Friday, July 23, 2010
Deuterium Decoupling
Bruker NMR spectrometers equipped with a 2H TX board and 2H amplifier can be setup to carry out 2H observation and decoupling experiments while still maintaining a 2H lock. Two channel systems can use the 2H transmitter for 2H, 1H[2H], 2H[1H] and X[2H] measurements. In addition to these, a three channel system can be set up for X[2H, 1H] measurements. The first figure below shows the 13C and 13C[2H] spectra collected for a mixture of deuterated solvents using two channels of an AVANCE spectrometer. The second figure shows the 13C, 13C[1H], 13C[2H] and 13C[1H, 2H] spectra for the standard 13C sensitivity sample (40% para-dioxane and 60% deuterobenzene) collected on a three channel Bruker AVANCE spectrometer.
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4 comments:
Hi Glenn,
I really enjoy reading your blog, I've learnt heaps.
I was wondering if the 13C[1H,2H] spectrum was collected using the zgigf2igf3 pulse program and WALTZ-16 for the 2H. I'm very keen to give this a go.
Thanks
Alasdair
Hi Alasdair
I collected the data in this post 10 years ago on an AVANCE I console and unfortunately I no longer have it in my archive. I believe I used the pulse program below to collect the data. I believe I used waltz decoupling for 1H and garp decoupling for 2H but not 100% sure.
Good luck
Glenn
;zgig2h
;avance-version (07/04/03)
;1D sequence with inverse gated decoupling
;using 2H lockswitch unit or BSMS 2H-TX board
;2H decoupling in f2
;1H decoupling in f3
;
;$CLASS=HighRes
;$DIM=1D
;$TYPE=
;$SUBTYPE=
;$COMMENT=
#include
"d11=30m"
"d12=20u"
"acqt0=-p1*2/3.1416"
1 ze
d11 pl12:f2 pl13:f3 LOCKDEC_ON
d11 H2_PULSE
2 30m do:f2 do:f3
30m H2_LOCK
6m LOCKH_OFF
d1
50u LOCKH_ON
d12 H2_PULSE
p1 ph1
go=2 ph31 cpd2:f2 cpd3:f3
30m do:f2 do:f3 mc #0 to 2 F0(zd)
d11 H2_LOCK
d11 LOCKH_OFF
d11 LOCKDEC_OFF
exit
ph1=0 2 2 0 1 3 3 1
ph31=0 2 2 0 1 3 3 1
;pl1 : f1 channel - power level for pulse (default)
;pl12: f2 channel - power level for CPD/BB decoupling
;p1 : f1 channel - high power pulse
;d1 : relaxation delay; 1-5 * T1
;d11: delay for disk I/O [30 msec]
;d12: delay for power switching [20 usec]
;NS: 1 * n, total number of scans: NS * TD0
;cpd2: decoupling according to sequence defined by cpdprg2
;pcpd2: f2 channel - 90 degree pulse for decoupling sequence
;$Id: zgig2h,v 1.10 2007/04/11 13:34:31 ber Exp $
Hi,
We were recently asked if we could acquire some 13C{1H,2H} spectra. By searching about this topic, I found this page. Indeed, 2 LF channels and appropriate probe would be the best option. But unfortunately not available.
We have a Bruker Avance DPX at our lab, equipped with a two channel probe (X/1H) and a 2H lockswitch.
I was looking for a sequence able to use that lockswitch to switch from lock for field stability to 2H (homo or bb)decoupling during the sequence. The sequence zgig2h use f3 which is not defined with our dual probe. I would indeed be able to use the lock channel for this f3.
I was wondering if you have any clue on the possibility to perform such acquisitions with our setup? I've seen this manual : https://2210pc.chem.uic.edu/nmr/downloads/BASHCD10/pdf/z31491.pdf.
It describes a zgdc_2h sequence for Avance (not DPX) and AMX but still using a f3 channel on the avance version. So not convinced of the feasability.
Any help or comment that you could give would be welcome.
Thanks a lot!
Laurent,
The data were collected on an AVANCE I console with the pulse program listed in the comments for this post 15 years ago. I have now been retired for 4 years so no longer have access the information I would need to help you. I would suggest that you modify the pulse program in the comments so that it would work on your older DPX instrument. Sorry I couldn’t be of any more help. Good luck.
Glenn
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