; PUREST-T2 ; ; Pure Shift Relaxation Encoded Selective TOCSY (PUREST2) ; Using PROJECT T2 relaxation weighting and PSYCHE J refocussing element ; DIPSI-2 with ZQF ; ; 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 ;Data can be reconstructed using a macro available at http://nmr.chemistry.manchester.ac.uk ;Avance II+/III Version ;Topspin 4.x ; ;$CLASS=HighRes ;$DIM=3D ;$TYPE= ;$SUBTYPE= ;$COMMENT= #include #include #include define delay tauA define delay tauB ;PULSES "p2=p1*2" "p3=p1" "p18=1m" "p19=1m" "p11=p40" "FACTOR1=(d9/(p6*115.112))/2" "l1=FACTOR1*2" ;DELAYS "in0=inf1/2" "d0=0" "d11=30m+1s/(cnst12)-1s/(cnst12)" "d11=30m" "tauA=in0/2-p18-d18-50u" "tauB=dw*2*cnst4" "d18=1m" "d19=1m" "spoff12=bf1*(cnst12/1000000)-o1" "spoff32=0" "spoff34=0" ; Zero Quantum Filter Pulse Calculation "p33=1000000.0/(cnst53*4)" "cnst33= (p33/p1) * (p33/p1)" "spw32=plw1/cnst33" "p35=1000000.0/(cnst54*4)" "cnst35= (p35/p1) * (p35/p1)" "spw34=plw1/cnst35" ; SALTIRE PULSE "cnst50=(cnst20/360)*sqrt((2*cnst21)/(p40/2000000))" "p30=1000000.0/(cnst50*4)" "cnst31= (p30/p1) * (p30/p1)" "spw40=plw1/cnst31" "spoff40=0" ;Acquistion "acqt0=0" baseopt_echo 1 ze 2 30m pl1:f1 10u UNBLKGRAMP p8 ph21 p8 ph22 p15:gp8*-1 d15 BLKGRAMP 50u LOCKH_OFF d1 50u LOCKH_ON 50u UNBLKGRAMP p1 ph1 3 d20 p2 ph2 d20 p3 ph3 d20 p2 ph2 d20 lo to 3 times c 4 p16:gp1 d16 pl0:f1 p12:sp12:f1 ph4 ;selective 180r p16:gp1 d16 pl1:f1 5 p1 ph5 20u gron0 pl0:f1 (p32:sp32 ph6):f1 10u groff 200u pl10:f1 ;begin DIPSI2 6 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 6 times l1 ;end DIPSI2 p17:gp2 500u 10u gron10 pl0:f1 (p34:sp34 ph6):f1 ;Zero Quantum Filter 200u groff 10u pl1:f1 7 p1 ph7 d0 tauA 50u p18:gp3 d18 p2 ph8 p18:gp3 d18 50u tauA tauB 50u d19 p19:gp4 d19 10u pl0:f1 ( center (p40:sp40 ph9):f1 (p11:gp11) ) ;PSYCHE element d19 10u pl1:f1 p19:gp4 d19 50u BLKGRAMP d0 ;End PSYCHE go=2 ph31 30m mc #0 to 2 F1QF(id0) F2QF(ivc) exit 50u LOCKH_OFF ph1=0 ph2=0 ph3=1 ph4=0 1 2 3 ph5=0 ph6=0 ph7=0 ph8=0 ph9=0 0 0 0 1 1 1 1 2 2 2 2 3 3 3 3 ph21=0 ph22=1 ph23=3 ph25=1 ph31=0 2 0 2 2 0 2 0 ;POWER LEVEL ;pl0 : zero power (0W) ;pl1 : power level for pulse (default) ;pl10 : power level for TOCSY-spinlock ;spw10 : power level of double-chirp PSYCHE pulse element ;spw12 : power level of refocusing shaped pulse ;spw32 : power level of adiabatic pulse of first ZQF element ;spw34 : power level of adiabatic pulse of last ZQF element ;spw40: power level of Saltire pulse ;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] ;pl0 : zero power [O W] ;p12 : 180 degree refocusing shaped pulse Selective TOCSY ; choose p12 according to desired selectivity ;p32 : first ZQF 180 degree inversion shaped pulse (adiabatic) [10 msec] ;p34 : second ZQF 180 degree inversion shaped pulse (adiabatic) [30 msec] ;p40: f1 channel - duration of SALTIRE pulse ;GRADIENT DURATION ;p11: duration of gradient under SALTIRE pulse ;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 PSYCHE selective pulse [1 msec] ;DELAY ;d0 : incremented delay ;d1 : relaxation delay; [2-10 s] ;d9 : TOCSY mixing time [50-200 ms] ;d11 : delay for disk I/O [30 msec] ;d15 : recovery delay for homospoil gradient [1 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 msec] ;d20 : inter pulse delay in PROJECT element [3-5 ms] ;PULSE SHAPE ;spnam12 : file name for the selective 180 refocusing shaped pulse selective TOCSY [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) ;spnam40 : file name for the adiabatic shaped pulse for PSYCHE element [SALTIRE] ; ;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 : CTP gradient [47%] ;gpz4 : CTP gradient for SALTIRE pulse [67%] ;gpz8 : saturation recovery gradient [31%] ;gpz10: last ZQF gradient [4%] ;gpz11 : Gradient for PSYCHE J refocussing element [1-3%] ;CONSTANTS ;cnst4: number of drop points [4] ;cnst12: chemical shift for selective pulse (offset, in ppm) ;cnst20: desired flip angle for saltire pulse element (degree) (normally 10-50) ;cnst21: bandwidth of saltire pulse (Hz) (normally 10000 Hz) ;cnst53: GammaB1/2*pi of first adiabatic ZQF shaped pulse ;cnst54: GammaB1/2*pi of last adiabatic ZQF shaped pulse ;OTHER ;PSYCHE: set O1 on in the center of the spectral window to be excited ;td1 number of t1 increments [16-64] ;td2 : number of delays in VDLIST ;vc : variable counter, taken from vc-list ;define VDLIST ;this pulse program produces a ser-file (PARMOD = 3D) ;NS: 16 * n, total number of scans: NS * TD0 ;in0 : 1/(2 * SW) = DW ;nd0 : 2 ;DS: 16