602: 5mm CPQCI 1H-31P/13C/15N/D Z-GRD (Aug 2014) #Z132808/0002


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)
(There is no manual for QCI probe available yet)

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:

Nucleus Type Attenuation Channel 90deg Pulse Power [W] Calc. Date
1H -8.50 dB f1 9.0 us 7.08 W 12/20/19
waltz16 f1 70.0 us
TOCSY f1 26.0 us
ROESY f1 90.0 us
.
13C hard -20.65 dB f2 12.0 us 116.1 W 12/20/19
AcGly cpd -6.70 dB f2 60.0 us 4.68 W -6.67 dB 12/20/19
TOCSY -14.30 dB f2 25.0 us 26.9 W -14.27 dB 12/20/19
2nd cpd -3.70 dB f2 84.6 us 2.34 W -3.69 dB 12/20/19
low pow cpd -0.60 dB f2 120.0 us 1.15 W -0.65 dB 12/20/19
Het TOCSY med sens -7.90 dB f2 52.0 us 6.17 W -7.91 dB 12/20/19
Het TOCSY high sens -4.40 dB f2 78.0 us 2.75 W -4.39 dB 12/20/19
Het TOCSY super sens +5.90 dB f2 250.0 us 0.26 W +5.73 dB 12/20/19
.
15N hard -21.20 dB f3 32.0 us 131.8 W 12/20/19
-4.50 dB f3 220.0 us 2.82 W -4.45 dB 12/20/19
-1.50 dB f3 310.0 us 1.41 W -1.48 dB 12/20/19
-0.50 dB f3 350.0 us 1.12 W -0.42 dB 12/20/19
-13.60 dB f3 78.0 us 22.9 W -13.46 dB 12/20/19
.
31P hard -13.00 dB f1 40.0 us 19.95 Wfully T/M 9/16/17
+3.75 dB f1 250.0 us 0.42 W 9/16/17
-4.60 dB f4 100.0 us 2.88 W 9/16/17
+3.50 dB f4 250.0 us 0.44 W 9/16/17
.
2H -17.20 dB f1 68.0 us 52.5 W 9/15/17
Urea -5.40 dB f1 250 us 3.47 W 9/15/17

3. Soft Pulses:

Nucleus Type Channel Pulse Attenuation (Calculated) Power [W] Resonance Date
13C , Cali/CO; Q5_sebop.1 350us f2 90 deg -17.70 dB (-17.85)58.9 W on 12/20/19
Cali/CO Q5tr_sebop.1 350us f2 90 deg -17.80 dB (-17.85)60.3 W on 12/20/19
Q5.1000 1500us f2 90 deg -3.60 dB (-3.98)2.29 W on 12/20/19
Q5tr.1000 1500us f2 90 deg -3.95 dB (-3.98)2.48 W on 12/20/19
Cali/CO Q3_surbop.1 270us f2 180 deg -17.75 dB (-18.01)59.6 W on res 12/20/19
Ca sel Q3_surbop.1 1050us f2 180 deg -5.80 dB (-6.21)3.80 W on res 12/20/19
med sel Q3_surbop.1 740us f2 180 deg -8.95 dB (-9.25)7.85 W on res 12/20/19
Ca or Co dec Q3_surbop.1 810us f2 180 deg -8.15 dB (-8.47)6.53 W on res 12/20/19
13C direct detect
13C hard, 12us f1 -20.30 dB 107.2 W 8/29/14
Cali/CO Q5.1000 320us f1 90 deg -17.60 dB (-17.05)57.5 W on 8/29/14
Cali/CO Q5tr.1000 320us f1 90 deg -17.90 dB (-17.05)61.7 W on 8/29/14
Q5.1000 1500us f1 90 deg -3.70 dB (-3.63)2.34 W on 8/29/14
Q5.1000 1500us f1 90 deg -4.1 dB (-3.63)2.51 W on 8/29/14
Cali/CO Q3.1000 256us f1 180 deg -16.30 dB (-16.13)42.7 W on 8/29/14
Cali/CO Q3.1000 700us f1 180 deg -4.3 dB (-4.30)2.69 W
8/29/14
Cali/CO Q3.1000 1000us f1 180 deg -7.45 dB (-7.40)5.56 W
8/29/14

4. Miscellaneous:

Offset Ca - carbonyl (38 - 174ppm): 136 ppm
1H offset @ 4.7 pppm: 2820 Hz
Main Field: 600.21 MHz
BSMS Field: +1317 units (10-13-2003)
BSMS Field: -3891 units (03-03-2011)

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
    or:
    13C: AcGly in D2O: 13C-shift: 21.0ppm, J=128.0Hz, offset = 136ppm

  • Temperature: 298K
  • NO RF-Filters:
  • NO attenuators at amplifier input: none