800: 5mm TXI-XYZ, #8435-0022

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: 8432_022ws.shim is a good starting point for aqueous samples

2. Hard Pulses:

Nucleus Type Attenuation Channel 90deg Pulse Amplifier Calculated Date
1H -1.0 dB f1 10.4 us 100W 1-13-2004
1H -2.0 dB f1 9.2 us 100W 1-13-2004
+4.0 dB f1 18.75 us 100W 1-13-2004
+10.0 dB f1 37.7 us 100W 1-13-2004
+16.0 dB f1 74.7 us 100W 1-13-2004
waltz16 f1 70.0 us 100W
TOCSY f1 25-35.0 us 100W
ROESY f1 100.0 us 100W
.
13C hard -4.0 dB f2 12.95 us 500W 11-6-2003
+3.90 dB TOCSY +3.5 dB f2 32.0 us 500W +3.9 dB 11-6-2003
Dec +8.05 dB f2 54.0 us 500W +8.05 dB 11-6-2003
LowDec 1 +11.55 dB f2 80.0 us 500W +11.61 dB 11-6-2003
LowDec 2 +17.0 dB f2 160.0 us 500W +17.30dB 11-6-2003
.
15N hard -4.95 dB f3 40.0 us 300W 11-6-2003
-4.05 dB f3 45.0 us 300W -3.93 dB 11-6-2003
-3.25dB f3 50.0 us 300W -3.13 dB 11-6-2003
+8.70 dB f3 200.0 us 300W +8.91 dB 11-6-2003
.
2H dB us 300W
dB 400 us 20W 3-30-2002

3. Soft Pulses:

Nucleus Type Channel Pulse Attenuation Amplifier Calculated Date
13C G4.256 340us f2 90 deg -1.5 dB500W 11-6-2003
G4.256 680us f2 90 deg +4.6 dB500W 11-6-2003
G3.256 200us f2 180 deg -3.05 dB500W 11-6-2003
G3.256 640us f2 180 deg +7.05 dB500W 11-6-2003
G4tr.256 340us f2 90 deg -0.9dB500W 11-6-2003
Sinc1 160us f2 90 deg dB500W
Sinc1 160us f2 180 deg dB500W
1H Sinc1.1000 1.2ms f1 180 deg +40.36 dB100W 3-30-2002

G3 and G4 pulses were determined with spoal=0.5, on-resonance

4. Miscellaneous:

Magic angle on GREAT III: factor Z/XY = 1.30 (11-6-2003)
Offset Ca - carbonyl (56 - 175ppm): -18109Hz
1H offset @ 4.7 pppm: 2820 Hz
Main Field: 600.21 MHz
BSMS Field: +1317 units (10-13-2003)

5. Conditions for pulse determination:

  • Samples:
    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:
    1H = none
    X = Highpass 800MHz 13C-Pass; 2H-Stop
    Y = Lowpass 800MHz 15N-pass; 2H-Stop
    Z = none
  • Attenuators at amplifier input: none
    1H = 4dB
    X = 4dB
    Y = 0dB
    Z = 0dB
  • Cortab combinations done 3-27-2002 (mc) XWIN-NMR 3.0:
    1H: --> FCU 1+2, Mult, Mod, BLA, redone after amplifier change 1-13-2004
    13C:
    FCU 1+2, 500_1: Mult, Mod, BLA
    FCU 3+4, 300_5: Mult, Mod, BLA, 300_6, 500_1: BLA
    15N:
    FCU 1+2, 500_1: Mult, Mod, BLA
    FCU 3, 300_5: Mult, Mod, BLA, 300_6, 500_1: BLA
    Modify the file: /u/exp/stan/nmr/lists/cpd.hwt/cortab :
    At the end of the file add the line "jump to 1", add 4ms delay.
    Do this only for Amplifier Cortab!