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Specifications of TCI CryoProbe on Bruker Avance 800 NMR Spectrometers

Specifications of TCI CryoProbe on Bruker Avance 800 NMR Spectrometers. Presented by Dr. Youlin Xia at UH, on 5/8/06. 1. 1 H Hump Test with Sample Rotation. SPECS of hump: 8/16 Hz SPECS of resolution: 0.8 Hz. Resolution = 0.52 @ 50% height. 4.7 Hz @ 5.5% height.

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Specifications of TCI CryoProbe on Bruker Avance 800 NMR Spectrometers

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  1. Specifications of TCI CryoProbe on Bruker Avance 800 NMR Spectrometers Presented by Dr. Youlin Xia at UH, on 5/8/06

  2. 1. 1H Hump Test with Sample Rotation SPECS of hump: 8/16 Hz SPECS of resolution: 0.8 Hz Resolution = 0.52 @ 50% height 4.7 Hz @ 5.5% height 9.7 Hz @ 1.1% height

  3. 2.  1H Hump Test without Sample Rotation Resolution = 0.82 @ 50% height SPECS of hump: 12/24 Hz SPECS of resolution: 1 Hz 7.1 Hz @ 5.5% height 10.8 Hz @ 1.1% height

  4. 3.  1H Sensitivity Test SPECS: 6000:1 S/N = 7737:1 using 200 Hz noise range = 6175:1 using 1 ppm noise range

  5. 4.  Sucrose Sensitivity and Water Suppression SPECS of hump: 150/300 Hz Sensitivity: 792-1027 from survey 66.7 Hz @ 50% height of DSS S/N= 963:1 140.9 Hz @ 10% height of DSS 24%

  6. 5.  13C Hump Test with Sample Rotation Resolution = 0.37 Hz @ 50% height SPECS of hump: 6/10 Hz SPECS of resolution: 0.6 Hz This is a real peak, not from shimming. 1.9 Hz @ 5.5% height 5.1 Hz @ 1.1% height

  7. 6.  13C Sensitivity Test with Sample Rotation S/N = 517:1 SPECS: 700:1 S/N = 982:1

  8. 7.  Stability Test Using 3D HNCO Stability test using 3D HNCO, which represents stability performance of 1H, 13C and 15N channels.

  9. 8.  Sensitivity between CryoProbe (CP) TCI and Room Temperature (RT) TXI probe Water Suppression zgesgp pulse sequence is used. Sensitivity enhancement: 1.8-fold

  10. First spectra of C-H HSQC Sensitivity enhancement: 1.7-fold

  11. First spectra of N-H HSQC Sensitivity enhancement: 1.8-fold

  12. Water Suppression zgesgp pulse sequence is used. Sensitivity enhancement: 1.2-fold

  13. 9.  Dependence of Signal on Salt Concentration S/N=527:1 200 mM NaCl, p1=15.75s S/N=650:1 100 mM NaCl, p1=13.40s 50 mM NaCl, p1=11.62s S/N=837:1 S/N=1272:1 10 mM NaCl, p1=10.25s

  14. 10.  Comparison of 1D spectra of same experimental time         acquired with 800 MHz CPTCI and 600 MHz RT TXI probe

  15. Comparison of NOESY of similar sensitivity but different experimental time, acquired with 800 MHz CPTCI and 600 MHz TXI (next slide) probes: there are about 4-fold sensitivity enhancement

  16. Comparison of NOESY of similar sensitivity but different experimental time, acquired with 800 MHz CPTCI (previous slide) and 600 MHz TXI probes: there are about 4-fold sensitivity enhancement

  17. 11.  Linearity Test of 1H Power amplifiers Sample: 0.1% EB in CDCl3 For 1H channel, 1H decoupling power level (~10 dB) in triple resonance experiments and power level for water suppression (~30 dB) are calculated based on pulse width, power level of 90 hard pulse and a linear power amplifier. So from the above table, it looks like that the calculation of 1H decoupling power level is ok, but the calculation of water suppression power level is not good and we need to calibrate the power level.

  18. Linearity test of 13C Power amplifier: Sample: 60% C6D6 in p-dioxane 13C channel has a lot of shaped pulses. The power levels of these shaped pulses all are calculated based on pulse width, power level of 90 hard pulse and a linear power amplifier. It looks like the linearity of 13C is better than that of 1H. So I suppose the 13C channel is ok. Linearity test of 15N Power amplifier: There is no shaped pulse with 15N channel. The power level of 15N-decoupling is calculated based on pulse width, power level of 90 hard pulse and a linear power amplifier. I think this is ok.

  19. 12.  Test of Temperature Gradient Within A Sample Principal: http://calmarc3.cchem.berkeley.edu/archives/ammrl/93/archive/0078.html The temperature gradient within the sample is less than 0.2 C.

  20. 13. Some other spectra:

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