University of Ottawa NMR Facility Web Site

Please feel free to make suggestions for future posts by emailing Glenn Facey.

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.


Alasdair said...

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.


Glenn Facey said...

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

;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





1 ze
d11 pl12:f2 pl13:f3 LOCKDEC_ON
d11 H2_PULSE

2 30m do:f2 do:f3
30m H2_LOCK
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

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 $