------------------------------------------------------------------------------- -- -- -- Experiment Source Code -- -- Delta NMR Experiment & Machine Control Interface -- -- -- -- Copyright (c) 2021 JEOL Ltd -- -- All Rights Reserved -- -- -- ------------------------------------------------------------------------------- -- HELP.eng: double_cp_2d -- Category: solids, ultrafast mas, 2D, heteronuclear correlation -- Modified from double_cp_2d.jxp (Matsunaga) header filename => "double_cp_2d"; sample_id => ""; comment => "double_cp_2d"; process = "2d_solid.list"; include "header_solid"; end header; instrument include "instrument_solid"; end instrument; acquisition x_domain => "Proton"; x_offset => 5[ppm]; x_sweep => 100[kHz]; x_points => 1024; scans => 8; x_prescans => 0; mod_return => 2; y_domain => "Carbon13"; y_offset => 100[ppm]; y_sweep => 250[ppm]; y_points => 32; include "acquisition_solid"; y_acq_time =? y_points / y_sweep; y_resolution =? 1 / y_acq_time; y_dwell =? 1 / x_sweep; end acquisition; pulse collect COMPLEX,OBS COMPLEX,IRR; initial_wait = 10.0[ms]; irr_domain = y_domain , help "decoupled nucleus"; irr_offset = y_offset , help "decoupler offset"; Pulse_Setup =? "#Setup hard pulses#"; obs_width_90 => x90; obs_amp_pulse => 100[%], 0[%]->100[%] : 10[m%]; irr_width_90 => irr90; irr_amp_pulse => 100[%]; CP1_Setup =? "#Setup first CP#"; obs_shape_cp = "RAMP_cp"; contact_time => 4[ms], 0[us]->20[ms] : 10[us], help "contact time"; obs_amp_cp => 30[%], 0[%]->100[%] : 10[m%], help "CP amplitude of irr channel"; obs_amp_grad => 10[%], -100[%]->100[%] : 0.1[%], help "irr CP sweep range (-irr_amp_grad/2->+irr_amp_grad)"; irr_shape_cp = "RAMP_cp"; irr_amp_cp => 30[%], 0[%]->100[%] : 10[m%], help "amplitude of obs channel"; irr_amp_grad => 1[%], -100[%]->100[%] : 0.1[%], help "obs CP sweep range (-obs_amp_grad/2->+obs_amp_grad)"; CP2_Setup =? "#Setup second CP#"; obs_shape_cp2 = "RAMP_cp2"; contact_time2 => 4[ms], 0[us]->20[ms] : 10[us], help "contact time"; obs_amp_cp2 => obs_amp_cp, 0[%]->100[%] : 10[m%], help "CP amplitude of irr channel"; obs_amp_grad2 => -obs_amp_grad; irr_shape_cp2 = "RAMP_cp2"; irr_amp_cp2 => irr_amp_cp, 0[%]->100[%] : 10[m%], help "amplitude of obs channel"; irr_amp_grad2 => -irr_amp_grad; -------- constant of RF intensity --------- obs_nu = 0.25/x90; -------- SLAP (SLAP_obs.jxi)--------- block_slap =? "#SLAP#"; slap_ofs => 1.2[ppm]; --irradiation offset obs_nu_CW => 10[kHz]; --intensity of CW slap_ad_nu1 => obs_nu_CW*1.41; --intensity of adrot slap_ad_nua => 1[kHz]; --rotation frequency of ad rot obs_amp_CW =? obs_nu_CW /obs_nu*100[%], 0[%]->100[%] : 0.01[%]; slap_ad_amp =? slap_ad_nu1 /obs_nu*100[%], 0[%]->100[%] : 0.01[%]; obs_width_slap =? 1 / slap_ad_nua; time_cw => 10[ms]; time_slap => 50[ms]; lp_slap =? upper (time_slap / obs_width_slap); macro SLAP_obs (time_CW, lp_slap, obs_width_slap, obs_atn, obs_amp_CW, slap_ad_amp, slap_ofs) is time_cw, (OBS.GATE, OBS.ATN.obs_atn, OBS.AMP.obs_amp_CW, OBS.PHS.{0}, OBS.OFFSET.slap_ofs); loop lp_slap times obs_width_slap, (OBS.GATE, OBS.ATN.obs_atn, OBS.SHAPE.{"adrot_PM", "SLAP"}, OBS.PHS.