Department of Chemistry NMR Facility
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Read the procedures completely before running.
Procedures to run 2D experiments on the Bruker 500 using ICON NMR.1. In a blue UNIX window type login chem357 or chem657 then enter the password. Unix windows are created under the ToolChest menu -> Desktop->Open new UNIX shell
2. Type xwinnmr at the prompt.
3. Use a sample with one drop of compound or pour out 1/2 to 1/3 of your existing sample and refill with CDCl3. Too concentrated a sample will lead to poor shims.
4. Type ej to eject sample in the magnet and insert your properly prepared sample.
5. Type ij to insert your sample. Next, you need to lock on to your solvent:a. Type rsh 5mm.tbi.cdcl36. Tune the probe to your solvent follow:
b. Type lock cdcl3a. Type rpar PROTON all7. Type iconnmr to start ICON.
b. Type ro answer yes and 20Hz.
c. Type a to see the acquisition window.
d. Type wobb to see the tune/match curve.
e. If you do not see the dip click on wobb-sw and press enter then type in 40 MHz for the window size.
f. Go and tune and match the curve with the small tool.
g. Type stop.
h. Type rpar C13CPD all
i. Type a
j. Type wobb
k. This tune/match curve is for C13. Use the stick with the blue stripe to center the curve.
h. Type stop.
8. Login under you ID
9. Follow standard procedures for ICON.
10. Following is a list of individual experiments and composite experiments:wfu_gCOSYSteps 11 - 17 will make this process go faster but must you follow closely. You can skip directly to Start at the expense of taking more time.
wfu_gHMQC
wfu_gHMBC
wfu_gNOESY
wfu_ROESY
wfu_cosy_hmqc_bc (Use this one and do the NOESY or ROESY if you have time left)
wfu_gcosy_hmqc_hmbc_noesy
wfu_gcosy_hmqc_hmbc_roesy
11. Look at an existing 1H spectra for your compound and make the following chart:
Entry Parameter How the value is found 1 sw (used in left column) Find the left and right ppm range in your 1H spectra that will encompass all of your peaks. Subtract these numbers 2 o1p Determine the middle of this range 1H range by taking an average of left and right values. 3 sw (used in right column) 250 for 13C 4 o2p 110 for 13C 12. Before starting look at the top of the window you have been working in and click on Parameters and choose Edit Acquisition Parameters.
14. Choose Proton and change the value of SW (left column near top) to the sw for 1H in your chart (first entry).
15. Scroll down and change the parameter O1P (left column) to the 1H value (second entry in the chart).
16. Click on Save and go back to Parameters and edit the COSY by changing the SW parameter in BOTH columns to the value for your 1H spectra (first entry in chart). Scroll down to o1p and change to the value in your 1H spectra (second entry in chart).
17. Click on Save and go back to Parameters and edit the HMQC by changing the SW (in left column) to the 1H value (first entry in chart) and SW (in right column) to 250 (third entry in chart). Next change O1P (scroll down and look in left column) to the value for your 1H (second entry in chart). Scroll down a little more and change O2P (look at left column) to 110 (fourth entry in chart) .
18. Click on Save and go back to Parameters and edit the HMBC just like you did the HMQC in step 1.
19. When finished click on Start.
Common Problems and their solutions:
Fail to Lock: Stop and restart again. If fails again, exit to XWIN and type rsh and click on a good shim file. Most common is 5mm.tbi.cdcl3. Type lockdisp then lock and chose your solvent. If locks try ICON again. If fails to lock get NMR lab manager.
Fail to Spin: Stop and restart again, if still no spin eject, check tube depth, clean and try again. If still no spin type another tube. If still no spin get NMR lab manager.