Specifications of TCI CryoProbe
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Specifications of TCI CryoProbe on Bruker Avance 800 NMR Spectrometers PowerPoint PPT Presentation


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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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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


Specifications of tci cryoprobe on bruker avance 800 nmr spectrometers

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


Specifications of tci cryoprobe on bruker avance 800 nmr spectrometers

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


Specifications of tci cryoprobe on bruker avance 800 nmr spectrometers

3.  1H Sensitivity Test

SPECS: 6000:1

S/N = 7737:1 using 200 Hz noise range

= 6175:1 using 1 ppm noise range


Specifications of tci cryoprobe on bruker avance 800 nmr spectrometers

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%


Specifications of tci cryoprobe on bruker avance 800 nmr spectrometers

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


Specifications of tci cryoprobe on bruker avance 800 nmr spectrometers

6.  13C Sensitivity Test with Sample Rotation

S/N = 517:1

SPECS: 700:1

S/N = 982:1


Specifications of tci cryoprobe on bruker avance 800 nmr spectrometers

7.  Stability Test Using 3D HNCO

Stability test using 3D HNCO, which represents stability performance of

1H, 13C and 15N channels.


Specifications of tci cryoprobe on bruker avance 800 nmr spectrometers

8.  Sensitivity between CryoProbe (CP) TCI

and Room Temperature (RT) TXI probe

Water Suppression zgesgp pulse sequence is used.

Sensitivity enhancement: 1.8-fold


Specifications of tci cryoprobe on bruker avance 800 nmr spectrometers

First spectra of C-H HSQC

Sensitivity enhancement: 1.7-fold


Specifications of tci cryoprobe on bruker avance 800 nmr spectrometers

First spectra of N-H HSQC

Sensitivity enhancement: 1.8-fold


Specifications of tci cryoprobe on bruker avance 800 nmr spectrometers

Water Suppression zgesgp pulse sequence is used.

Sensitivity enhancement: 1.2-fold


Specifications of tci cryoprobe on bruker avance 800 nmr spectrometers

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


Specifications of tci cryoprobe on bruker avance 800 nmr spectrometers

10.  Comparison of 1D spectra of same experimental time

        acquired with 800 MHz CPTCI and 600 MHz RT TXI probe


Specifications of tci cryoprobe on bruker avance 800 nmr spectrometers

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


Specifications of tci cryoprobe on bruker avance 800 nmr spectrometers

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


Specifications of tci cryoprobe on bruker avance 800 nmr spectrometers

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.


Specifications of tci cryoprobe on bruker avance 800 nmr spectrometers

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.


Specifications of tci cryoprobe on bruker avance 800 nmr spectrometers

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.


Specifications of tci cryoprobe on bruker avance 800 nmr spectrometers

13. Some other spectra:


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