Z-filter pulse program from Bruker for 3QMAS of half-integer spin quadrupole nuclei




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Below NMR pulse program describes the z-filter approach for (1D and 2D) +3Q-MAS experiment applied to quadrupolar nuclei with half-integer spin.

Z-filter 3QMAS sequence and coherence transfer pathway for a spin I = 3/2

Fig. 1: Z-filter 3QMAS NMR pulse sequence and coherence transfer pathway.
The echo amplitude and the antiecho amplitude have the same sign.
The phase cyling for 3 strong pulses is discussed.

This NMR pulse program is for Bruker Avance spectrometers.

A pure absorption 2D spectrum is obtained with the shearing transformation.

Code for Avance III spectrometers

; mp3qzqf

; 3Q MAS pulse program for half-integer spin nuclei 
; 3-pulse experiment with zero quantum filter: 
; excitation(3Q) - conversion(0Q) - tau - 90 selective - ACQ(-1Q) 
; 90 selective pulse should be determined first using Hahn-echo, 
; determination by single pulse excitation is also possible 
; Then optimise P2 and finally P1, 2 or more iterations for P1 and P2 
; may be needed.
; For processing shearing transformation may be requested,
; use AU program xfshear

;ns :  12*n
;d1 :  recycle delay
;p1 :  excitation pulse at pl11
;p2 :  conversion pulse at pl11
;p3 :  90 degree selective pulse at pl21
;pl1 :  = 120 db
;pl11 : power level for excitation and conversion pulses
;pl21 : power level for 180 degree selective pulse, ca. pl11 + 30 db
;d4 :  z-filter delay
;d0  : = 1u or longer
;in0 : 1 rotor period for synchronised experiment
;td1 : number of t1-experiments
;FnMODE : States
;MC2 : States

  ze                  ; clear memory, new data replace old data,
                      ; switch AD converter to replace mode,
                      ; perform DS before next acquisition,
1 d1                  ; recycle delay,
  10u pl11:f1         ; 10 microsecond delay,
                      ; set high power in f1 channel,
  (p1 ph1):f1         ; high-power excitation pulse,
  d0                  ; delay between pulses, t1 increment,
  (p2 ph2):f1         ; high-power conversion pulse,
  d4 pl21:f1          ; set low power in f1 channel,
  (p3 ph3):f1         ; low-power 90 pulse,
  go=1 ph31           ; signal acquisition,
                      ; loop to 1, ns times for averaging,
  d1 mc #0 to 1 F1PH(ip1, id0)
                      ; delay for disk I/O, store signal,
                      ; increase FID number,
                      ; delete memory data,
                      ; do not perform dummy scans
                      ; with next acquisition,
                      ; increment p1 pulse phase by 360/12 for States procedure,
                        ; loop to 1, 1 time for States procedure,
                      ; increment time d0 by in0,
                        ; loop to 1, td1/2 time for 2D experiment
  exit                ; end of the pulse program

ph1=(12) 0                        ; excitation pulse phase
ph2=(6)  0 0 1 1 2 2 3 3 4 4 5 5  ; conversion pulse phase
ph3=     0 2                      ; 90 selective pulse phase
ph0=     0
ph31=    0 2 2 0                  ; receiver phase
  

If the third pulse must be a strong RF pulse for better excitation of off-resonance nuclei, the phase cyclings of ph1, ph2, ph3, and ph31 should be the following for spin I = 3/2. However, there is no harm in applying these phase cyclings concerning 3-strong pulse sequence even when the third pulse is a weak RF pulse.

