;purest_t1_irmf_wvm ; ; Pure shift T1-relaxation encoded selective TOCSY (PUREST1) ; measurement using inversion recovery ; All shape pulses wavemaker compatible ; multiple frequency selectivity ; DIPSI-2 with ZQF. Option between ZS and PSYCHE Pure shift ; ; University of Manchester ; Manchester NMR methodology group ; https://www.nmr.chemistry.manchester.ac.uk/ ; ; Mathias Nilsson ; Mathias.Nilsson@manchester.ac.uk ; ; Marshall Smith ; marshall.smith@manchester.ac.uk ;University of Manchester ; Marshall Smith ; marshall.smith@manchester.ac.uk ; ; ;Avance II+/III Version ;Topspin 4.x ; ;$CLASS=HighRes ;$DIM=3D ;$TYPE= ;$SUBTYPE= ;$COMMENT= ;Pure shift 3D broad-band experiment ; with interferogram acquisition ; ZGOPTION= -DZS (Zangger-Sterk) ; ZGOPTION= -DdSALTIRE (PSYCHE on) ; ; "wvm -a" command to generate pulse shapes with wavemaker #include #include #include define delay tauA define delay tauB ;PULSES "p2=p1*2" "p3=p1" "p18=1m" "p19=1m" ;"p11=p50" ; Selective TOCSY "FACTOR1=(d9/(p6*115.112))/2" "l1=FACTOR1*2" ;DELAYS "in0=inf1/2" "d0=0" "tauA=in0/2-p18-d18-50u" "tauB=dw*2*cnst4" "d18=1m" "d19=1m" "d11=30m" "d11=30m+1s/(cnst12)-1s/(cnst12)" "d11=30m+1s/(cnst13)-1s/(cnst13)" "d11=30m+1s/(cnst41)-1s/(cnst41)" "d11=30m" ;OFFSETS "spoff22=0" "spoff32=0" "spoff34=0" "cnst30=0" # ifdef ZS "d11=30m+1s/(cnst42)-1s/(cnst42)" # endif # ifdef dSALTIRE "d11=30m+1s/(1+cnst48)" "d11=30m+1s/(1+cnst50)" "d11=30m+1s/(1+cnst51)" "p50=cnst51*1000.0" "spw50=plw1/(((1000000.0/(((cnst48/360)*sqrt((2*cnst50*1000)/(p50/1000000)))*4))/p1)*((1000000.0/(((cnst48/360)*sqrt((2*cnst50*1000)/(p50/1000000)))*4))/p1))" # endif ;Acquistion "acqt0=0" baseopt_echo 1 ze 2 d11 pl1:f1 10u UNBLKGRAMP p8 ph21 p8 ph22 p18:gp8*-1 d18 BLKGRAMP 50u BLKGRAD 50u LOCKH_OFF d1 pl1:f1 50u LOCKH_ON 50u UNBLKGRAD ; T1 inversion recovery p2 ph1 vd p1 ph2 ; Selective TOCSY p16:gp1 d16 pl0:f1 p12:sp12:f1 ph3 ;selective 180r p16:gp1 d16 pl1:f1 3 p1 ph4 20u gron0 (p32:sp32 ph5):f1 20u groff 200u pl10:f1 ;begin DIPSI2 4 p6*3.556 ph23 p6*4.556 ph25 p6*3.222 ph23 p6*3.167 ph25 p6*0.333 ph23 p6*2.722 ph25 p6*4.167 ph23 p6*2.944 ph25 p6*4.111 ph23 p6*3.556 ph25 p6*4.556 ph23 p6*3.222 ph25 p6*3.167 ph23 p6*0.333 ph25 p6*2.722 ph23 p6*4.167 ph25 p6*2.944 ph23 p6*4.111 ph25 p6*3.556 ph25 p6*4.556 ph23 p6*3.222 ph25 p6*3.167 ph23 p6*0.333 ph25 p6*2.722 ph23 p6*4.167 ph25 p6*2.944 ph23 p6*4.111 ph25 p6*3.556 ph23 p6*4.556 ph25 p6*3.222 ph23 p6*3.167 ph25 p6*0.333 ph23 p6*2.722 ph25 p6*4.167 ph23 p6*2.944 ph25 p6*4.111 ph23 lo to 4 times l1 ;end DIPSI2 5 p17:gp2 d17 pl0:f1 100u gron10 (p34:sp34 ph5):f1 ;Zero Quantum Filter 100u groff d17 pl1:f1 p1 ph6 ; Pure shift J refocussing 6 d0 tauA 50u p18:gp3 d18 p2 ph7 p18:gp3 d18 50u tauA tauB ; Delay for drop points 50u d19 pl0:f1 p19:gp4 d19 # ifdef ZS 10u gron20 ;spatial encoding (p22:sp22 ph8):f1 10u groff ;spatial encoding # endif # ifdef dSALTIRE 10u ( center (p50:sp50 ph8):f1 (p11:gp11) ) 10u # endif d19 p19:gp4 d19 50u BLKGRAMP d0 go=2 ph31 d11 mc #0 to 2 F1QF(id0) F2QF(ivd) exit 50u LOCKH_OFF ph1= 0 0 0 0 2 2 2 2 ph2= 0 0 0 0 0 0 0 0 2 2 2 2 2 2 2 2 ph3= 0 1 2 3 ph4= 0 ph6= 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 ph5= 0 ph7=0 ph8=0 ph9=0 ph21=0 ph22=1 ph23=3 ph25=1 ph29=0 ph31= 0 2 0 2 0 2 0 2 2 0 2 0 2 0 2 0 1 3 1 3 1 3 1 3 3 1 3 1 3 1 3 1 ;POWER LEVEL ;pl0 : zero power (0W) ;pl1 : power level for pulse (default) ;pl10 : power level for TOCSY-spinlock ;sp12 : power level of refocusing shaped pulse ;sp22 : power level of ZS ASR pulse ;sp32 : power level of adiabatic pulse of first ZQF element ;sp34 : power level of adiabatic pulse of last ZQF element ;sp50: calculated power level of the PSYCHE pulse [35-60 dB] ;PULSE DURATION ;p1 : 90 degree high power pulse ;p2 : 180 degree high power pulse ;p6 : 90 degree low power pulse ;p8 : Saturation recovery pulse [1-1.5 msec] ;p12 : 180 degree refocusing shaped pulse ; choose p12 according to desired selectivity ;p22 : 180 degree refocusing shaped pulse in ZS element ;p32 : first ZQF 180 degree inversion shaped pulse (adiabatic) [10 msec] ;p34 : second ZQF 180 degree inversion shaped pulse (adiabatic) [30 msec] ;p50 : Length of SALTIRE pulse [25-70 ms] ;GRADIENT DURATION ;p11 : duration of gradient pulse under SALTIRE pulse [=p50] ;p16 : duration of CTP gradients for Selective pulse [1 msec] ;p17 : duration of CTP gradients for z-TOCSY [1 msec] ;p18 : saturation recovery gradient pulse [1 msec] ;p19 : duration of CTP gradients for ZS selective pulse [1 msec] ;DELAY ;d1 : relaxation delay; [2-10 s] ;d9 : TOCSY mixing time [50-200 ms] ;d11 : delay for disk I/O [30 ms] ;d16 : recovery delay for gradients of selective pulse CTP [1 ms] ;d17 : selective spin-echo delay in selective-TOCSY block [200 us] ;d18 : recovery delay for saturation gradients [1ms] ;d19 : recovery delay for CTP gradients for ZS selective pulse [1 ms] ;PULSE SHAPE ;spnam12 : file name for the selective 180 refocusing shaped pulse for selective TOCSY [RSNOB or REBURP] ;spnam22 : file name for the selective 180 refocusing shaped pulse PS [RSNOB or REBURP] ;spnam32 : file name for the adiabatic shaped pulse using in first ZQF [CHIRP] ; smoothed chirp (low to high, 20% smoothing, 1000 points, 20KHz) ;spnam34 : file name for the adiabatic shaped pulse using in last ZQF [CHIRP] ; smoothed chirp (low to high, 20% smoothing, 1000 points, 20KHz) ;GRADIENT SHAPE ;gpnam1 : SMSQ10.100 ;gpnam2 : SMSQ10.100 ;gpnam3 : SMSQ10.100 ;gpnam4 : SMSQ10.100 ;gpnam8 : SMSQ10.100 ;gpnam11: RECT.1 ;GRADIENT STRENGTH ;gpz0 : first ZQF gradient [3%] ;gpz1 : CTP gradient [13 or 23%] ;gpz2 : homospoil gradient [37%] ;gpz3 : saturation recovery gradient [47%] ;gpz4 : saturation recovery gradient [63%] ;gpz8 : saturation recovery gradient [31%] ;gpz10: last ZQF gradient [4%] ;gpz11: gradient under SALTIRE pulse [1-3%] ;gpz20: z-encoding gradient in ZS element [0-1%] ;CONSTANTS ;cnst4 : Number of drop points [4] ;cnst12: chemical shift for first frequency of selective pulse (offset, in ppm) ;cnst13: chemical shift for second frequency of selective pulse (offset, in ppm) ;cnst22: chemical shift for selective pulse (offset, in ppm) ;cnst41: Bandwidth for selective pulse (Hz) ;cnst42: Bandwidth for ASR selective pulse (Hz) ;cnst48: beta flip angle of the PSYCHE pulse [20] ;cnst50: sweep-width of the PSYCHE pulse [10 kHz] ;cnst51: duration of the PSYCHE pulse [30 ms] ;;;; WAVEMAKER ;;;; ;sp12:wvm:mjs_multi_rsnob:f1 rsnob(cnst41 Hz, cnst12 ppm; NPOINTS=1000; PA=0.5; PHI=0;) ;sp22:wvm:mjs_asr_rsnob:f1 rsnob(cnst42 Hz; NPOINTS=1000; PA=0.5; PHI=0;) ;sp32(p32):wvm:mjs_ZQS1:f1 wurst-80(20 kHz, 10 ms; NPOINTS=10000, L2H, Q=11) ss=5.0us; ;sp34(p34):wvm:mjs_ZQS2:f1 wurst-80(20 kHz, 30 ms; NPOINTS=10000, L2H, Q=11) ss=5.0us; ;sp50(p50):wvm:mjs_psyche:f1 cawurst-40(cnst50 kHz, cnst51 ms; L2H) cawurst-40(cnst50 kHz, cnst51 ms; H2L) ss=2.0us ;OTHER ;ZGOPTNS : -DZS (Zangger-Sterk), -DdSALTIRE (PSYCHE on) ;td1 : number of delays in VDLIST ;vd : variable delay, taken from vd-list ;define VDLIST ;this pulse program produces a ser-file (PARMOD = 3D) ;in0 : 1/(2 * SW) = DW ;nd0 : 2 ;NS: 16 * n, total number of scans: NS * TD0 ;DS: 16