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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
- The JEOL sample tube (rotor) manual: JEOL Sample tube manual PDF
- 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 tubeRequired sample tube: NM-05410ST32 (Zirconia, ZrO2); Order through parts@jeol.com
Sample tube packing kit: NM-02611SHP32
JEOL 3.2 mm Sample Tube
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Taking apart an empty JEOL tube
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Packing a sample tube without spacers (50 mm-cubed sample volume)
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Unpacking the tube (without spacers) and cleaning
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Using spacers in JEOL 3.2 mm tube to pack a smaller sample volume (27 µl or mm-cubed)
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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
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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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