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Biomolecular NMR Facility at UT Southwestern
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Latest "Hard" Pulse Calibrations
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Spectrometer
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Date
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pwH/tpwr
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pwC/dpwr
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pwN/dpwr2
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pwD/dpwr3 |
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Saturn500
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2-5-08
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7.0us/59
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16.1us/61
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35.0us/58
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-- |
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Artemis
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1-31-08
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6.1us/58
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15.0us/58
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45.0us/61
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-- |
| Pele500 (RT Probe) |
3-27-08 |
5.5us/58 |
14.5us/63 |
37.0us/61 |
-- |
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Pele500 (Cold Probe)
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5-22-07
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7.4us/51
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13.0us/59
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35.5us/59
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1) 185us/49
2) 340us/44
3) 520us/41
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| Pele600 (RT Probe) |
2-14-07 |
5.6us/56 |
14.0us/62 |
38.0us/61 |
-- |
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Pele600 (Cold Probe)
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12-12-06
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7.2us/51
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15.0us/59
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34.0us/60
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1) 190us/52
2) 340us/47
3) 510us/44
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Apollo (RT Probe)
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2-26-07
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5.9us/58
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14.0us/61
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42.0us/62
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-- |
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Apollo (Cold Probe)
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10-26-07
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8.3us/50
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13.0us/57
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44.4us/60
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-- |
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Pele800 (RT Probe)
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1-15-07
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5.3us/59
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9.4us/60
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35.0us/60
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1) 170us/48
2) 330us/43
3) 500us/40
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| Pele800 (Cold Probe) |
4-12-07 |
8.0us/55 |
12.7us/55 |
37us/59 |
-- |
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These calibrations were performed with the following samples and experiments:
- 13C: 100mM Sodium acetate in 10% D2O/H2O, hetcal_echorm
- 15N: 0.1% 15N-Benzamide in d6-DMSO, hetcal_echo_lek2
- 1H: 4Hz Dopped 1% H2O in D2O, s2pul
- 2H: 40% p-dioxane / 60% d6-benzene, hetcal_echo_lek3
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Automated BioPack Calibrations
Sample: 0.5 mM U-13C,15N-GB1 protein, 25 C
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Spectrometer
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Date
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pwH/tpwr
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pwC/dpwr
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pwN/dpwr2
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pwD/dpwr3
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Saturn500 (RT Probe)
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2-5-08
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7.3us/59
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14.8us/61
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36.0us/58
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--
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Artemis (RT Probe)
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1-30-08
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6.9us/58
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14.1us/58
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44.0us/61
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--
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| Pele500 (RT Probe) |
3-27-08 |
6.4us/58 |
14.3us/63 |
40.0us/61 |
--
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Pele500 (Cold Probe)
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9-7-07
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8.8us/51
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11.5us/59
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34.0us/59
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--
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| Pele600 (RT Probe) |
5-26-06 |
6.6us/56 |
14.0us/62 |
40.0us/61 |
--
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Pele600 (Cold Probe)
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12-7-07
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7.6us/51
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14.1us/59
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38.0us/60
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--
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Apollo (RT Probe)
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2-27-07
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6.0us/58
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14.2us/61
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44.0us/62
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--
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Apollo (Cold Probe)
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10-26-07
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9.1us/51
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13.8us/57
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42.0us/60
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200us/59
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Pele800 (RT Probe)
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5-16-06
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6.6us/59
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9.4us/60
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35.0us/60
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--
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Pele800 (Cold Probe)
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4-12-07
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8.7us/57
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12.4us/55
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37.4us/59
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200us/55
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Temperature Calibrations
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Spectrometer
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Date
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Regression Analysis Formula*
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Saturn500
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4-26-05
