;cpcodex2d.mh ;centerband-only detection of exchange to probe slow dynamic process ;double resonance mode ;deAzevedo ER, Hu WG, Bonagamba TJ, Schmidt-Rohr K. ;J. Am. Chem. Soc., volume 121, 8411, 1999 ;cd15mp1:tr/4 - p1 ;cd15mp2: tr/4 - p2 ;d1: recycle delay ;d13: mixing time ;d14: z-filter time ;d10: z-filter after t1, ~2-4 ms ;d18: gamma integral, e.g. 30us ;p1: 13C 90 pulse ;p2: 13C 180 pulse ;p15: CP contact time ;p8: 1H TPPM pulse during acq ;p18: 1H TPPM pulse during texc, trec ;pl1: F1 CP power ;pl11: F1 hard pulse power ;pl12: 1H dec during acq ;pl22: 1H dec during CODEX, strong ;l0: even, total No rotor periods = L0+2 ;l5: gamma integral loop, 2 or 4 ;in18: tr/L5 define delay cd15mp1 define delay cd15mp2 define delay cd15m1h "d15=0.25s/l31" "cd15mp1=0.25s/l31-p1-2u" "cd15mp2=0.25s/l31-p2" "cd15m1h=0.25s/l31-p1-p1/2" "l1=aq/(p8*2)" "d3=1s/l31-p2/2" define loopcounter td1half "td1half=td1/2" 1 ze 2 d1 10u pl1:f1 10u pl2:f2 1u:f2 ph1 1u:f1 ph2 rpp5 ;reset phase for xy-8 3 p3:f2 ph1 ;1H 90 excitation 1u pl3:f2 ;change 1H power (p15:sp1 ph2):f1 (p15 ph23):f2 ;CP contact 1u cw:f2 pl22:f2 1u pl11:f1 d0 ;t1, iso. shift evolution p1:f1 ph6 ;cosine/sine modulation 1u do:f2 d10 ;dephasing transverse M, ~10ms trigpe1 ;record rotor phase 1u cw:f2 pl22:f2 1u:f1 ph7 p1:f1 ph7 ;read out, same phase as after ph2 ;----------- excitation --------------------------- 4 cd15mp1 ;tr/4 d15:f1 ph5 p2:f1 ph5^ d15 5 cd15mp2:f1 ph5 p2:f1 ph5^ ;13C 180 pulse d15 lo to 5 times l0 ;L0=2n, even number cd15m1h:f1 ph8 ;texc=(n+1)tr=(L0/2+1)tr p1:f1 ph8 ;------------ exchange mixing time ------------------------ 1u do:f2 d13 ;mixing time trigpe1 ;same rotor phase as above 1u cw:f2 pl22:f2 1u:f1 ph9 p1:f1 ph9 ;----------- reconversion --------------------------- cd15m1h ;tr/4 6 d15:f1 ph5 p2:f1 ph5^ ;13C 180 deg. pulse cd15mp2 lo to 6 times l0 ;L0=2n, an even number d15:f1 ph5 p2:f1 ph5^ d15 cd15mp1:f1 ph3 ;tr/4 2u ;------------ z-filter, to control for T1 relaxation ----------------- 7 p1:f1 ph3 1u do:f2 d14:f1 ph4 ;z-filter 1u cw:f2 pl12:f2 p1:f1 ph4 d3 ;Hahn echo detection to .. p2:f1 ph12 ;.. remove pulse ringdown .. d3 ;... get flat baseline in the spectrum 2u:f1 ph0 ;dead time delay, reset RF phase to detect 2u adc ph31 ;start ADC with ph31 signal routing 8 p8:f2 ph13 p8:f2 ph14 lo to 8 times l1 aq do:f2 ;allow time for data sampling rcyc=2 ;do NS scans 10m id14 ;increment d18 by in18=tr/L5 //gamma integral// lo to 2 times l5 wr #0 exit ph0= 0 ;reference phase for detection ph1= +x -x ;1H 90 excitation ph23= +y ;1H CP ph2= +x +x +y +y -x -x -y -y ;F1 CP ph5= +x +y +x +y +y +x +y +x ;xy-8 ph6= +y +y -x -x -y -y +x +x ;store to z-axis -y -y +x +x +y +y -x -x ph7= -y -y +x +x +y +y -x -x ;read out ph8= -y -y +x +x +y +y -x -x ;+z cosine store for tm -y -y +x +x +y +y -x -x ;+z cosine -x -x -y -y +x +x +y +y ;+z sine -x -x -y -y +x +x +y +y ;+z sine +y +y -x -x -y -y +x +x ;-z cosine +y +y -x -x -y -y +x +x ;-z cosine +x +x +y +y -x -x -y -y ;-z sine +x +x +y +y -x -x -y -y ;-z sine ph9= +y +y -x -x -y -y +x +x ;read-out after tm -y -y +x +x +y +y -x -x +x +x +y +y -x -x -y -y -x -x -y -y +x +x +y +y ph3= -y -y +x +x +y +y -x -x ;store for second z period -y -y +x +x +y +y -x -x -y -y +x +x +y +y -x -x -y -y +x +x +y +y -x -x ph4= +y +y -x -x -y -y +x +x ;readout after second z period ;ph3= -y -y +x +x +y +y -x -x ;store for second z period ;ph4= +y +y -x -x -y -y +x +x ;readout after second z period ph12= +x +x +y +y -x -x -y -y ph13= (360) 14 ph14= (360) 0 ph31= 0 2 1 3 2 0 3 1 0 2 1 3 2 0 3 1 0 2 1 3 2 0 3 1 0 2 1 3 2 0 3 1 2 0 3 1 0 2 1 3 2 0 3 1 0 2 1 3 2 0 3 1 0 2 1 3 2 0 3 1 0 2 1 3