502: 5mm TXI-XYZ, #Z8281-0165

In principle: Do NOT trust these values blindly - verify them if questionable!

Amplifiers can go bad or your sample environment like salt, temperature, ... might alter the pulse width!

1. General Information:

  • Shimfile: chloshim.600 is a good starting point for aqueous samples
  • Read Pulses from Master List:
    • Read in pulse sequence and Parameter file
    • Use the getprosol command or click on the test tube symbol in ased
    • For Bruker Pulse Sequences type: getprosol 1H 'p1' ' pl1' , where p1 is the determined pulse length [us] at the power level pl1 [dB].

2. Hard Pulses:

Nucleus Type Attenuation Channel 90deg Pulse Amplifier Calc. Date
1H -12.5 dB f1 7.50 us 17.8W 40W max 8/28/17
waltz16 f1 80.0 us
TOCSY f1 26.0 us
ROESY f1 90.0 us
.
13C hard -23.35dB f2 12.0 us 216.3W 300W max 8/28/17
Urea TOCSY -16.65 dB f2 26.0 us 46.2 W -16.63 dB 8/28/17
TOCSY -14.10 dB f2 35.0 us 25.7 W-14.05 dB 8/28/17
Dec -8.10 dB f2 70.0 us 6.45 W -8.03 dB 8/28/17
LowDec -4.95 dB f2 100.0 us 3.12 W -4.93 dB 8/28/17
.
15N hard -24.00 dB f3 40.0 us 251.2 W 300W max 8/28/17
Urea -17.20 dB f3 90.0 us 52.5 W -16.95 dB 8/28/17
-11.20 dB f3 180.0 us 13.2 W -10.95 dB 8/28/17
-8.50 dB f3 240.0 us 7.08 W -8.44 dB 8/28/17
-5.20 dB f3 350.0 us 3.30 W -5.16 dB 8/28/17
.
2H -12.97 dB 2HTX 68 us 19.8 W 30 W max 8/29/17
-0.20 dB 2HTX 300 us 1.04W 8/29/17

3. Soft Pulses: (Urea)

Nucleus Type Channel Pulse Attenuation Amplifier Calc. Date
13C, α+β Q5_sebop 420us f2 90 deg -18.70 dB (-18.97) 74.1 W on res. 8/27/17
α+β Q5tr_sebop 420us f2 90 deg -18.95 (-18.97) dB78.5 W on/off res. 8/27/17
α Q5.1000 1800us f2 90 deg -4.90 dB (-5.10) 3.10 W on/off res. 8/27/17
α Q5tr.1000 1800us f2 90 deg -5.00 dB (-5.10) 3.16 W on/off res. 8/27/17
α+β Q3_surbop 324us f2 180 deg -18.95 dB (-19.12) 78.5 W on res. 8/27/17
α Q3_surbop 888us f2 180 deg -10.20 dB (-10.73)10.5 W on res. 8/27/17
α Q3_surbop 972us f2 180 deg -9.40 dB (-9.58)8.71 W on res. 8/27/17
CO dec Q3_surbop 1260us f2 180 deg -7.15 dB (-7.33) 5.19 W on res. 8/27/17

4. Miscellaneous:

Magic angle on GREAT III: factor Z/XY = 1.39 (4-21-03)
Offset Ca - carbonyl (56 - 175ppm): -14965 Hz
1H offset @ 4.7 pppm: 2350.6 Hz
Main Field: 500.13 MHz
BSMS Field: +2966 units (10-13-2003)

5. Conditions for pulse determination:

  • Sample:
    1H-pulses: 2mM Sucrose + 0.5mM DSS + 2mM NaN3, 90% H2O 10% D2O
    X-pulses: 13C, 15N labled Urea in DMSO
    13C-shift: 48.5ppm, J=138.5Hz
    15N-shift: 76.0ppm, J=88.5Hz
  • Temperature: 298K
  • RF-Filters: none
    1H = none
    X = none
    Y = none
    Z = none
  • Attenuators at amplifier input: none
    1H = 0dB
    X = 0dB
    Y = 0dB
    Z = 0dB
  • Cortab combinations done 11-28-03:
    1H --> FCU 1+2, MOD, MULT, BLA
    13C --> FCU 1+2, obn X-Amplifier: MOD, MULT, BLA
    15N Version 3.5 does not work, use cortab v3.1, which is NOT linear