602: 5 mm CPTXI 1H/2H-13C/15N Z-GRD (Apr 2002) #Z44866-0009

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!

IMPORTANT POWER REFERENCES FOR CRYOPROBES (full document)

4.2 Pulse and power recommendations

 

Note: All values require a minimum repetition period d1 +aq of 1sec 2)

Important: observe the separate notes on the foIIowing pages!

Important: Be CAREFUL when pushing these limits!

 

 

5mm 600 MHz TXI CryoProbe TM

1H

 

Hard pulse 3)

(max. length 360o)

8 usec

Hard pulse for lossy sample

Power level corresponding to 8.0 usec pulse for non-lossy samples

trim pulse p28 4)

2 msec @ 10 usec

TOCSY spin lock

200 msec @ 25 usec

400 msec @ 35 usec

ROESY spin lock

Up to CW for power level

corresponding to a 100 usec pulse

WALTZ 16 decoupling

during 13C-detection

Up to CW for power level corresponding to a 100 usec pulse

DIPSI2-decoupling in triple resonance

400 msec @ 50 usec

13C

 

hard pulse 6)

(max. length 360o)

15.0 usec

trim pulse 5)

2msec @ 25 usec

CC spin lock 5)

20msec @ 25 usec

GARP decoupling 7)

140msec @ 55 usec

selective pulses 8)

Q5: 320 usec

Q3: 256 usec

CHIRP: 2ms @ 25 usec

15N

 

hard pulse 6)

(max. length 360o)

40.0 usec

GARP4 decoupling 7)

140 msec @ 170 usec

CPMG T2 9)

250 msec @ 80 usec (see warning 9))

2H

 

hard pulse

(max. length 360o)

150 usec

WALTZ16 decoupling

100 msec @ 250 usec

Z-Gradient

 

Absolute max. current 10)

10 A

Max. overall length 11)

10 ms @ 10A

 

Date: 13.02.2003

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 -4.5 dB f1 8.70 us 100W 10/04/10
    waltz16 f1 70.0 us 100W
    TOCSY f1 25 us 100W
    ROESY f1 125.0 us 100W
    .
    13C hard -5.20 dB f2 15.0 us 300W 10/04/10
    AcGly TOCSY -3.40 dB f2 20.0 us 300W dB 10/04/10
    AcGly TOCSY -1.80 dB f2 25.0 us 300W dB 10/04/10
    TOCSY +0.20 dB f2 32.0 us 300W dB 10/04/10
    Dec +6.40 dB f2 65.0 us 300W dB 10/04/10
    LowDec 1 +8.25 dB f2 80.0 us 300W dB 10/04/10
    LowDec 2 +14.20 dB f2 160.0 us 300W dB 10/04/10
    .
    15N hard -4.45 dB f3 45.0 us 300W 10/04/10
    +0.80 dB f3 90.0 us 300W dB 10/04/10
    +8.65 dB f3 200.0 us 300W dB 10/04/10
    .
    2H -2.7 dB 2HTX 150 us 20W 12/21/09
    AcGly + 8.20 dB 2HTX 300 us 20W dB 12/21/09

    3. Soft Pulses:

    Nucleus Type Channel Pulse Attenuation Amplifier Resonance Date
    13C , Cali/CO Q5.1000 320us f2 90 deg -4.20 dB300W on/off 6/8/10
    Cali/CO Q5tr.1000 320us f2 90 deg -4.30 dB300W on 6/8/10
    Cali/CO Q5.1000 410us f2 90 deg -2.50 dB300W on 6/8/10
    Cali/CO Q5tr.1000 410us f2 90 deg -2.70 dB300W on 6/8/10
    Cα Q5.1000 1500us f2 90 deg +8.50 dB300W on 6/8/10
    Cα Q5tr.1000 1500us f2 90 deg +8.70 dB300W on 6/8/10
    Cali/CO Q3.1000 256us f2 180 deg -3.50 dB300W on 6/8/10
    Cali/CO Q3.1000 256us f2 180 deg -3.50 dB300W off(-136ppm) 6/8/10
    CO Q3.1000 360us f2 180 deg -0.55 dB300W on 6/8/10
    Cali/CO Q3.1000 360us f2 180 deg -0.50 dB300W off(-136ppm) 6/8/10
    CO dec Q3.1000 768us f2 180 deg +5.90 dB300W on 6/8/10
    Cα Q3.1000 1000us f2 180 deg +8.45 dB300W on 6/8/10
    CO Sinc1.1000 160us f2 90 offs=0ppm +9.30 dB300W dB 06/27/06
    CO Sinc1.1000 160us f2 90 offs=136ppm +9.30 dB300W dB 06/27/06
    CO Sinc1.1000 160us f2 180 offs=0ppm +3.60 dB300W dB 06/27/06
    CO Sinc1.1000 160us f2 180 offs=136ppm +3.60 dB300W dB 06/27/06
    Seduce seduce1c6 330us delta=119ppm f2 90 offs=119ppm +7.50 dB300W dB 06/27/06
    seduce1c6 300us delta=132ppm f2 90 offs=132ppm +6.60 dB300W dB 06/27/06
    seduce1c6 284us delta=140ppm f2 90 offs=140ppm +6.20 dB300W dB 06/27/06
    adiabatic:α+β hsec.3 500us f2 180 deg + dB300W
    adiabatic: CO sech1024_4.8 600us f2 180 deg +dB300W
    1H sinc1.1000 1.1ms f1 180 deg dB100W

    4. Miscellaneous:

    Magic angle on GREAT III: factor Z/XY = N/A
    Offset Ca - carbonyl (56 - 175ppm): -18109 Hz
    1H offset @ 4.7 pppm: 2820 Hz
    Main Field: 600.13 MHz
    BSMS Field: -432 units (10-10-2003)

    5. Conditions for pulse determination:

    • Sample: 13C, 15N labled Urea in DMSO
      13C-shift: 48.5ppm, J=138.5Hz
      15N-shift: 76.0ppm, J=88.5Hz
      Acetyl Glycine 13C/15N, in D2O
      X-pulses: 13C, 15N labled Acetyl Glycine
      13C-shift: 22.1ppm, J=128.6Hz (1H 1.96 ppm )
      15N-shift: 76.0ppm, J=88.5Hz
    • Temperature: 298K
    • RF-Filters: none
    • Attenuators at amplifier input:
      1H =12dB
      X = 3dB
      Y = 5dB
      Z = 0dB