; ns: 24*n
; pl21 = pl11
ph1=(12) 0 2 4 6 8 10               ; excitation pulse phase
ph2=     0                          ; conversion pulse phase
ph3=(4)  0 0 0 0 0 0  1 1 1 1 1 1 
         2 2 2 2 2 2  3 3 3 3 3 3   ; 90 pulse phase
ph0=     0
ph31=    0 2 0 2 0 2  1 3 1 3 1 3 
         2 0 2 0 2 0  3 1 3 1 3 1   ; receiver phase
  

Example: LZY-84 zeolite

90 pulse duration of 27Al in solution with zg

27Al spectra of reference solution versus the excitation pulse p1 duration (pl1 = 0.5 dB) in zg pulse program, acquired with a 4-mm diameter rotor, D1 = 1 sec recycle delay, and recorded with Bruker Avance III, 500 MHz WB US magnet.

90 pulse duration of 27Al in solution with zg with low power

27Al spectra of reference solution versus the excitation pulse p1 duration (pl1 = 24 dB) in zg pulse program.

Pulseprogram parameters for zg:

General  
PULPROG zg
TD 4604
NS 8
DS 0
SWH [Hz] 20000.00
AQ [s] 0.1151500
RG 128
DW [s] 25.000
DE [s] 6.50
D1 [s] 1.00000000
TD0 1
Channel f1  
NUC1 27Al
P1 [s] 3.50
PL1 [dB] 0.50
PL1W [W] 234.39410400
SFO1 [MHz] 130.3270545


27Al FID of LZY84 zeolite

27Al MAS FID of LZY-84 zeolite, acquired with a 4-mm diameter rotor spinning at 15 kHz, D1 = 0.2 sec recycle delay, and recorded with Bruker Avance III, 500 MHz.

27Al spectrum of LZY84 zeolite

27Al MAS spectrum of LZY-84 zeolite, acquired with a 4-mm diameter rotor spinning at 15 kHz, D1 = 0.2 sec recycle delay, and recorded with Bruker Avance III, 500 MHz.

Pulseprogram parameters for zg:

General  
PULPROG zg
TD 4604
NS 24
DS 0
SWH [Hz] 50000.00
AQ [s] 0.0460900
RG 64
DW [s] 10.000
DE [s] 6.50
D1 [s] 0.20000000
TD0 1
Channel f1  
NUC1 27Al
P1 [s] 2.00
PL1 [dB] 0.50
PL1W [W] 234.39410400
SFO1 [MHz] 130.3311212


27Al spectra of LZY84 zeolite versus the excitation pulse p2 duration

27Al MAS spectra of LZY-84 zeolite versus the excitation pulse p2 duration (pl11 = 0.5 dB) in mp3qzqf pulse program, acquired with a 4-mm diameter rotor spinning at 15 kHz, D1 = 0.2 sec recycle delay, and recorded with Bruker Avance III, 500 MHz.

Pulseprogram parameters for mp3qzqf:

General  
PULPROG mp3qzqf
TD 4604
NS 120
DS 0
SWH [Hz] 50000.00
AQ [s] 0.0460900
RG 64
DW [s] 10.000
DE [s] 6.50
CNST11 0.0000000
D0 [s] 0.00000300
D1 [s] 0.20000000
D4 0.00002000
Channel f1  
NUC1 27Al
P1 [s] 5.00
P2 [s] 2.00
P3 [s] 16.00
PL1 [dB] 120
PL1W [W] 0.00000000
PL11 [dB] 0.50
PL11W [W] 234.39410400
PL21 [dB] 18.00
PL21W [W] 4.16818190
SFO1 [MHz] 130.3311212


27Al spectra of LZY84 zeolite versus the excitation pulse p1 duration

27Al MAS spectra of LZY-84 zeolite versus the excitation pulse p1 duration (pl11 = 0.5 dB) in mp3qzqf pulse program.

