z-filter 3QMAS pulse program for spins 3/2, 5/2, and 7/2
Contributor: Y. Millot




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Below NMR pulse program describes the z-filter 3QMAS (1D and 2D) experiment with cogwheel phase cycling or nested phase cycling applied to nuclei with 3/2, 5/2, or 7/2 spins.

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.

This NMR pulse program is for Bruker Avance spectrometers.

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

Code for Avance NMR spectrometers

; 3qzfilter.ym (XWIN-NMR 3.0)
; 01072009

;3Q MAS pulse program for half integer spin nuclei
;ZGOPTNS (zg-options) are:
;  -DTQS3Cog ... used with I=3/2 (ns=24)  Cog24(0,4,19,7)  = Cog24(23,3,18,6)
;  -DTQS3Nes ... used with I=3/2 (ns=24)  nested phase cycling with standard receiver
;  -DTQS5Cog ... used with I=5/2 (ns=36)  Cog36(0,6,29,11) = Cog36(34,4,27,9)
;  -DTQS5Nes ... used with I=5/2 (ns=36)  nested phase cycling with standard receiver
;  -DTQS7Cog ... used with I=7/2 (ns=48)  Cog48(0,8,25,1)  = Cog48(11,19,36,12)
;  -DTQS7Nesdig .used with I=7/2 (ns=48)  nested phase cycling with digital receiver

;d1 : recycle delay
;p1 : excitation pulse at pl11
;p2 : conversion pulse at pl11
;p3 : 90 degree selective pulse at pl13
;pl1 : =120 dB
;pl11 : power level for excitation and conversion pulses
;pl13 : power level for selective pulse
;d4 : =20u, delay for z-filter 
;d0 : =3u
;in0 : 1 rotation period for synchronised experiment
;td1 : number of t1-experiments
;FnMODE : States or TPPI
;Shearing use AU program xfshear (FnMode = States) 
;ph30 ph31:r for receiver phase <> kpi/2

  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  pl13:f1          ; set low power in f1 channel,
  (p3 ph3):f1          ; low-power 90 pulse,
#ifdef TQS7Nesdig
  go=1 ph30 ph31:r     ; instruction must be in that order
                       ; signal acquisition,
                       ; loop to 1, ns times for averaging,
#else
  go=1 ph31            ; signal acquisition,
                       ; loop to 1, ns times for averaging,
#endif
  d1 mc #0 to 1 F1PH(ip1, id0)
                       ; delay for disk I/O, store signal,
                       ; increase FID number,
                       ; delete memory data,
                       ; increment p1 pulse phase by 360/12 
                       ; for States procedure,
                       ; increment time d0 by in0,
  exit                 ; end of the pulse program

#ifdef TQS3Cog 
 ph10= (24) {0 1 2 3 4 5 6 7 8 9 10 11}^12
                       ; a series of integer numbers from 0 to 23
 ph1 = (12)  ph10*23   ; excitation pulse phase
 ph2 =       ph10*3    ; conversion pulse phase
 ph3 =       ph10*18   ; 90 selective pulse phase
 ph31=       ph10*6    ; receiver phase :(360/24)*6*m=90*m
#else
#ifdef TQS3Nes 
 ph1 = (12)  0 2 4 6 8 10
 ph2 =       0
 ph3 =     {{0}*6}^1^2^3
 ph31=       ph1*3 + ph3
#else 
#ifdef TQS5Cog 
 ph10= (36) {0 1 2 3 4 5 6 7 8 9 10 11}^12^24
                       ; a series of integer numbers from 0 to 35
 ph1 = (12)  ph10*34   ; excitation pulse phase
 ph2 =       ph10*4    ; conversion pulse phase
 ph3 =       ph10*27   ; 90 selective pulse phase
 ph31=       ph10*9    ; receiver phase :(360/36)*9*m=90*m
#else
#ifdef TQS5Nes 
 ph1 = (12)  0 2 4 6 8 10
 ph2 = (6) {{0}*6}^1^2^3^4^5
 ph3 =       0
 ph31=       ph1*3 - ph2*3
#else 
#ifdef TQS7Cog 
 ph10= (48) {0 1 2 3 4 5 6 7 8 9 10 11}^12^24^36
                       ; a series of integer numbers from 0 to 47
 ph1 = (12)  ph10*11   ; excitation pulse phase
 ph2 =       ph10*19   ; conversion pulse phase
 ph3 =       ph10*36   ; 90 selective pulse phase
 ph31=       ph10*12   ; receiver phase :(360/48)*12*m=90*m
#else
#ifdef TQS7Nesdig 
 ph1 = (12)  0 2 4 6 8 10
 ph2 =       0
 ph3 = (8) {{0}*6}^1^2^3^4^5^6^7
 ph30=       ph1*3 + ph3
 ph31=       0
#endif
#endif
#endif
#endif
#endif
#endif
  

This pulse program remains valid for the third pulse with strong amplitude for better excitation of off-resonance nuclei.

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