DRX routine operation

DRX routine operation (revised 03/26/06)

The most recent version of this handout can be found at http://www.msg.ku.edu/~msg/new400.html.

To see the current signup policies for the Avance instruments, go to http://www.msg.ku.edu/~msg/fees.html.

Advance reservations are made using the "reserve" program; your charges are based on actual use, as logged on the host workstation.

At the present time, the following rules are used on the 400:

On Mon-Sat: the time period of 8:30am-8pm is restricted; the nighttime hours, and all day on Sundays and holidays are unrestricted.
For restricted times: signup begins at 4pm the day before.
During the period 9:30am-3pm: you can reserve or use no more than 20 minutes
From 8:30-9:30am and from 3-8 pm: you can reserve or use no more than 60 minutes

Bold words are commands to be typed at the xwinnmr prompt. Italicized words indicate things to select with the mouse.

1. Change the sample. DON'T LEAN AGAINST THE MAGNET--IT IS SUSPENDED ON ANTIVIBRATION DAMPERS. Start the sample spinning, if you are taking survey spectra; for 2D experiments, nonspinning is preferred.

2. Log in on the Silicon Graphics workstation with your user name and password. Open a UNIX shell and type xwinnmr. To open a lock window, type lockdisp.

3. Type new. Starting a new sample, change the file name, put in an appropriate experiment number, and a user name if you want to. For additional experiments on the same sample, change the number only.

4. Type rpar and choose either AAPROTON or AAC13CPD. Then select Copy All. If you open any old spectrum with search, double click it with the mouse to bring it into the Portfolio, and then choose Apply, you bring with it all the parameters used for acquisition, processing, and plotting of that spectrum.

5. Optional step: type eda to edit the acquisition parameters. Make any desired changes and click SAVE. For experiments other than survey spectra, click the PROSOL button to read TRUE. The ased command can be used to examine or change the values of all the pulses, delays, and power levels.

6. Lock the sample with lock cdcl3 (or other solvent name--if you aren't sure what abbreviation is used, just type lock, then choose from the menu). Lock should be found automatically. If it is not found within 20 seconds, try the following: increase the lock gain; slowly move the field setting manually toward lower numbers; reload default shims by typing rsh and then choosing AAQNP or another probe-specific shim file.

7. After lock is established, you may shim Z1, Z2, Z3 manually. If the lock level goes off the top of the screen, then use Lock Gain to bring the lock level down. Then start shimming again with the Z1. For computer shim, type tune and choose example. The computer will shim and then activate Z1/Z2 autoshim for the duration of the experiment. Note: on the 500, you must press the ON AXIS key, so it is illuminated, before you press the Z shim keys.

8. Type rga to set the receiver gain. Like to shim on the fid? Type a (acquisition window), then gs (go setup), shim away. Choose return to go back to the main display.

9. Type zg to take your data. The experiment is finished when the message "checklockshift: finished" appears. To look at a spectrum during the acquisition, type tr, wait for the data to be copied, follow step 10. To stop it early, type halt.

10. Type ef to process, apk to phase your spectrum automatically. Fine adjustment can be performed by choosing phase, biggest, sliding PH0 and PH1 with the mouse, return, save and return.

11. Type abs to straighten the baseline and auto-cut integrals. For manual integration, choose the integrate menu, lock the cursor to the baseline by pressing the left mouse button, and cut the integral with the middle mouse button. Release the cursor with the left mouse button, choose return, Save as 'intreg' and return.

12. If necessary adjust the reference by choosing calibrate, put the arrow on your reference peak, click the middle mouse button, enter the correct chemical shift, exit with the left mouse button.

13. Adjust the vertical scale as desired with the mouse, type pscal and choose global. With CY set to 0, the spectrum will look the way it does on the screen. Choose DP1, enter chemical shift limits for downfield and upfield edges of the plot.

14. Type edg to edit plot options. Most defaults are okay.

15. Type setti if you want to edit a custom title for your plot (using the "jot" editor).

16. Type view to preview the plot. If you are satisfied with it, type plot to plot your spectrum.

17. For a line list/table of peaks, type pps and click on list, then click OK to exit the window.

18. Before ejecting the sample, turn off the lock, the spin, and the autoshim (if you did a "tune") control buttons.

19. Log off the Silicon Graphics computer, remove your sample, and sign the instrument logbook. Remember to take everything with you that you brought into the lab, and dispose of your trash.

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