Optimizing Lineshape 60MHz
Instructions for optimizing the lineshape for the Eft NMR.
(Note: The PNMR instructions are printed in blue. NUTS commands are printed in red.)
1) For spinning rate and referencingwater sample - spinning
- run the prep routine (type: prep <Enter> and follow onscreen prompts)
- you’ll need to slow the spinning at one point and then speed it up later.
- Make sure the sample is spinning at a constant speed (4-6 squares apart)
- shims X, Z, C and Y to minimize spinning sidebands and improve spinning lineshape
- Also sets the correct spin speed for later data acquisition.
- takes about 5 minutes
2) For lineshape optimization
- water sample - spinning
- run the shim2 routine (type: shim2 <Enter> and follow onscreen prompts)
- shims 4th, 3rd, C and Y to improve spinning lineshape
- takes about 15-20 minutes
3) Reduce spinning sidebands further
- water sample - spinning
- run the suprep routine (type: suprep <Enter> and follow onscreen prompts)
- you’ll need to slow the spinning at one point and then speed it up later.
- Make sure the sample is spinning at a constant speed (4-6 squares)
- shims XY, X, ZY, Z, C and Y to eliminate spinning sidebands and improve spinning lineshape
- Also sets the correct spin speed for later data acquisition.
- takes about 20 minutes
NOTE: Sometimes, you’ll need to repeat steps 2 and 3
4) OPTIONAL: For final lineshape optimization
- 5% ethyl methacrylate or 5% ethyl benzene or 5% ethyl trans-crotonate – spinning
- run the shim3 routine (type: shim3 <Enter> and use a 5 second relaxation delay)
- shims 3rd, C and Y to improve spinning lineshape for organic samples
- takes about 15 minutes
5) Calibrate the pulse widths and decoupler
- 98% n-propylbenzoate sample – spinning
- Shim the sample (type: shim <Enter> and use RD=2)
- Set the reference(type: zgh, a2, fo, zgh, a2, etc…)
- Go to the TST> prompt (type: nu tst <Enter> )
- Run the full Calibration (type: chcal <Enter> <Enter> )
- Call to make sure the numbers make sense (call us if they don’t at 866-494-9369)
- Run Calibration again (type: chcal <Enter> <Enter> )
6) Check the calibration
- 98% n-propylbenzoate sample – spinning
- Go to the C13> prompt (type: nu C13 <Enter> )
- Run a DEPT experiment (type: dept <Enter> )
- Process the DEPT. (in NUTS type: <CTRL>+F11 )