NMR training and manuals

SIL rules sheet: After completion scan using department copier and email to [email protected]

SOP's

Please watch all of these videos before coming down for hands on training.

First time user training : After completion scan using department copier and email to [email protected]

• Documented NMR training
• Documented SIL rules

Nitrogen filling training : After completion scan using department copier and email to [email protected]

• Documented Nitrogen fill training

Manuals

Agilent 7600- AS User Guide autosampler on DMS NMR (2065 is magnet/autosampler alignment error)

Commands and Parameters VNMRJ version 4.0

Custom Pulse Sequence Generation with button

• make 3 necessary files - all three files should have the same name, see page 483 of Spectroscopy Guide

1. construct yout pulse sequence and save it in psglib, then compile it in a terminal by typing seqgen filename
2. save your parameters in /home/walkup/vnmrsys/parlib (File -> Save as in vnmrj and select par as the file type)
3. save your macro in maclib

• then go Tools -> Study Clones... -> Command & Protocol Button
• click Make Protocol button

Determination of the diffusion constant by NMR

• collect a 1D proton of your sample and optimize pw90 and gain on v400 (data is inconsistent on 400-mr/still working on it)
• use diffusionSS button
• make sure spinner is off
• use at least an nt of 2
• Array gzlvlE with the following values 0, 2000, 6000, 8000,10000,14000,16000,20000
• here is the excel workup of the 1% CHCl₃ in d6-acetone on v400 where you calibrate the gradients with acetone and then workup the CHCl₃ data using the calibrated gradients
• here is a handout on the PFG-SE
• here is a video of the data workup

Running Deuterium NMR

Here is the easy way to do it:

1. Put your sample into the NMR
2. Under automation acquire a proton spection (letting the system autolock and autoshim)
3. After it is done load in a Carbon experiment directly by clicking on it (don’t start a new study queue)
4. Turn off lock by going to the Start tab then Lock, then uncheck the Lock box
5. Now go to te Acquire tab and select channels option then change the Nucleus/freq box from C13 to lk
6. set the gain to desired value (up to 60)
7. set the number of scans to the desired value (nt=xxx, for example nt=128)
8. collect the data, type ga in the command line