Below NMR pulse program describes the z-filter ±9QMAS (1D and 2D) experiment with cogwheel phase cycling or nested phase cycling applied to nuclei with spin 9/2.
This NMR pulse program is for Bruker Avance spectrometers.
A pure absorption 2D spectrum is obtained with the shearing transformation.
; 9qzfilter.ym (XWIN-NMR 3.0) ; 01072009 ;±9Q MAS pulse program for half integer spin nuclei ;ZGOPTNS (zg-options) are: ; -DNQS9Cog ... used with I=9/2 (ns=180) cog180(0,10,1,91) = cog180(134,144,135,45) ; -DNQS9Nesdig used with I=9/2 (ns=180) nested phase cycling with digital receiver ; -DNQS9Nes .. used with I=9/2 (ns=324) nested phase cycling with standard 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) ;ph31 ph30: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 NQS9Cog go=1 ph31 ; signal acquisition, ; loop to 1, ns times for averaging, #else #ifdef NQS9Nesdig go=1 ph31 ph30:r ; instruction must be in that order ; signal acquisition, ; loop to 1, ns times for averaging, #else #ifdef NQS9Nes go=1 ph31 ; signal acquisition, ; loop to 1, ns times for averaging, #endif #endif #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°/36 ; for States procedure, ; increment time d0 by in0, exit ; end of the pulse program #ifdef NQS9Cog ph10= (180) {0 1 2 3 4 5 6 7 8 9}^10^20^30^40^50^60^70^80^90^100^110^120^130^140^150^160^170 ; a series of integer numbers from 0 to 179 ph1 = (36) ph10*134 ; excitation pulse phase ph2 = ph10*144 ; conversion pulse phase ph3 = ph10*135 ; 90° selective pulse phase ph31= ph10*45 ; receiver phase : (360/180)*45*m=90*m #else #ifdef NQS9Nesdig ph1 = (36) 0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30 32 34 ph2 = 0 ph3 = (10) {{0}*18}^1^2^3^4^5^6^7^8^9 ph30= ph1*9 + ph3 ph31= 0 #else #ifdef NQS9Nes ph1 = (36) 0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30 32 34 ph2 = (18) {{0}*18}^1^2^3^4^5^6^7^8^9^10^11^12^13^14^15^16^17 ph3 = 0 ph31= ph1*9 - ph2*9 #endif #endif #endif
This pulse program remains valid for the third pulse with strong amplitude for better excitation of off-resonance nuclei.