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I am on JEOL 300

 

Contents

 

Planning Solid-state MAS experiments

Preparation of a sample tube

Preparing the sample on a benchtop spinner

Basic solid-state experiment

Importing NMR data to MNova and Topspin

 

 

 

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Planning Solid-state MAS experiments

Please, read the following documents:

• The JEOL solid-state operation manual:    ECAXS_Solid_Measurement_Manual.pdf

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• The JEOL sample tube (rotor) manual: JEOL Sample tube manual PDF

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• A Solid-state NMR tutorial by Michael Frey of JEOL:  Solids_Tutorial_MHF_2019-01 (Read-Only).pdf

 

The next sections outline protocols specific to our JEOL 300 MHz MAS solid-state system.

 

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Preparation of a sample tube

Required sample tube: NM-05410ST32  (Zirconia, ZrO2); Order through  parts@jeol.com

Sample tube packing kit: NM-02611SHP32

JEOL Sample tube manual PDF

 

 

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Preparing the sample on a benchtop spinner

 

NOTE: You must follow this protocol for packing the tube on a bench-top spinner or testing a prepacked tube prior to inserting it in the probe: User Protocol - Packing the sample.pdf

 

 

 

 

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Basic solid-state experiment

 

A standard protocol for a basic Solid-State NMR experiment

• Download:   User Protocol - Solid state experiment - v4.pdf

 

 

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Importing NMR data to MNova and Topspin

 

MNova Lite CDE

• MNova Lite is available to ND users from our website
• Import of NMR data to MNova is simple: just drag-and-drop from the file browser.

 

Topspin

• From main menu in Topspin, click File:Open
  • choose "Open NMR data stored in special format"
  • set File Type: JCAMP-DX
  • click OK - browser window opens
    
    
• Navigate the window into the folder containing your NMR experiments
  
  
• Select one of the experiments (name.jdf) and click Open button
  
  
• A fromjdx window opens
  • set EXPNO field to 1
  • DIR field should contain a full path to where your converted data should be. I suggest creating a separate folder on the same level with the original Varian data. Example:
    • My data were in /Users/kovrigin_laptop/Documents/Workspace/Data/Data.XVIII/EKN98.Dale.full_reaction.repeat/data
    • experiment was exp7.fid
    • I copy-paste the ENTIRE path from VNMR-name field into DIR omitting the actual experiment name
    • modify last folder name data to become data_converted
    • select entire path and copy it to clipboard - we will need it to set up a new folder in Topspin Browser (below)
      
      
      
    • Click OK
      
      
• Add the folder with converted data to the Topspin Browser:
  • Right-click in the Browser window of Topspin and select Add New Data Dir
  • paste the new path from clipboard to DIR field
  • Enter convenient name to in ALIAS field to be displayed in Topspin Browser (in my example Varian)
    
    
• View the newly converted dataset same way as standard Bruker data
  
  
• Now you can return to File:Open to convert more files
  • the conversion window remembers your paths. All you need to do is to select a new Varian .fid folder
  • to refresh a list of converted files in Browser you should fold and unfold the folder by clicking on an arrow next to its name
    
    
    
  • Whether you have .fid extension on Varian datasets or no extension - does not matter.
    
    
    
• NOTE: Sometimes Topspin hangs after conversion. To clear the condition navigate your file browser to the folder (on Mac) /Applications/TopSpin 3.5pl7 Utilities and launch the Terminate TopSpin.app.
  
  
  
  
• After that - start Topspin again
  

 

 

 

 

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