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VT = (Temp + 0.08286) / 1.0362
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Artemis
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4-18-05
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VT = (Temp - 0.83497) / 0.94442
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Pele500 (RT Probe)
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10-2-06
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VT = (Temp + 1.1712) / 1.0787
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Pele500 (Cold Probe)
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7-28-06
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VT = (Temp + 0.86682) / 0.98269
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| Pele600 (RT Probe) |
7-6-06 |
VT = (Temp - 0.31684) / 0.99389 |
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Pele600 (Cold Probe)
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6-7-06
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VT = (Temp - 0.91071) / 0.95857
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Apollo (RT Probe)
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6-9-06
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VT = (Temp - 1.4528) / 0.96393
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Apollo (Cold Probe)
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10-29-07
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VT = (Temp - 0.1505) / 0.9625
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Pele800 (RT Probe)
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5-16-06
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VT = (Temp - 1.9237) / 0.89521
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Pele800 (Cold Probe)
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4-13-07
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VT = (Temp - 0.2738) / 0.9498
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*Temperature in degrees Celcius |
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Direct and Indirect* Referencing to DSS
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Spectrometer
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Date
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1H
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13C*
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15N*
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2H*
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Pele500
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6-9-06
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tof=-2548.07Hz=0ppm, sfrq=499.725693MHz
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dof=0Hz=97.5ppm, dfrq=125.668047MHz
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dof2=0Hz=98.1ppm, dfrq2=50.641732MHz
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dof3=0HZ=5.1ppm, dfrq3=76.711325MHz
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Saturn500
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11-3-05
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tof=-2554.2 Hz=0ppm, sfrq=499.7602127MHz
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dof=0Hz=97.6ppm, dfrq=125.676729MHz
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dof2=0Hz=98.1ppm, dfrq2=50.6452312MHz
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dof3=0Hz=5.1ppm, dfrq3=76.7166253MHz
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Pele600
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5-23-06
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tof=-3097.5Hz=0ppm, sfrq=599.4476078MHz
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dof=0Hz,92.1ppm, dfrq=150.744699MHz
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dof2=0Hz=89.1ppm, dfrq2=60.746909MHz
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dof3=0Hz,-0.02ppm, dfrq3=92.01933MHz
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Apollo
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6-8-06
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tof=-3072.0Hz=0ppm, sfrq=599.775633MHz
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dof=0Hz,92.0ppm, dfrq=150.827182MHz
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dof2=0Hz=89.0ppm, dfrq2=60.780148MHz
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dof3=0Hz=5.1ppm, dfrq3=92.06968MHz
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Artemis
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1-28-08
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tof=-3083.8Hz=0ppm, sfrq=599.7095005MHz
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dof=0Hz=92.0ppm, dfrq=150.8105541MHz
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dof2=0Hz=89.1ppm, dfrq2=60.7734475MHz
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dof3=0Hz=5.1ppm, dfrq3=92.0595304MHz
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Pele800
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5-16-06
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tof=-4116.5Hz=0ppm, sfrq=800.4738662MHz
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dof=0Hz=92.0ppm, dfrq=201.297307MHz
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dof2=0Hz=89.1ppm, dfrq2=81.118536MHz
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dof3=0Hz=5.1ppm, dfrq3=122.878241MHz
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*Indirect referencing: 13C = 0.251449530, 15N=0.101329118, 2H=0.153506088
Example: to set dof=174ppm in Saturn500: (174-97.6)*125.676729 = 9601.7 Hz
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Typical Reflected Powers for Cold Probes
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Pele500
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Pele600
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Pele800
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Apollo
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| Channel |
Reflected Power |
| 1 |
7 |
| 2 |
13 |
| 3 |
185 |
| 4 |
25 |
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| Channel |
Reflected Power |
| 1 |
8 |
| 2 |
33 |
| 3 |
97 |
| 4 |
67 |
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| Channel |
Reflected Power |
| 1 |
-- |
| 2 |
-- |
| 3 |
-- |
| 4 |
-- |
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| Channel |
Reflected Power |
| 1 |
1 |
| 2 |
39 |
| 3 |
10 |
| 4 |
43 |
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These values are for the following sample: 0.5mM 15N,13C-GB1, 50 mM NaPi, 50 mM NaCl, pH=6.5
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Signal-to-noise Ratios, Line Shape Analysis, and Magnet Drift Rate
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| Spectrometer |
Date |
S/N Ratio* |
S/N
Glucose
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S/N
Salty Glucose
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Line Shape+
55%, 0.55%, 0.11%
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Line Shape+
Square Tube
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Magnet Drift Rate |
| Saturn500 |
2-5-08 |
870:1 |
-- |
-- |
0.54, 6.12, 7.57 |
-- |
0.9 Hz/hr (5-3-07) |
| Artemis |
1-31-08 |
1226:1 |
-- |
-- |
0.67, 7.70, 9.43 |
-- |
0.2 Hz/hr (1-5-07) |
| Pele500 (RT Probe) |
3-27-08 |
678:1 |
-- |
-- |
0.21,2.69,3.07 |
-- |
-- |
| Pele500 (Cold Probe) |
5-22-07 |
3245:1 |
542:1 |
-- |
0.47, 5.31, 6.01 |
-- |
-- |
| Pele600 (RT Probe) |
2-14-07 |
931:1 |
-- |
-- |
0.67,7.92,9.75 |
-- |
9Hz/hr (5-23-06) |
| Pele600 (Cold Probe) |
5-31-07 |
4150:1 |
-- |
-- |
0.91, 8.82, 13.59 |
-- |
-- |
| Apollo (RT Probe) |
2-26-07 |
1092:1 (P4926) |
-- |
-- |
0.71, 7.51, 9.43 |
-- |
0.3Hz/hr (2-13-07) |
| Apollo (Cold Probe) |
10-30-07 |
4605:1 |
675:1 |
345:1 |
0.55, 4.68, 9.36 |
0.76, 6.02, 10.62 |
-- |
| Pele800 (RT Probe) |
1-15-07 |
1688:1 |
-- |
-- |
0.68, 4.82, 6.00 |
-- |
1.7 Hz/hr |
| Pele800 (Cold Probe) |
4-12-07 |
5300:1 |
906:1 |
506:1 |
0.75, 5.86, 10.48 |
0.67, 3.78, 9.43 |
-- |
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*0.1% Ethylbenzene in CHCl3, +1% CHCl3 in d6-Acetone, non-spin |
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