31p nmr data collection on the bruker advance 400insert the nmr tube containing the sample in a...

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31P NMR Data Collection on the Bruker Advance 400 There are two ways to run a sample against an external H3PO4 reference shimmed on the FID: a. Use of a capillary tube filled with H3PO4. b. Use of a H3PO4 reference tube; create a shim file first. For a: Insert the NMR tube containing the sample in a non-deuterated solvent (i.e. CHCl3) and a H3PO4 capillary tube and follow steps 15-20 and 26-29. For b: To obtain a 31P-NMR spectrum by using a H3PO4 reference tube, a shim file for an equivalent deuterated solvent should be created/saved on the computer (i.e. to run a sample in CHCl3, write a shim file for CDCl3). Insert the H3PO4 reference NMR tube in the magnet and follow step 13 through 29. Process the data and calibrate the reference phosphorus-peak in the spectrum. Once finished, run the sample in non-deuterated solvent the same way the H3PO4 reference was scanned. *Note Make sure the levels of the solvents in the tubes (H3PO4 reference, deuterated solvent and sample) are at the same height. Creating/saving a shim file of a deuterated solvent The following steps are needed to write a shimfile for a deuterated solvent: 1. Log into the computer under nmr superuser with Topspin as password. 2. Open Topspin 1.3. 3. Insert the deuterated solvent by using the lift on/off key located on the BSMS

keyboard (top left). 4. Go to Spectrometer, then Data Acquisition Flowchart.

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The Flowchart window will open.

5. In the Flowchart, click on New Experiment, the new experiment window will open.

Enter the appropriate information: NAME: Enter the sample code and nucleus to be investigated. The data will be stored under this code. EXPNO: Start with 10 (similar to the automated runs) and continue with 20, 30etc. for the next runs. PROCNO: start with 1 (similar to the automated runs) and continue with 2, 3etc. for the next runs. DIR: will open as C:\Bruker\Topspin.

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USER: enter your username (if you’re checked out on the NMR, you will have a username; the data will then be stored in your file). Solvent: choose the deuterated solvent used i.e. CDCl3 and choose NONE if a non-deuterated solvent is used. Experiment: P31CPD for 31P NMR (H decoupled). TITLE: title of the run Click OK. 6. In the flowchart, click on LOCK while skipping Frequency Routing.

Click on to display the black lock window: Select your deuterated solvent and wait for lock to finish. It should display a horizontal line in the upper half of the window when done.

7. Click on Probe Match/tune in the Flowchart while skipping Temperature.

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Select automatic tuning and wait for it to finish (the acquisition status bar will read atma: finished). When finished the window will look like the figure below.

8. Click on Sample rotation in the Flowchart.

Enter 20 (normally used) and click on start the rotation. On the BSMS keyboard the “spin on-off” key will illuminate. When done the acquisition status bar will read ro: finished.

9. Click on Prosol Pars in the Flowchart. When done the acquisition status bar will

read Prosol pars: finished. 10. Click on Acquisition Parameters in the Flowchart.

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Change the appropriate parameters: NS = 16 DS = 4 AQ(s) = 3.958 D1(s) = 1.0 When done the acquisition status bar will read ased: finished.

11. Click on Shim in the Flowchart, select Gradient Shimming and click OK.

A new shimming window will open. Click Start Gradient Shimming and wait for it to finish (the acquisition status bar will read setsh: finished). Once finished a new window will pop up with the old and new Z values.

12. Type WSH RY CDCL3 (Write Shim file Personal Initials and Solvent) in the

command-line and . Use AK (Andrew Knight) instead of RY in the future.

Select OK in the window with the Z values (this will close this window). Close the Gradient run window.

Running a sample vs. a H3PO4 reference. 13. Replace the deuterated solvent with the H3PO4 reference in the magnet.

If    step  1-‐13  was  done  at  another  time,  insert  the  sample  in  the  magnet  and  type  RSH  RY  CDCl3,  (Recall  Shim  file  Personal  Initials  Solvent)  and  .    

14. Turn  off  Lock  and  Sweep  located  on  the  BSMS  keyboard.  

15. Go to Spectrometer, then Data Acquisition Flowchart.

16. Go to New Experiment (step 5).

17. Go to Probe Match (step 7).

18. Go to Sample Rotation (step 8).

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19. Go to Prosol Pars (step 9).

20. Go to Acq. Pars (step 10). Change the appropriate parameters:

NS = 4 (H3PO4) and

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29. Click on Processing, then Phase Correction, select Automatic Phasing and click OK.

30. Replace the H3PO4 reference with the sample in a non-deuterated solvent in the magnet.

31. Recall  the  shim  file  by  typing  RSH  RY  CDCl3,  (Recall  Shim  file  Personal  Initials  

Solvent)  and  .      32. Repeat step 20 through 29 (remember to use

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Closing the program.

Go to File, click on exit and then OK. Turn of the screen Sign the Logbook

Notes: a. Acquisition with a D1 (delay time) of 4s will take about 22 min for 256 scans 2 min for 16 scans b. It is easier to first open a previously ran file before starting with a new experiment. In the New Experiment window, select current parameters for Experiment instead of P31CPD. 3/2/10 10:54 AM