/* gNcpmgex_X.c This is to replace gNcpmgex_NH.c because the latter doesn't give signal. Use gNcpmgex_NH to setup the experiment, and set seqfil='gNcpmgex_X' f1coef='1 0 -1 0 0 -1 0 -1' gzlvl6=5000 gzlvl5=16000 gt8=0.002 gzlvl8=18000 gzlvl11=17940 dpwr2_comp=48 ssfilter=200 or use macro gNcpmgex_x to setup the experiment. Youlin Xia at University of Minnesota on Jan 8, 2014 If comp_flg='y' there is a N15 pulse applied after d1 to compensate for RF/coil heating from the cpmg pulse train. This pulse be longest for the ncyc small and increases with ncyc to maintain a constant heating as a function of ncyc. Cryogenic probe tuning and shimming can be sensitive to power dissapation, so this compensates for the heating. Room temperature probes are not as sensitive to coil heating or deshimming, but may experience sample heating. The pulse is applied at dpwr2_comp power and the duration is calculated within the pulse sequence. The power should be determined by setting up a cpmg pulse train for the maximum ncyc to be used, starting the sequence, and then determining the heating power remaining (for a cold probe) after attaining steady-state. This should be done with comp_flg='n'. Then, set the N15 power levels other that dpwr2_comp to zero,ncyc=0 and set comp_flg='y'. Set ncyc_max to the largest ncyc value to be used in the queue of experiments. Try various compensation power levels until the heating power value achieves the same level as above. This represents a power level that produces the same heating as the cpmg pulse train. Now re-set ncyc and the cpmg pulse train power level to their proper values and leave comp_flg='y'. Use sufficient steady-state pulses to get to a stable heater value and then run the series of 2D experiments as a function of ncyc, one after the other. Once this is done the heating characteristics should be very similar from sample to sample so that the same settings could be used. */ #include #include "bionmr.h" char comp_flg[MAXSTR]; static int phx[1]={0}, phy[1]={1}, ph_x[1]={2}, phi2[2] = {0,2}, phi3[4] = {0,0,2,2}, phi5[4] = {0,0,2,2}, phi6[4] = {2,2,0,0}, phi9[8] = {0,0,0,0,1,1,1,1}, rec[8] = {0,2,2,0,2,0,0,2}; static double d2_init=0.0; pulsesequence() { /* DECLARE AND LOAD VARIABLES */ char f1180[MAXSTR], /* Flag to start t1 @ halfdwell */ c_flg[MAXSTR]; /* do TROSY on N15 and H1 */ int icosel, /* used to get n and p type */ t1_counter; /* to obtain maximum relaxT, ie relaxTmax */ double tau1, /* t1 delay */ taua, /* < 1 / 4J(NH) 2.25 ms */ taub, /* 1 / 4J(NH) in NH : 2.68 ms */ /* the sech/tanh pulse is automatically calculated by the macro "proteincal", */ /* and is called directly from your shapelib. */ pwClvl = getval("pwClvl"), /* coarse power for C13 pulse */ pwC = getval("pwC"), /* C13 90 degree pulse length at pwClvl */ rf0, /* maximum fine power when using pwC pulses */ rfst, /* fine power for the stCall pulse */ compH = getval("compH"), /* adjustment for H1 amplifier compression */ compN = getval("compN"), /* adjustment for N15 amplifier compression */ compC = getval("compC"), /* adjustment for C13 amplifier compression */ tpwrsf_t = getval("tpwrsf_t"), /* fine power adustment for first soft pulse(TROSY=n)*/ tpwrsf_n = getval("tpwrsf_n"), /* fine power adustment for first soft pulse(TROSY=y)*/ tpwrsf_d = getval("tpwrsf_d"), /* fine power adustment for second soft pulse(TROSY=y)*/ pwHs = getval("pwHs"), /* H1 90 degree pulse length at tpwrs */ tpwrs, /* power for the pwHs ("H2Osinc") pulse */ pwNlvl = getval("pwNlvl"), /* power for N15 pulses */ pwN = getval("pwN"), /* N15 90 degree pulse length at pwNlvl */ sw1 = getval("sw1"), dpwr2_comp, /* power level for CPMG compensation */ dpwr2_cp, /* power level for N CPMG */ pwn_cp, /* PW90 for N CPMG */ tauCPMG, /* CPMG delay */ ncyc, /* number of times to loop */ ncyc_max, /* max number of times to loop */ time_T2, /* total time for T2 measuring */ timeC, /* compensation time */ gt1, gt2, gt3, gt4, gt5, gt6, gt7, gt8, gt9, gt10, gt11, gstab, gzlvl0, gzlvl1, gzlvl2, gzlvl5, gzlvl6, gzlvl7, gzlvl8, gzlvl9, gzlvl10, gzlvl11; /* LOAD PHASE TABLE */ taua = getval("taua"); taub = getval("taub"); dpwr2_comp = getval("dpwr2_comp"); dpwr2_cp = getval("dpwr2_cp"); pwn_cp = getval("pwn_cp"); ncyc = getval("ncyc"); ncyc_max = getval("ncyc_max"); time_T2 = getval("time_T2"); getstr("f1180",f1180); getstr("c_flg",c_flg); gt1 = getval("gt1"); gt2 = getval("gt2"); gt3 = getval("gt3"); gt4 = getval("gt4"); gt5 = getval("gt5"); gt6 = getval("gt6"); gt7 = getval("gt7"); gt8 = getval("gt8"); gt9 = getval("gt9"); gt10 = getval("gt10"); gt11 = getval("gt11"); gstab = getval("gstab"); gzlvl0 = getval("gzlvl0"); gzlvl1 = getval("gzlvl1"); gzlvl2 = getval("gzlvl2"); gzlvl5 = getval("gzlvl5"); gzlvl6 = getval("gzlvl6"); gzlvl7 = getval("gzlvl7"); gzlvl8 = getval("gzlvl8"); gzlvl9 = getval("gzlvl9"); gzlvl10 = getval("gzlvl10"); gzlvl11 = getval("gzlvl11"); getstr("comp_flg",comp_flg); settable(t1,1,phx); settable(t2,2,phi2); settable(t3,4,phi3); settable(t4,1,phx); settable(t5,4,phi5); settable(t6,4,phi6); settable(t9,8,phi9); settable(t10,1,phx); settable(t11,1,phy); settable(t12,8,rec); /* INITIALIZE VARIABLES */ /* maximum fine power for pwC pulses (and initialize rfst) */ rf0 = 4095.0; rfst=0.0; /* 180 degree adiabatic C13 pulse from 0 to 200 ppm */ if (c_flg[A]=='y') {rfst = (compC*4095.0*pwC*4000.0*sqrt((30.0*sfrq/600.0+7.0)/0.35)); rfst = (int) (rfst + 0.5); if ( 1.0/(4000.0*sqrt((30.0*sfrq/600.0+7.0)/0.35)) < pwC ) { text_error( " Not enough C13 RF. pwC must be %f usec or less.\n", (1.0e6/(4000.0*sqrt((30.0*sfrq/600.0+7.0)/0.35))) ); psg_abort(1); }} /* selective H20 one-lobe sinc pulse */ tpwrs = tpwr - 20.0*log10(pwHs/(compH*pw*1.69)); /*needs 1.69 times more*/ tpwrs = (int) (tpwrs); /*power than a square pulse */ /* CHECK VALIDITY OF PARAMETER RANGES */ if((dm[A] == 'y' || dm[B] == 'y' || dm[C] == 'y' )) { text_error("incorrect dec1 decoupler flags! Should be 'nnn' "); psg_abort(1); } if((dm2[A] == 'y' || dm2[B] == 'y')) { text_error("incorrect dec2 decoupler flags! Should be 'nny' "); psg_abort(1); } if( dpwr2 > 50 ) { text_error("don't fry the probe, DPWR2 too large! "); psg_abort(1); } if( pw > 50.0e-6 ) { text_error("dont fry the probe, pw too high ! "); psg_abort(1); } if( pwN > 100.0e-6 ) { text_error("dont fry the probe, pwN too high ! "); psg_abort(1); } if( ncyc > 100) { printf("ncyc exceeds 100. May be too much \n"); psg_abort(1); } if( time_T2 > 0.090 ) { printf("total T2 recovery time exceeds 90 msec. May be too long \n"); psg_abort(1); } if( ncyc > 0) { tauCPMG = time_T2/(4*ncyc) - pwn_cp; if( ix == 1 ) printf("nuCPMG for current experiment is (Hz): %5.3f \n",1/(4*(tauCPMG+pwn_cp)) ); } else { tauCPMG = time_T2/4 - pwn_cp; if( ix == 1 ) printf("nuCPMG for current experiment is (Hz): not applicable \n"); } ncyc_max = time_T2/1e-3; if( tauCPMG + pwn_cp < 0.000250) { printf("WARNING: value of tauCPMG must be larger than or equal to 250 us\n"); printf("maximum value of ncyc allowed for current time_T2 is: %5.2f \n",ncyc_max); psg_abort(1); } /* PHASES AND INCREMENTED TIMES */ /* Phase incrementation for hypercomplex 2D data, States-Haberkorn element */ if (phase1 == 1) {tsadd(t10,2,4); icosel = +1;} else {tsadd(t3,2,4); icosel = -1;} /* Set up f1180 */ tau1 = d2; if((f1180[A] == 'y') && (ni > 1.0)) { tau1 += ( 1.0 / (2.0*sw1) ); if(tau1 < 0.2e-6) tau1 = 0.0; } tau1 = tau1/2.0; /* Calculate modifications to phases for States-TPPI acquisition */ if( ix == 1) d2_init = d2; t1_counter = (int) ( (d2-d2_init)*sw1 + 0.5 ); if(t1_counter % 2) { tsadd(t3,2,4); tsadd(t12,2,4); } /* BEGIN PULSE SEQUENCE */ status(A); obspower(tpwr); decpower(pwClvl); decpwrf(rf0); dec2power(pwNlvl); txphase(zero); decphase(zero); dec2phase(zero); delay(d1); obspower(tpwr); obsoffset(tof); delay(0.000001); /* xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx */ rcvroff(); dec2rgpulse(pwN, zero, 0.0, 0.0); /*destroy N15 magnetization*/ zgradpulse(gzlvl1, gt1); delay(1.0e-4); dec2rgpulse(pwN, one, 0.0, 0.0); zgradpulse(0.7*gzlvl1, gt1); decpwrf(rfst); txphase(t1); delay(5.0e-4); /* apply the compensation 15N pulses if desired */ if(comp_flg[A] == 'y') { dec2power(dpwr2_comp); /* Set decoupler2 compensation power */ timeC = time_T2*(ncyc_max-ncyc)/ncyc_max; dec2rgpulse(timeC,zero,0.0,0.0); dec2power(pwNlvl); delay(1e-3); } rgpulse(pw,t1,0.0,0.0); /* 1H pulse excitation */ txphase(zero); dec2phase(zero); zgradpulse(gzlvl2, gt2); delay(taua - gt2); sim3pulse(2.0*pw, 0.0, 2.0*pwN, zero, zero, zero, 0.0, 0.0); txphase(one); zgradpulse(gzlvl2, gt2); delay(taua - gt2); rgpulse(pw, one, 0.0, 0.0); txphase(two); if (tpwrsf_t<4095.0) { obspower(tpwrs+6.0); obspwrf(tpwrsf_t); shaped_pulse("H2Osinc_t", pwHs, zero, 5.0e-5, 0.0); obspower(tpwr); obspwrf(4095.0); } else { obspower(tpwrs); shaped_pulse("H2Osinc_n", pwHs, zero, 5.0e-5, 0.0); obspower(tpwr); } zgradpulse(gzlvl5, gt5); dec2phase(t3); delay(gstab); /* dec2rgpulse(pwN, t2, 0.0, 0.0); delay(taub); sim3pulse(2.0*pw, 0.0, 2.0*pwN, zero, zero, zero, 0.0, 0.0); dec2phase(one); delay(taub); dec2rgpulse(pwN, one, 0.0, 0.0); zgradpulse(gzlvl7, gt7); delay(gstab); */ dec2power(dpwr2_cp); /* Set decoupler2 power to dpwr2_cp for CPMG period */ dec2rgpulse(pwn_cp,t2,4.0e-6,2.0e-6); dec2phase(zero); /* start of the CPMG train for first period time_T2/2 on 2NyHz */ if(ncyc > 0) { delay(tauCPMG - (2/PI)*pwn_cp - 2.0e-6); dec2rgpulse(2*pwn_cp,one,0.0,0.0); delay(tauCPMG); } if(ncyc > 1) { initval(ncyc-1,v4); loop(v4,v5); delay(tauCPMG); dec2rgpulse(2*pwn_cp,one,0.0,0.0); delay(tauCPMG); endloop(v5); } /* change 2NyHz to Nx */ delay(2.0e-6); zgradpulse(gzlvl6,gt6); delay(gstab); delay(taub - gt6 - gstab -2.0e-6 - pwn_cp - 10.0e-6 - pwHs -2.0*POWER_DELAY - WFG_START_DELAY - WFG_STOP_DELAY ); if (tpwrsf_t<4095.0) { obspower(tpwrs+6.0); obspwrf(tpwrsf_t); shaped_pulse("H2Osinc_t", pwHs, t5, 5.0e-5, 0.0); obspower(tpwr); obspwrf(4095.0); } else { obspower(tpwrs); shaped_pulse("H2Osinc_n", pwHs, t5, 5.0e-5, 0.0); obspower(tpwr); } /* composite 1H 90y-180x-90y on top of 15N 180x */ dec2rgpulse(pwn_cp-2*pw,zero,2.0e-6,0.0); sim3pulse(pw,0.0e-6,pw,one,zero,zero,0.0,0.0); sim3pulse(2*pw,0.0e-6,2*pw,t6,zero,zero,0.0,0.0); sim3pulse(pw,0.0e-6,pw,one,zero,zero,0.0,0.0); dec2rgpulse(pwn_cp-2*pw,zero,0.0,2.0e-6); /* composite 1H 90y-180x-90y on top of 15N 180x */ if (tpwrsf_t<4095.0) { obspower(tpwrs+6.0); obspwrf(tpwrsf_t); shaped_pulse("H2Osinc_t", pwHs, t5, 5.0e-5, 0.0); obspower(tpwr); obspwrf(4095.0); } else { obspower(tpwrs); shaped_pulse("H2Osinc_n", pwHs, t5, 5.0e-5, 0.0); obspower(tpwr); } delay(taub - gt6 - gstab -2.0e-6 - pwn_cp - 10.0e-6 - pwHs -2.0*POWER_DELAY - WFG_START_DELAY - WFG_STOP_DELAY); delay(2.0e-6); zgradpulse(gzlvl6,gt6); delay(gstab); /* start of the CPMG train for second period time_T2/2 on Nx */ if(ncyc > 1) { initval(ncyc-1,v4); loop(v4,v5); delay(tauCPMG); dec2rgpulse(2*pwn_cp,zero,0.0,0.0); delay(tauCPMG); endloop(v5); } if(ncyc > 0) { delay(tauCPMG); dec2rgpulse(2*pwn_cp,zero,0.0,0.0); delay(tauCPMG - (2/PI)*pwn_cp - 2.0e-6); } dec2phase(one); dec2rgpulse(pwn_cp,one,2.0e-6,0.0); delay(4.0e-6); dec2power(pwNlvl); /* Set decoupler2 power back to pwNlvl */ dec2phase(t3); delay(2.0e-6); zgradpulse(gzlvl7,gt7); delay(gstab); /* xxxxxxxxxxxxxxxxxx N15 EVOLUTION xxxxxxxxxxxxxxxxxxxxx */ dec2rgpulse(pwN, t3, 0.0, 0.0); txphase(zero); decphase(zero); txphase(zero); dec2phase(t9); if ( (c_flg[A]=='y') && (tau1 > 0.5e-3 + WFG2_START_DELAY) ) {delay(tau1 - 0.5e-3 - WFG2_START_DELAY); /* WFG2_START_DELAY */ simshaped_pulse("", "stC200", 2.0*pw, 1.0e-3, zero, zero, 0.0, 0.0); delay(tau1 - 0.5e-3);} else {delay(tau1); rgpulse(2.0*pw, zero, 0.0, 0.0); delay(tau1);} delay(taub); sim3pulse(2.0*pw, 0.0, 2.0*pwN, zero, zero, t9, 0.0, 0.0); zgradpulse(gzlvl8, gt8); /* 2.0*GRADIENT_DELAY */ txphase(t4); dec2phase(t10); delay(taub -gt8 - 2.0*GRADIENT_DELAY +2.0*pw); /* xxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxxx */ sim3pulse(pw, 0.0, pwN, t4, zero, t10, 0.0, 0.0); txphase(zero); dec2phase(zero); zgradpulse(gzlvl9, gt9); /*modified amp according to Frans Mulder and LEK suggestion */ delay(taub - 1.3*pwN - gt9); sim3pulse(2.0*pw, 0.0, 2.0*pwN, zero, zero, zero, 0.0, 0.0); zgradpulse(gzlvl9, gt9); txphase(one); dec2phase(t11); delay(taub - 1.3*pwN - gt9); sim3pulse(pw, 0.0, pwN, one, zero, t11, 0.0, 0.0); txphase(zero); dec2phase(zero); zgradpulse(gzlvl10, gt10); delay(taua - 1.3*pwN - gt10); sim3pulse(2.0*pw, 0.0, 2.0*pwN, zero, zero, zero, 0.0, 0.0); dec2phase(t10); zgradpulse(gzlvl10, gt10); delay(taua - 0.65*pwN - gt10); rgpulse(pw, zero, 0.0, 0.0); delay(0.1*gt8 + 1.0e-4 +gstab - 0.65*pw + 2.0*GRADIENT_DELAY + POWER_DELAY); rgpulse(2.0*pw, zero, 0.0, 0.0); dec2power(dpwr2); /* POWER_DELAY */ zgradpulse(icosel*gzlvl11, 0.1*gt8); /* 2.0*GRADIENT_DELAY */ delay(gstab); rcvron(); statusdelay(C,1.0e-4); setreceiver(t12); }