Estimate proton T1
Please read TOPSPIN_note to learn how to run TOPSPIN if needed.
(1) Create H-1 file.
Open one of your files.
(Click) “New” and give a new filename and “EXPND” number.
(2) Lock and Shim as usual
Insert your sample and spin it.
Load shim file: (Type) ‘rsh’ -> (select) “xxx_current.shim”.
Select solvent and lock: (Type) ‘lock’ -> (select) “CDCL3”.
Shimming: (Type) ‘gradshimau’.
(3) Get normal H-1 spectrum
Load standard parameters for proton: ‘rpar PROTON all’.
Tuning probe with command ‘atma’ for b500b and ‘wobb’ for other machines.
If probe tuning is bad, please contact the managers.
(Click)“AcquPar” -> Change Pulprog to ‘zg’ ->
‘getprosol’ -> ‘rga’ -> change ‘ns’ if needed ->
‘zg ef apk’ -> get a correctly phased spectrum.
(4) Reset O1 if necessary.
Move the cursor to the peak interested and click on ‘O1’.
Repeat step (3) with the new O1.
(5) Check p180 pulse degree.
Copy above experiment to a new experiment,
“AcquPar” -> Change Pulprog to ‘t1ir1d’ ->
‘getprosol’ and set d7 = 0.001s.
‘zg efp” (do not use ‘apk’ here!) and see if the peak is negative and has almost the same amplitude as one got from step 4.
If it is not, talk to manager and do not continue.
(6) Estimate T1
Change d7, ‘zg efp’ (do not use ‘apk’!) until get zero signal.
Write down d7 when signal is near zero. T1 ~ 1.4*d7.
(7) Confirm T1.
Set d1 = 5*T1, keep the same d7 value for zero signal.
‘zg efp’ to see if get a zero signal.