Presaturated QCPMG pulse program for 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

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:

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:

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:

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:

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:

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)

Solid-state NMR bibliography for: