------------------------------------------------------------------------------- -- -- -- Experiment Source Code -- -- Delta NMR Experiment & Machine Control Interface -- -- -- -- Copyright (c) 2009 JEOL Ltd -- -- All Rights Reserved -- -- -- ------------------------------------------------------------------------------- ----By Rongchun Zhang, 2022/02/09 ----Ref: Rongchun Zhang et al. J. Magn. Reson. 2016, 266, 59-66 ---Record a CP and a NOE spectrum separately in a single experiment ----Mobile signals come from pure 1H-13C NOE effect -- HELP.eng: Cross Polarization with polarization inversion ++ NOE -- Category: solids, 1D standard, cpmas --- loop (+XCP -- -XCP -- -XCP -- +XCP)--NOE header filename => "cp-noe-2s-1D"; sample_id => ""; comment => "Cross Polarization with transient NOE"; process = "1d_solid.list"; include "header_solid"; end header; instrument include "instrument_solid"; end instrument; acquisition x_domain => "Carbon13"; x_offset => 100[ppm]; x_sweep => 300[ppm]; x_points_input => 512; x_points =? if x_points_input/x_sweep < 50 [ms] then x_points_input else 2; scans => 4; x_prescans => 0; mod_return => 1; include "acquisition_solid"; end acquisition; pulse collect COMPLEX,OBS; include "pulse_solid"; include "dec_solid"; CP_Setup =? "#Setup CP#"; irr_shape_cp = "constant_cp"; irr_shape_cp2 = "constant_cp2"; irr_width_90 => irr90, help "90deg pulse width for excitation pulse"; irr_amp_prep => 100[%], 0[%]->100[%]:0.01[%], help "amplitude of excitation pulse"; obs_shape_cp => "constant_cp", ("constant_cp", "RAMP_cp"),help "CP shape for obs channel"; obs_shape_cp2 => "constant_cp2", ("constant_cp2", "RAMP_cp2"),help "CP shape for obs channel"; contact_time => 2[ms], 10[us]->20[ms]:10[us], help "contact time"; irr_amp_cp => 70[%], 0[%]->90[%]:0.01[%], help "CP amplitude of irr channel"; irr_amp_cp2 => irr_amp_cp; obs_amp_cp => 70[%], 0[%]->90[%]:0.01[%], help "CP amplitude of obs channel"; obs_amp_cp2 => obs_amp_cp; when obs_shape_cp = "ramp_cp" do obs_amp_grad => 10[%], -100[%]->100[%]:0.1[%], help "obs CP sweep range (-obs_amp_grad/2->+obs_amp_grad)"; end when; when obs_shape_cp2 = "ramp_cp2" do obs_amp_grad2 => -obs_amp_grad, help "obs CP sweep range (-obs_amp_grad/2->+obs_amp_grad)"; end when; irr_noise => "CW",("CW", "SPINAL64", "TPPM", "XiX"), help "decoupling sequence"; initial_wait = 10.0[ms]; irr_Setup =? "#Setup Irradiation#"; irr_domain => "Proton", help "decoupled nucleus"; irr_offset => 5[ppm], help "decoupler offset"; tauNOE => 0.5[s], help "transient NOE mixing time"; num_cp_cycle => 2; obs_width_90 => 3[us], help "90deg pulse width for X excitation pulse"; obs_amp_pulse => 100[%], 0[%]->100[%]:0.01[%], help "amplitude of X excitation pulse"; irr_amp_cwdec => 80[%], 0[%]->90[%]:0.01[%], help "amplitude of CW decoupling pulse"; recycle_Setup =? "#Setup Recycle Times#"; relaxation_delay => 5.0[s], help "relaxation delay"; repetition_time =? relaxation_delay + x_acq_time, help"relaxation_delay+x_acq_time"; atn_Setup =? "#Experiment Attenuator Settings#"; obs_atn => xatn, help "attenuator for obs"; irr_atn => irratn, help "attenuator for irr"; irr_phs_prep = { 90, 270}; irr_phs_cp = { 0,0}; irr_phs_cp2 = {180,180}; irr_phs_cwdec = { 180,0 }; irr_phs_dec = { 0 }; obs_phs_cp = { 0,0,180,180,90,90,270,270}; obs_phs_cp2 = { 180,180,0,0,270,270,90,90}; irr_phs_flip = {90, 270}; obs_phs_read = {0,180,90,270}; obs_phs_acq1 = {0,180,180,0,90,270,270, 90}; ---phase for CP obs_phs_acq2 = {0, 180, 90, 270}; -----phase for NOE obs_phs_flip1 = {270}; obs_phs_flip2 = {90}; irr_phs_flip3 = {270, 90}; module_config = "solid_sample continuous_fid"; begin initial_wait; relaxation_delay; irr_width_90, (irr.gate, irr.phs.irr_phs_prep, irr.amp.irr_amp_prep, irr.atn.irr_atn); loop num_cp_cycle times contact_time, (irr.gate, irr.phs.irr_phs_cp, irr.shape.{irr_shape_cp,"irr"}, irr.atn.irr_atn, obs.gate, obs.phs.obs_phs_cp, obs.shape.{obs_shape_cp,"obs"}, obs.atn.obs_atn); contact_time, (irr.gate, irr.phs.irr_phs_cp2, irr.shape.{irr_shape_cp2,"irr"}, irr.atn.irr_atn, obs.gate, obs.phs.obs_phs_cp2, obs.shape.{obs_shape_cp2,"obs"}, obs.atn.obs_atn); contact_time, (irr.gate, irr.phs.irr_phs_cp2, irr.shape.{irr_shape_cp2,"irr"}, irr.atn.irr_atn, obs.gate, obs.phs.obs_phs_cp2, obs.shape.{obs_shape_cp2,"obs"}, obs.atn.obs_atn); contact_time, (irr.gate, irr.phs.irr_phs_cp, irr.shape.{irr_shape_cp,"irr"}, irr.atn.irr_atn, obs.gate, obs.phs.obs_phs_cp, obs.shape.{obs_shape_cp,"obs"}, obs.atn.obs_atn); end loop; on (irr.gate, irr.phs.irr_phs_cwdec, irr.amp.irr_amp_cwdec, irr.atn.irr_atn); acq( dead_time, delay, obs_phs_acq1 ); off (irr.gate); irr_width_90, (irr.gate, irr.phs.irr_phs_flip, irr.amp.irr_amp_prep, irr.atn.irr_atn); tauNOE; obs_width_90, (obs.gate, obs.phs.obs_phs_read, obs.amp.obs_amp_pulse, obs.atn.obs_atn); on (irr.gate, irr.phs.irr_phs_dec, irr.amp.irr_amp_dec, irr.atn.irr_atn, irr.noise.irr_noise); acq( dead_time, delay, obs_phs_acq2 ); off (irr.gate); end pulse;