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 ... for I=9/2 (ns=180) cog180(0,10,1,91) = cog180(134,144,135,45) ; -DNQS9Nesdig for I=9/2 (ns=180) nested phase cycling with digital receiver ; -DNQS9Nes .. for 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 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60 61 62 63 64 65 66 67 68 69 70 71 72 73 74 75 76 77 78 79 80 81 82 83 84 85 86 87 88 89 90 91 92 93 94 95 96 97 98 99 100 101 102 103 104 105 106 107 108 109 110 111 112 113 114 115 116 117 118 119 120 121 122 123 124 125 126 127 128 129 130 131 132 133 134 135 136 137 138 139 140 141 142 143 144 145 146 147 148 149 150 151 152 153 154 155 156 157 158 159 160 161 162 163 164 165 166 167 168 169 170 171 172 173 174 175 176 177 178 179 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}*18 {2}*18 {3}*18 {4}*18 {5}*18 {6}*18 {7}*18 {8}*18 {9}*18 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}*18 {2}*18 {3}*18 {4}*18 {5}*18 {6}*18 {7}*18 {8}*18 {9}*18 {10}*18 {11}*18 {12}*18 {13}*18 {14}*18 {15}*18 {16}*18 {17}*18 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.