601: 5 mm CPTCI 1H-13C/15N/D Z-GRD (Nov 2010) #Z122990-0001

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 TCI 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 @ 35 usec

13C

 

hard pulse 6)

(max. length 360o)

12.0 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)

35.0 usec

GARP4 decoupling 7)

140 msec @ 170 usec

CPMG T2 9)

250 msec @ 52 usec (see warning 9))

2H

 

hard pulse

(max. length 360o)

68 usec

WALTZ16 decoupling

100 msec @ 250 usec

Z-Gradient

 

Absolute max. current 10)

10 A

Max. overall length 11)

10 ms @ 10A

 

Valid from the date of shipment: January first 2006

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' ' pldb1' , where p1 is the determined pulse length [us] at the power level PldB1 [dB].

    2. Hard Pulses:

    70.0 us 25.0 us 125.0 us
    Nucleus Type 90deg Pulse Channel Attenuation Power [W] Calc. Date
    1H 9.00 us f1 -9.00 dB 7.94 W 06/11/21
    salty samples 10.0 us f1
    waltz16 f1
    TOCSY f1
    ROESY f1
    .
    13C hard 12.0 us f2 -19.80 dB 95.5 W 06/11/21
    AcGly cpd 60.0 us f2 -5.85 dB 3.85 W -5.82 dB 06/11/21
    TOCSY 25.0 us f2 -13.40 dB 21.9 W -13.42 dB 06/11/21
    2nd cpd 84.6 us f2 -2.90 dB 1.95 W -2.84 dB 06/11/21
    low pow cpd 120.0 us f2 +0.20 dB 0.95 W +0.20 dB 06/11/21
    Het TOCSY med sens 52.0 us f2 -7.10 dB 5.13 W -7.06 dB 06/11/21
    Het TOCSY high sens 78.0 us f2 -3.60 dB 2.29 W -3.54 dB 06/11/21
    .
    15N hard 32.0 us f3 -22.00 dB 158.5 W 06/11/21
    220.0 us f3 -5.30 dB 3.39 W -5.25 dB 06/11/21
    310.0 us f3 -2.40 dB 1.74 W -2.28 dB 06/11/21
    350.0 us f3 -1.30 dB 1.35 W -1.22 dB 06/11/21
    78.0 us f3 -14.40 dB 27.5 W -14.26 dB 06/11/21
    .
    2H 68.0 us f1 -18.85 dB 76.7 W 10/29/20
    Urea 250.0 us f1 -8.70 dB 7.41 W -7.54 dB 10/29/20

    3. Soft Pulses:

    Nucleus Type Channel Pulse Attenuation [dB] Power [W] Resonance Date
    13C , Cali/CO Q5_sebop.1 350us f2 90 deg -16.50 dB (-17.10 dB)44.7 W on 06/11/21
    Cali/CO Q5tr_sebop.1 350us f2 90 deg -16.85 dB (-17.10)48.4 W on 06/11/21
    Cα Q5.1000 1500us f2 90 deg -3.00 dB (-3.23)2.00 W on 06/11/21
    Cα Q5tr.1000 1500us f2 90 deg -3.20 dB (-3.23)2.09 W on 06/11/21
    Cali/CO Q3_surbop.1 270us f2 180 deg -16.90 dB (-17.26)49.0 W on 06/11/21
    Cα sel Q3_surbop.1 1050us f2 180 deg -5.00 dB (-5.46)3.16 W on 06/11/21
    med sel Q3_surbop.1 740us f2 180 deg -8.20 dB (-8.50)6.61 W on 06/11/21
    Cα or CO dec Q3_surbop.1 810us f2 180 deg -7.40 dB (-7.72)5.50 W on 06/11/21
    13C direct detect
    13C hard, 12us f1 -19.15 dB 82.2 W 4/9/15
    Cali/CO Q5.1000 320us f1 90 deg -15.80 dB (-15.90)38.0 W on 4/9/15
    Cali/CO Q5tr.1000 320us f1 90 deg -16.00 dB (-15.90)39.8 W on 4/9/15
    Cα Q5.1000 1500us f1 90 deg -2.40 dB (-2.48)1.74 W on 4/9/15
    Cα Q5.1000 1500us f1 90 deg -2.60 dB (-2.48)1.82 W on 4/9/15
    Cali/CO Q3.1000 256us f1 180 deg -15.20 dB (-14.98)33.1 W on 0/9/15
    Cali/CO Q3.1000 1000us f1 180 deg -3.30 dB (-3.15)2.14 W on
    		4/9/15

    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: 600.21 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 = none
      X = none
      Y = none
      Z = none