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Nuclear Magnetic Resonance Facility

EZ Procedure for One Dimensional Experiment on Unity 300

(LC: left click; RC: right click; CC: center click)
1. Sign the logbook.
2. Type user ID and password
3. LC Main Menu, LC File, LC Set Directory, LC Home or change to a specific directory.
4. LC Main Menu, LC Setup and choose the appropriate nucleus and solvent button. If you are going to run a routine 1D experiment like 13C {1H} in CDCl3 then LC 1:C13, CDCl3, type su.
5. Position your sample, Type e, after hearing air, insert your sample into magnet, Type i.
6. For CDCl3 solvent, type rts('cdcl3') su . For other solvent type rts('std') su to read shim file.
7. LC acqi. The new window should appear. LC Lock, LC Lock off, LC Spin off,
Adjust lock gain 40 to 45 and lock power 30 to 45 until you see wave pattern(within the range try low power and high gain). Adjust Z0 until you are on resonance (wave pattern become straight line) and then LC Lock on. The sample should now be locked. Decrease the Lock power and Lock gain to maintain the lock so that it is not saturated (approx. settings: lock power = 36 and lock gain = 40) and the lock level is approximately 40-80%. Adjust the Lock phase to get the maximum signal. Keep the spinning rate set at 20 Hz. LC Spin on.
LC Shim for interactive shimming. Maximize the lock level by adjusting Z1 and Z2. You should have to adjust Z1 and Z2 only to increase the value as high as possible. Set lock level is approximately 50-80% by adjusting lock gain then LC close to close the Acqi window.
8. You will not have to tune the probe for 1H and 13C UNLESS you will be working with very polar or ionic solutions or you are going to run an experiment that requires precise tuning.
9. Type dg to display parameters. The parameters are changed by typing in for example nt=256. Type bs=16, Type time to see how long the experiment will take. Type ga to run experiment.
10. Type wft. Type f full aph to perform the automatic phasing. Manually phasing if necessary: LC phase, LC on biggest peak, hold left button and move mouse to get right phase for biggest peak, then RC on far peak, hold right button and move to get right phase. Type ds.
11. The middle mouse button adjusts the intensity of the spectrum. Hold CC and drag the mouse to make changes the display intensity.
12. To expand define spectral region for example 0-180ppm Type ds, type cr=180p, RC on spectrum to get right cursor, type delta=180p, LC expand to expand a defined region shown by the two cursors. LC full or by typing f to get full spectrum.
13. LC at the center of ref peak, type nl, type rl(7.26p) reference the selected line to 7.26ppm
14. (optional) To integrate the spectrum first LC partial integral then:
1). Type cz to reset the integral values, cdc to cancel drift correction and dc to apply drift correction.
2). LC on left side of farthest left peak, Type z to cut the first integral, LC the right side of the peak and type z to define the other side of the integral. Repeat this for all peaks of interest.
3). To calibrate integration, LC at one integral peak, LC Set Int.
15. LC th. Move the left mouse button to set the position of the threshold line. Type dpf to display the peaks found on the screen.
16. Type vp=12 to move the spectrum up to allow for plotting the numerical integral values
17. type in text('abc=description of data') where abc is the filename that you will save the data under and the written portion after the = sign is a personal description of the sample, notebook page, solvent etc.
18. To save the spectrum, make sure that you are in your home directory by typing pwd. It should display a directory string. If it does not show the directory you want, repeat step 3. then type svf('abc') where abc is the filename that you assigned to the dataset. There is a 10-12 character limit for the filename. To retrieve the data type rt('abc') at the dataset directory, or find the dataset of interest and click on to highlight it then LC load. Type wft to transform the data then display it or type su to use the parameters to collect new data from these starting parameters.
19. To plot the spectrum type pl pscale pltext ppf pap pir page, pscale, pltext, ppf, pap and pir are optional.
20. To finish using the Varian Unity Plus NMR spectrometer, LC acqi, LC lock off, LC spin off then LC eject and stop the air flow with the LC insert, LC Close.
21. To exit VNMR you must follow these steps. If no experiment is running it will say that it is idle. If there is an experiment running stop it by typing sa or aa or LC abort acquisition. Once you have determined that no experiments are running then move mouse out of the VNMR window and Hold RC and choose the exit option from the pull down menu.