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.
Friday, July 23, 2010
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2 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 $
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