Presaturated QCPMG pulse program for topSpin2.1 operating system




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Carr-Purcell-Meiboom-Gill echo train


*** Outline ***


Code for Avance III spectrometers with topSpin2.1 operating system

; qcpmgpresat.fau (TopSpin 2.0)
; AVANCE III
; FAU, 09/05/2007
; written by Stefan Steuernagel
; use rotor-synchronized CPMG train of refocusing pulses to create the echoes

; pulse program for presaturated quadrupolar CPMG sequence
; samples continuously, including ALL pulses and ringdown delays
; may be used with digmod digital
; important: only runs via SGU in channel 1

;parameters:
;ns : 16 * n
;d1 : recycle delay
;d20 : delay between saturation pulses

;d3 : time to allow pulse ringdown, 10 to 100 us
;d6 : enter duration of FID

;pl1  : f1 power level for presaturation pulses 
;pl21 : RF power level
;pl22 : =pl21 usually, =120 dB if 180° pulses are not desired

;p1 : presaturation pulses at power pl1
;p3 : 90 degree pulse
;p4 : 180 degree pulse
;p25 : dummy pulse, used for showing cnst1 in ased
;l20 : # of pulses in saturation pulse train, 0 if undesired
;l22 : # of echos to be acquired
;cnst1 : set td to number of acquired complex data points
;cnst31 : spinning speed
;zgoptns :-Dpresat or blank

;$COMMENT=presaturated quadrupolar CPMG sequence, samples continuously, pulses blanked out, requires DRU
;$CLASS=Solids
;$DIM=1D
;$TYPE=half integer quadrupoles
;$SUBTYPE=simple 1D
;$OWNER=fabien

#include <Avancesolids.incl>

  "p4=p3*2"
  "cnst1=((d6*2+d3*2+p4)*l22+d6+d3)/dw"
  "p25=cnst1"

define delay rest
  "rest=aq-(cnst1*dw)"
  "d31=1s/cnst31"

;cnst11 : to adjust t=0 for acquisition, if digmod = baseopt
"acqt0=1u*cnst11"

1 ze                   ;clear data

2 d31

#ifdef presat                  ;set with -Dpresat
pres, d20                      ;delay between saturation pulses
  (p1 pl1 ph10):f1             ;saturation loop if required
  lo to pres times l20
#endif /* presat */

  d1                   ;relaxation delay
  STARTADC
  RESETPHASE
  (p3 pl21 ph1):f1
  d3
  (p4 ph2):f1
  d3 DWL_CLK_ON        ;start acquisition

3 d6 RG_ON
  0.1u RG_OFF
  d3
  (p4 pl22 ph3):f1
  d3
  d6 RG_ON
  lo to 3 times l22    ;next echo

  d6
  d3
  rest RG_OFF
  0.1u DWL_CLK_OFF     ;stop acquisition
  rcyc=2               ;next scan
  10m wr #0            ;save data
exit

;two coherence transfert pathways are selected:
;0Q -> (+1Q, -1Q) -> (-1Q, +1Q) -> ... -> -1Q
ph0=0 
ph10=0                 ;for saturation pulse
ph1=0 2
ph2=1 1 3 3
ph3=1 1 1 1 3 3 3 3
ph30=0
ph31=2 0

;one coherence transfert pathway is selected depending
;on the number L22 of observed echos:
;either 0Q -> +1Q -> -1Q -> ... -> -1Q     if L22 is even
;or     0Q -> -1Q -> +1Q -> ... -> -1Q     if L22 is odd
;ph0=0
;ph10=0                ;for saturation pulse
;ph1=0 1 2 3
;ph2=1 0 1 0 3 2 3 2 1 0 1 0 3 2 3 2
;ph3=1 0 1 0 3 2 3 2 3 2 3 2 1 0 1 0
;ph30=0
;ph31=2 3 0 1
  

Example1: 29Si in LZY-64 zeolite with AV500

Silicon-29 parameter optimization in LZY64 zeolite acquired with zgsat pulse program

Presaturated 29Si one-pulse duration p1 optimization of LZY64 zeolite in 4-mm diameter rotor spinning at 10 kHz, recycle delay D1 = 10 sec, NS = 32.