{0}, OBS.OFFSET.slap_ofs); end loop; end SLAP_obs; -------------------------------------- IRRdec_Setup =? "#Setup IRR dec#"; irr_noise =? "WALTZ"; irr_pwidth => 10[us]; irr_amp_dec => 1[%]; OBSdec_Setup =? "#Setup OBS dec#"; obs_noise => "CW", ("CM", "CW", "SPINAL64", "SPINAL64_vp", "swfTPPM", "TPPM", "XiX"), help "decoupling sequence"; obs_amp_dec => 5[%], 0[%]->100[%] : 10[m%], help "amplitude of decoupling"; when obs_noise /= "CW" and obs_noise /= "XIX" do obs_width_nominal90 => x90 * 100[%] / obs_amp_dec, help "modulation pulse width for decoupling"; end when; when obs_noise = "CM" or obs_noise = "SPINAL64_vp" or obs_noise = "swfTPPM" or obs_noise = "TPPM" do obs_phs_tppm => 15[deg], help "decoupling sequence phase modulation"; end when; when obs_noise = "XiX" do obs_width_xix => 50[us], help "XiX modulation pulse width: should be optimized around 1.85*tr"; end when; obs_pwidth = if obs_noise = "CW" then 0[us] else if obs_noise = "XiX" then obs_width_xix else obs_width_nominal90; -- HORROR_Setup =? "#Setup HORROR#"; -- -- tau_rr => 5[ms]; -- obs_amp_rr => 10[%]; MISC_Setup =? "#Setup Miscellaneous#"; t1 => 0[us]; SATURATION => FALSE; when SATURATION do obs_width_sat => x90; obs_amp_sat => 100[%], 0[%]->100[%]:0.01[%], help "amp for pre-saturation pulses"; sat_term => 1[s], help "saturation time"; sat_pulse_interval => 10[ms], help "interval of saturation pulse"; sat_loop =? round(sat_term/(sat_pulse_interval+obs_width_90)), help "loop of saturation pulse"; end when; relaxation_delay => 5[s], help "inter-pulse delay"; repetition_time =? relaxation_delay + x_acq_time, help "relaxation_delay+x_acq_time"; obs_atn => xatn, help "attenuator of obs"; irr_atn => irratn, help "attenuator of irr"; obs_phs_prep = {4( 0),4(180)}; obs_phs_cp1 = { 90}; obs_phs_dec = { 0}; obs_phs_cp2 = {2( 0),2(180)}; -- obs_phs_rrx = { 0}; -- obs_phs_rry = { 90}; irr_phs_cp1 = {{ 0,180},{ 90,270}}.ystep(180%2); irr_phs_store = { 90}; irr_phs_restore = {270}; irr_phs_cp2 = { 0}; irr_phs_dec = { 0}; obs_phs_acq = { 0,180,180, 0,180, 0, 0,180}.ystep(180%2); include "pulse_solid"; module_config = "solid_sample"; begin initial_wait; when SATURATION do loop sat_loop times sat_pulse_interval; obs_width_sat,(obs.gate, obs.phs.0, obs.amp.obs_amp_sat, obs.atn.obs_atn); end loop; end when; relaxation_delay; obs_width_90, (obs.gate, obs.phs.obs_phs_prep, obs.amp.obs_amp_pulse, obs.atn.obs_atn); contact_time, (obs.GATE, obs.PHS.obs_phs_cp1, obs.shape.{obs_shape_cp, "obs"}, obs.ATN.obs_atn, irr.GATE, irr.PHS.irr_phs_cp1, irr.SHAPE.{irr_shape_cp, "irr"}, irr.ATN.irr_atn); t1 ystep 1/y_sweep, (obs.GATE, obs.PHS.obs_phs_dec, obs.AMP.obs_amp_dec, obs.ATN.obs_atn, obs.NOISE.obs_noise); irr_width_90, (irr.gate, irr.phs.irr_phs_store, irr.amp.irr_amp_pulse, irr.atn.irr_atn); -- tau_rr, (obs.gate, obs.phs.obs_phs_rrx, obs.amp.obs_amp_rr, obs.atn.obs_atn); -- tau_rr, (obs.gate, obs.phs.obs_phs_rry, obs.amp.obs_amp_rr, obs.atn.obs_atn); ------------ SLAP ------------ SLAP_obs (time_CW, lp_slap, obs_width_slap, obs_atn, obs_amp_CW, slap_ad_amp, slap_ofs); ------------------------------ irr_width_90, (irr.gate, irr.phs.irr_phs_restore, irr.amp.irr_amp_pulse, irr.atn.irr_atn); contact_time2, (obs.GATE, obs.PHS.obs_phs_cp2, obs.shape.{obs_shape_cp2, "obs"}, obs.ATN.obs_atn, irr.GATE, irr.PHS.irr_phs_cp2, irr.SHAPE.{irr_shape_cp2, "irr"}, irr.ATN.irr_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_acq ); off(irr.gate); end pulse;