Pulseprogram parameters for mp3qzqf:

General  
PULPROG mp3qzqf
TD 4604
NS 120
DS 0
SWH [Hz] 50000.00
AQ [s] 0.0460900
RG 64
DW [s] 10.000
DE [s] 6.50
CNST11 0.0000000
D0 [s] 0.00000300
D1 [s] 0.20000000
D4 0.00002000
Channel f1  
NUC1 27Al
P1 [s] 6.00
P2 [s] 2.00
P3 [s] 16.00
PL1 [dB] 120
PL1W [W] 0.00000000
PL11 [dB] 0.50
PL11W [W] 234.39410400
PL21 [dB] 18.00
PL21W [W] 4.16818190
SFO1 [MHz] 130.3311212


27Al spectra of LZY84 zeolite versus the excitation pulse p3 duration

27Al MAS spectra of LZY-84 zeolite versus the excitation pulse p3 duration (pl21 = 24 dB) in mp3qzqf pulse program.

Pulseprogram parameters for mp3qzqf:

General  
PULPROG mp3qzqf
TD 4604
NS 120
DS 0
SWH [Hz] 50000.00
AQ [s] 0.0460900
RG 64
DW [s] 10.000
DE [s] 6.50
CNST11 0.0000000
D0 [s] 0.00000300
D1 [s] 0.20000000
D4 0.00002000
Channel f1  
NUC1 27Al
P1 [s] 6.00
P2 [s] 2.00
P3 [s] 18.00
PL1 [dB] 120
PL1W [W] 0.00000000
PL11 [dB] 0.50
PL11W [W] 234.39410400
PL21 [dB] 24.00
PL21W [W] 1.04700005
SFO1 [MHz] 130.3311212


27Al 3QMAS FID of LZY84 zeolite

27Al 3QMAS series of FID of LZY-84 zeolite acquired with a 4-mm diameter rotor spinning at 15 kHz, D1 = 0.2 sec recycle delay, and recorded with Bruker Avance III, 500 MHz.

27Al 3QMAS spectrum of LZY84 zeolite

Xfsheared 27Al 3QMAS spectrum of LZY-84 zeolite acquired with a 4-mm diameter rotor spinning at 15 kHz, D1 = 0.2 sec recycle delay, and recorded with Bruker Avance III, 500 MHz.

27Al 3QMAS spectrum of LZY84 zeolite

Zoomed 27Al 3QMAS spectrum of LZY-84 zeolite.

Pulseprogram parameters for mp3qzqf:

General  
PULPROG mp3qzqf
TD 4604
NS 120
DS 0
SWH [Hz] 50000.00
AQ [s] 0.0460900
RG 64
DW [s] 10.000
DE [s] 6.50
CNST11 0.0000000
D0 [s] 0.00000300
D1 [s] 0.20000000
D4 0.00002000
IN0 [s] 0.00002000
ST1CNT 128
Channel f1  
NUC1 27Al
P1 [s] 6.00
P2 [s] 2.00
P3 [s] 18.00
PL1 [dB] 120
PL1W [W] 0.00000000
PL11 [dB] 0.50
PL11W [W] 234.39410400
PL21 [dB] 24.00
PL21W [W] 1.04700005
SFO1 [MHz] 130.3311212

Acquisition parameters:

  F2 F1
Experiment    
PULPROG mp3qzqf  
AQ_mod DQD  
FnMODE   States
TD 4608 256
NS 128  
DS 0  
TD0 1  
Width    
SW [ppm] 383.6382 383.6382
SWH [Hz] 50000.000 50000.000
IN_F [µs]   20.00
AQ [s] 0.0460900 0.0025600
Nucleus1    
NUC1 27Al  
O1 [Hz] 2529.25 2529.25
O1P [ppm] 19.407 19.407
SFO1 [MHz] 130.3311212 130.3311212
BF1 [MHz] 130.3285920 130.3285920

Processing parameters:

  F2 F1
Reference    
SI 2048 512
SF [MHz] 130.3270970 184.6300540
OFFSET [ppm] 222.70329 166.28419
SR [Hz] -1495.03 -2117.96
Window Function    
WDW EM QSINE
LB [Hz] 20.00 30.00
SSB 0 3
Nucleus1    
Fourier transform    
TDeff 512 160

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