Acquisition parameters:

General  
PULPROG zgsat.ppm
TD 2048
NS 32
DS 0
SWH [Hz] 34722.22
AQ [s] 0.0295556
RG 912
DW [µs] 14.400
DE [µs] 6.50
D1 [s] 10.00000000
D20 [s] 0.10000000
L20 20
TD0 1
Channel f1  
NUC1 29Si
P1 [µs] 8.00
P20 [µs] 6.50
PL1 [dB] 6
SFO1 [MHz] 99.3581293

Silicon-29 parameter optimization in LZY64 zeolite acquired with zg pulse program

29Si one-pulse duration p1 optimization of LZY64 zeolite in 4-mm diameter rotor spinning at 10 kHz, recycle delay D1 = 10 sec, NS = 32.


Acquisition parameters:

General  
PULPROG zg
TD 2048
NS 32
DS 0
SWH [Hz] 34722.22
AQ [s] 0.0295556
RG 912
DW [µs] 14.400
DE [µs] 6.50
D1 [s] 10.00000000
TD0 1
Channel f1  
NUC1 29Si
P1 [µs] 4.00
PL1 [dB] 6.00
SFO1 [MHz] 99.3581293

Presaturated silicon-29 echo train in LZY64 zeolite acquired with qcpmgpresat.fau pulse program

Presaturated 29Si qcpmg echo train of LZY-64 zeolite in 4-mm diameter rotor spinning at 10 kHz, recycle delay D1 = 10 sec, p3 = 6.5 µsec, p4 = 13 µsec, NS = 1800, L22 = 41.


Acquisition parameters:

General  
PULPROG qcpmgpresat.fau
TD 23200
NS 1800
DS 0
SWH [Hz] 34722.22
AQ [s] 0.3341444
RG 912
DW [µs] 14.400
DE [µs] 6.50
const1 23150.210938
CONST11 0.0000000
CONST31 10000.0000000
D1 [s] 10.00000000
D3 [s] 0.00001000
D6 [s] 0.00400000
D20 [s] 0.10000000
L20 20
L22 41
P25 [µs] 0.00
ZGOPTNS -Dpresat
rest [s] 0.00078138
Channel f1  
NUC1 29Si
P1 [µs] 6.50
P3 [µs] 6.50
P4 [µs] 13.00
PL1 [dB] 6.00
PL21 [dB] 6.00
PL22 [dB] 6.00
SFO1 [MHz] 99.3581293

Silicon-29 echo train in LZY64 zeolite acquired with qcpmg.fau pulse program

29Si qcpmg echo train of LZY-64 zeolite in 4-mm diameter rotor spinning at 10 kHz, recycle delay D1 = 10 sec, p3 = 3 µsec, p4 = 13 µsec, NS = 1800, L22 = 41.


Acquisition parameters:

General  
PULPROG qcpmg.fau
TD 23200
NS 1800
DS 0
SWH [Hz] 34722.22
AQ [s] 0.3341444
RG 912
DW [µs] 14.400
DE [µs] 6.50
const1 23150.210938
CONST11 0.0000000
D1 [s] 10.00000000
D3 [s] 0.00001000
D6 [s] 0.00400000
L22 41
P25 [µs] 0.00
rest [s] 0.00078138
Channel f1  
NUC1 29Si
P3 [µs] 3.00
P4 [µs] 13.00
PL1 [dB] 120.00
PL21 [dB] 6.00
PL22 [dB] 6.00
SFO1 [MHz] 99.3581293

Silicon-29 FID in LZY64 zeolite acquired with zg pulse program

29Si one-pulse FID of LZY64 zeolite in 4-mm diameter rotor spinning at 10 kHz, recycle delay D1 = 10 sec, p1 = 3 µsec, NS = 1800.


Acquisition parameters:

General  
PULPROG zg
TD 2048
NS 1800
DS 0
SWH [Hz] 34722.22
AQ [s] 0.0295556
RG 912
DW [µs] 14.400
DE [µs] 6.50
D1 [s] 10.00000000
TD0 1
Channel f1  
NUC1 29Si
P1 [µs] 3.00
PL1 [dB] 6.00
SFO1 [MHz] 99.3581293

References

  1. Alan W. MacGregor, Luke A. O’Dell, and Robert W. Schurko
    New methods for the acquisition of ultra-wideline solid-state NMR spectra of spin-1/2 nuclides, (119Sn, 195Pt, 199Hg, 207Pb, WURST-CPMG)
    J. Magn. Reson. 208, 103-113 (2011).
    Abstract
     
  2. Ivan Hung and Zhehong Gan
    On the practical aspects of recording wideline QCPMG NMR spectra,
    J. Magn. Reson. 204, 256-265 (2010).
    Abstract
     
  3. Vladimir I. Bakhmutov
    On Hahn-echo measurements of short 29Si T2 times in some silica-based materials
    Solid State Nucl. Magn. Reson. 36, 164-166 (2009).
    Abstract
     
  4. W. J. Malfait and W. E. Halter
    Increased 29Si NMR sensitivity in glasses with a Carr-Purcell-Meiboom-Gill echotrain
    J. Non-Cryst. Solids 354, 4107-4114 (2008).
    Abstract
     
  5. J. W. Wiench, V. S.-Y. Lin, and M. Pruski
    29Si NMR in solid state with CPMG acquisition under MAS
    J. Magn. Reson. 193, 233-242 (2008).
    Abstract
     
  6. Julien Trebosc, Jerzy W. Wiench, Seong Huh, Victor S.-Y. Lin, and Marek Pruski
    Studies of organically functionalized mesoporous silicas using heteronuclear solid-state correlation NMR spectroscopy under fast magic angle spinning
    J. Am. Chem. Soc. 127, 7587-7593 (2005).
    Abstract
     
  7. Dimitris Sakellariou, Jacques-François Jacquinot, and Thibault Charpentier
    2D correlation spectra of isotropic and anisotropic 29Si chemical shifts in crystalline and amorphous natural abundance materials under very slow sample rotation
    Chem. Phys. Lett. 411, 171-174 (2005).
    Abstract
     
  8. Jian Zhi Hu and Robert A. Wind
    Sensitivity-enhanced phase-corrected ultra-slow magic angle turning using multiple-echo data acquisition
    J. Magn. Reson. 163, 149-162 (2003).
    Abstract
     
  9. Flemming H. Larsen and Ian Farnan
    29Si and 17O (Q)CPMG-MAS solid-state NMR experiments as an optimum approach for half-integer nuclei having long T1 relaxation times
    Chem. Phys. Lett. 357, 403-408 (2002).
     
  10. Andrew S. Lipton, Jesse A. Sears, and Paul D. Ellis
    A general strategy for the NMR observation of half-integer quadrupolar nuclei in dilute environments
    J. Magn. Reson. 151, 48-59 (2001).
    Abstract
     
  11. H. Y. Carr and E. M. Purcell
    Effects of diffusion on free precession in nuclear magnetic resonance experiments
    Phys. Rev. 94, 630-638 (1954).
    PDF file (2.2 MB)
     

  1. D. Li, A. E. Dementyev, M. Liu, and S. E. Barrett
    NMR studies of spin decoherence in phosphorus-doped silicon
    PDF file (600 kB)
     
  2. B. Blümich
    Introduction to mobile NMR
    PDF file (4.5 MB)
     

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[Contact me] - Last updated Last updated December 16, 2012
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