;1.3) Program: CP/T1/TOSS ;Description: Use to determine recycle delay for DP/MAS ;Requires: !; high sensitivity and therefore moderate spinning frequency (6.5 kHz) ;Reference(s): Mao et al., Soil Sci. Soc. of Am. J. 64, 873-884 (2000). Mao & KSR, Environ. ;Sci. Technol. 38, 2680-2684 (2004). ;srcpt1toss.cpd ;from srcpt1toss.ksr on SGI ;Uses CPDs2: type "eda", set "CPDPRG2" to "tppm15", set p30=p31=9u (180 on 1H at pl12) ;with tppm decoupling after gated decoupling (optional) ;13C T1 filter after CP and before ;TOtal Sideband Suppression (TOSS) using four 180 13C pulses ;durations between 180 pulses (d25-d29) are calculated from l31 (=SS in Hz) ;pl2 is power level for contact, pl12 is power level for decoupling on F2 "d25=(1s/l31)*0.1226-(p2/2)-2u" "d26=(1s/l31)*0.0773-p2" "d27=(1s/l31)*0.2236-p2" "d28=(1s/l31)*1.0433-p2" "d29=(1s/l31)*0.7744-(p2/2)-d13" "d30=d29-d14-1u" 1 ze 2 d1 do:f2 ;recycle delay, turn the decoupler off 10u pl2:f2 ;preselect pl2 drive power for F2 10u pl1:f1 ;preselect pl1 drive power level for F1 1u:f2 ph1 1u:f1 ph2 p3:f2 ph1 ;proton 90 pulse (p15 ph2):f1 (p15 ph10):f2 ;contact pulse p1:f1 ph6 d16 do:f2 ;13C T1 filter p1:f1 ph7 1u cpds2:f2 ;turn on F2 decoupling, (tppm15, set p30=p31=180 on 1H at pl12) 1u pl12:f2 pl11:f1 ;set decoupling drive power level d25 ; p2:f1 ph13 ;180 13C #1 d26 ; p2:f1 ph14 ;180 13C #2 d27 ; p2:f1 ph15 ;180 13C #3 d28 ; p2:f1 ph16 ;180 13C #4 d14 do:f2 ;gated decoupling 1u cpds2:f2 ;turn on F2 decoupling (tppm15, set p30=p31=180 on 1H at pl12) d30 ;rest of TOSS d29 2u:f1 ph0 ;dead time delay, reset RF phase to detect go=2 ph31 ;do NS scans 1m do:f2; turn the decoupler off wr #0 exit ph0= 0 ;reference phase ph1= 1 3 ph2= 0 0 1 1 2 2 3 3 ;13C CP ph6= 1 1 2 2 3 3 0 0 ;store to z for T1 filter 1 1 2 2 3 3 0 0 3 3 0 0 1 1 2 2 3 3 0 0 1 1 2 2 ph7= 3 3 0 0 1 1 2 2 ;read from z ph10= 0 ;1H CP ph13= 1 1 2 2 3 3 0 0 ;180 13C #1 ph14= 3 3 0 0 1 1 2 2 ;180 13C #2 ph15= 1 1 2 2 3 3 0 0 ;180 13C #3 3 3 0 0 1 1 2 2 ph16= 2 2 1 1 0 0 3 3 ;180 13C #4 0 0 3 3 2 2 1 1 ph31= 0 2 1 3 2 0 3 1 ;RLS 0 2 1 3 2 0 3 1 2 0 3 1 0 2 1 3 ;ph6 inversion 2 0 3 1 0 2 1 3