE 1: your filename path - where the R-1200 program puts your file and where GRAMS looks for it may be quite different!)
(NOTE 2: do NOT press enter or OK - this simply closes the box (nothing bad but it is time consuming and a pain).  If you inadvertently close this box, go back to step 2 above and reopen it - it should have the filename and path you had entered still there).
4. Check that the From R-1200 to PC button is selected.
5. Press Start File Transfer button - the computer will let you know when file transfer is done and a new window opens inside the R-1200 program.
6. When file transfer is complete, press enter or click the OK button (closes dialog box).
7. In R-1200 1.0a window, click on Operations on the menu bar and select Convert to ASCII - a dialog box should open with a From line with (yourfilename).nmr and a To line with (yourfilename).asp - if it doesn't check the path.
8. Click on the Convert File button or press enter - when done a second new window opens.
9. At this point, either close or minimize R-1200 1.0a (minimize may be preferable if you are running more than one spectrum) and open GRAMS by double clicking on the Shortcut to GRAMS icon.
10. In GRAMS, under File select Import/ Export (opens a dialog box for the GRAMS converter files.
11. In the new window, select ASCII for the converter name and click on the Import button.
12. A box is opened for the filename to enter (check path to make sure where you saved your file is where GRAMS is looking).  Click on your filename so that it is highlighted and click OK.  Note that double-clicking on the file name does NOT open the file in this instance.
13. A new dialog box opens that has a From box (should have your filename.asp) and a To box (should have your filename.spc).  Click OK or press enter.
14. At this point, go to File and select Open and find your file name etc. OR go to File and below Exit there are four filenames with a number 1, 2, 3, and 4.  File 1 should be the one which you have just converted into a .spc file and you can select it in that manner.
15. (This step is required for integration, it is NOT if you are just going to plot the spectrum as it is BUT you can do this in that case as well)  Under Arithmetic select Baseline and in the new dialog box that opens select Auto Level and click OK or press enter.
16. To plot, under File select Print and check that the printer is set to print in Landscape mode (preferable to Portrait in this case - check under Settings in the print dialog box) and print.
17. To integrate spectrum, under Arithmetic select Integrate - click that what you have is a .spc file (or Real Only) - screen should go from white background to black background.
18. In new dialog box, select Regions
19. In new dialog box, select Add
20. Place the cursor on the left side (start) of the area to be integrated and click Right mouse button (screen says left but that does not work). Repeat for the right side (end) of the area to be integrated.
21. Repeat Step #20 for each region of the spectrum you wish to integrate.
22. Copy the numbers for the integration down - the printer will NOT print integration.
23. Exit from the Regions dialog box and from the Integration dialog box - should return to a white background.
24. If you are done with your current sample but have other samples to run, close the file (under File, select Close and leave GRAMS open.  If you are done and have no additional samples to run, close GRAMS.
25. Shut down NMR (turn oscilloscope off, turn air off, place all samples in tray) as indicated for the instructions to that instrument. (see above)

Note: In GRAMS, if at any time the message "No Slots Available" occurs, under File select Clear All Slots.

CHEM4204 Experiment list

Revised 11/22/02