It doesn’t seem that anyone was able to get this sequence working in the past around the time it was published and is not currently being used. So I have tried to write it for my AVANCE I system. However, upon testing there are a few issues so I am hoping someone can help me out with the code (I have copied it to the end of this message).
When I run the sequence the spectrum does not seem to phase cycle properly. The final scan of the phase cycle generates a near null anti-phased spectrum. Also there are spurious peaks around the transmitter frequency and always appear with respect to the transmitter no matter which peak I place the transmitter on. I have tried turning off the gradients, optimized all pulse widths and powers for both excitation and decoupling channels but the same problems arise. One of my suspicions is that the line where the broadband decoupling pulse and shaped pulse are to occur simultaneously is not correct. Any insight and help is greatly appreciated.
I would like to thank Sebastian Kemper for suggesting to look at the1H-19F 1D HOESY sequence by Tim Claridge (
http://onlinelibrary.wiley.com/doi/10.1002/chem.201201577/abstract) as an alternative starting point as well.
Regards,
Joel
-----------------------------------------------------------------------------------------------------------------------------
;hetgoesy
;Gradient Enhanced 1D heteronuclear NOE with 1H detection
;
;K. Stott & J. Keeler, Magn.Res.Chem. 34, 554 (1996)
;
;$CLASS=HighRes
;$DIM=1D
;$TYPE=
;$SUBTYPE=
;$COMMENT=
#include <Avance.incl>
#include <Delay.incl>
"d9=d8-p2/2"
"d11=30m"
1 ze
2 30m do:f1
(d1 pl12 cpd2):f1
30m do:f1
3 (p2 pl2 ph1):f2
grad {(0)|(0)|(cnst23)}
1m
grad {(0)|(0)|(0)}
30m do:f1 pl13:f1
(center (p6:sp6 ph10):f2 (p6 cpd2):f1)
30m do:f1
grad {(0)|(0)|(-cnst23)}
1m
grad {(0)|(0)|(0)}
1u
grad {(0)|(0)|(-cnst24)}
1m
grad {(0)|(0)|(0)}
30m do:f1 pl13:f1
(center (p6:sp6 ph11):f2 (p6 cpd1):f1)
30m do:f1
grad {(0)|(0)|(cnst24)}
1m
grad {(0)|(0)|(0)}
(p2 pl2 ph1):f2
d9
grad {(0)|(0)|(cnst25)}
1m
grad {(0)|(0)|(0)}
(p1 pl1 ph1):f1
grad {(0)|(0)|(-cnst26)}
1m
grad {(0)|(0)|(0)}
(p1*2 pl1 ph1):f1
grad {(0)|(0)|(cnst27)}
1m
grad {(0)|(0)|(0)}
go=2 ph31
30m do:f2 mc #0 to 2 F0(zd)
exit
ph1 = 0
ph10=0 1 2 3
ph11=0 0 0 0 1 1 1 1 2 2 2 2 3 3 3 3
ph31=0 2 0 2 2 0 2 0
;pl1 : f1 channel - power level for pulse (default)
;pl2 : f2 channel - power level for pulse (default)
;pl12: f2 channel - power level for CPD/BB decoupling
;pl13 : f1 channel - dec power level duiring sel X pulses
;p1 : f1 channel - 90 degree high power pulse
;p2 : f2 channel - 90 degree high power pulse
;p6 : f2 channel - shape pulse duration [1.2 ms]
;d1 : relaxation delay; 1-5 * T1
;d8 : mixing time
;d9 : adjusted mixing time
;d12: delay for power switching [20 usec]
;NS: 16 * n
;DS: 4
;td1: number of experiments
;FnMODE: States-TPPI, TPPI, States or QSEQ
Received on Thu Oct 09 2014 - 10:04:46 MST