;zgsel3.fa ;1D sequence for calibration of shaped 1H 180 dgr. pulse ;Bruker Avance/Xwin-nmr version. ; ; shaped-180(x) - shaped-180(x) - acquire ; ;Written up by F. Abildgaard, NMRFAM (abild@nmrfam.wisc.edu) ; ; $Id ; ; Disclaimer: This pulse program is provided "as is" for your ; information. Support for the use of this pulse program is only ; provided to users of the National Magnetic Resonance Facility ; at Madison (NMRFAM). Users of this pulse program employ it at ; their own risk. Neither NMRFAM nor University of Wisconsin-Madison ; are liable for any physical or other damage incurred during the ; use of this pulse program. ; ; ;f1: 1H ;o1p: on-resonance or off-resonance for H2O, depending on the ; frequency shift of the shaped pulse ; ;d1: relaxation delay, 2-3s ;p12: 180 H1 shaped (spnam2) H2O pulse at power sp2. ;spnam2: fasqua.256 ;sp2: power level for shaped pulse ;spoffs2: offset for shaped pulse ;spoal2: 0.5 ; ;pl0: 120 dB ; ; How to use this sequence to calibrate a shaped HN 180 dgr. pulse ; with minimum excitation of the H2O resonance (for use in 15N T1 ; relaxation experiments): ; ; 1) Determine the offset and the length of the 180 dgr. shaped pulse: ; "offset" = (8.3-4.7)*bf1; 400 MHz: 1440 Hz; 500 MHz: 1800 Hz; ; 600 MHz: 2160 Hz, 750 MHz: 2700 Hz. ; ; p12 = sqrt(3)/(2*"offset"); 400 MHz: 601 us; 500 MHz: 481 us; ; 600 MHz: 401 us; 750 MHz: 321 us. ; ; 2) Set o1 to o1(H2O) - "offset" ; ; 3) Estimate the power level sp2. This can be done using the pw and pl ; for a regular 90 dgr. 1H pulse. If the proton 90 dgr. pulse is p1 at pl1, ; sp2 = pl1 + 20*log10(p12/(2*p1)). This works best if CORTAB has been ; done on your instrument. ; 4) Set spnam2 to fasqua.256, spoffs2 to "offset", spoal2 to 0.5. ; ; 5) Run a 1D 1H spectrum with rg = 1, ns = 1, ds = 0, and sp2 set ; to 1 dB lower than the value estimated in 3). ; FT and phase the water resonance (positive signal). ; ; 6) Optimize sp2 to make p12 180 dgr: ; run parnull (or paropt) varying sp2 in a +-3 dB window around the ; value estimated in 3). Look for the null. Then zoom in on the null ; by running parnull (or paropt) again with 0.1 dB steps. If the phasing ; is done correctly, a positive signal indicates that sp2 is too small, ; a negative signal is a sign that sp2 is too high. ; Be carefull not to miss the null by 6 dB: try varying sp2 from 60 dB ; in -1 dB steps (20-30 steps) and look for the second zero crossing. It ; should be the same the one found above. ; ;Define channel assignments: #define H f1 ;You shouldn't have to worry about anything beyond this point :-) "d11=100m" "d12=10u" "d13=5u" #include 1 ze 2 d11 d1 (d12 pl0 p12:sp2 ph11 d13 d12 pl0 p12:sp2 ph11):H go=2 ph31 d11 wr #0 exit ph11=0 2 1 3 ph31=0 2 1 3