Biomolecular NMR Facility at UT Southwestern

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Latest "Hard" Pulse Calibrations

Spectrometer
Date
pwH/tpwr
pwC/dpwr
pwN/dpwr2
pwD/dpwr3
Saturn500
4-20-09
6.8us/59
16.8us/61
34.5us/58
--
Artemis
4-21-09
6.6us/58
16.2us/58
46.5us/61
--
Pele500 (RT Probe) 3-27-08 5.5us/58 14.5us/63 37.0us/61 --
Pele500 (Cold Probe)
5-18-09
7.0us/51
12.6us/58
38.0us/58
--
Pele600 (RT Probe) 2-14-07 5.6us/56 14.0us/62 38.0us/61 --
Pele600 (Cold Probe)
12-12-06
7.2us/51
15.0us/59
34.0us/60
1) 190us/52

2) 340us/47

3) 510us/44

Apollo (RT Probe)
2-26-07
5.9us/58
14.0us/61
42.0us/62
--
Apollo (Cold Probe)
10-26-07
8.3us/50
13.0us/57
44.4us/60
--
Pele800 (RT Probe)
5-29-09
5.7us/59
10.6us/59
39.0us/59
1) 170us/48

2) 330us/43

3) 500us/40

Pele800 (Cold Probe) 4-12-07 8.0us/55 12.7us/55 37us/59 --
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

Spectrometer
Date
pwH/tpwr
pwC/dpwr
pwN/dpwr2
pwD/dpwr3
Saturn500 (RT Probe)
2-5-08
7.3us/59
14.8us/61
36.0us/58
--
Artemis (RT Probe)
1-30-08
6.9us/58
14.1us/58
44.0us/61
--
Pele500 (RT Probe) 3-27-08 6.4us/58 14.3us/63 40.0us/61
--
Pele500 (Cold Probe)
5-18-09
8.4us/51
11.5us/58
36.0us/58
--
Pele600 (RT Probe) 5-26-06 6.6us/56 14.0us/62 40.0us/61
--
Pele600 (Cold Probe)
12-7-07
7.6us/51
14.1us/59
38.0us/60
--
Apollo (RT Probe)
2-27-07
6.0us/58
14.2us/61
44.0us/62
--
Apollo (Cold Probe)
10-26-07
9.1us/51
13.8us/57
42.0us/60
200us/59
Pele800 (RT Probe)
5-29-09
6.8us/59
10.6us/59
36.0us/59
--
Pele800 (Cold Probe)
4-12-07
8.7us/57
12.4us/55
37.4us/59
200us/55
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Temperature Calibrations

Spectrometer
Date
Regression Analysis Formula*
Saturn500
4-26-05
VT = (Temp + 0.08286) / 1.0362
Artemis
4-18-05
VT = (Temp - 0.83497) / 0.94442
Pele500 (RT Probe)
10-2-06
VT = (Temp + 1.1712) / 1.0787
Pele500 (Cold Probe)
5-18-09
VT = (Temp - 4.1156) / 0.98387
Pele600 (RT Probe) 7-6-06 VT = (Temp - 0.31684) / 0.99389
Pele600 (Cold Probe)
5-18-09
VT = (Temp - 4.2587) / 0.97376
Apollo (RT Probe)
6-9-06
VT = (Temp - 1.4528) / 0.96393
Apollo (Cold Probe)
10-29-07
VT = (Temp - 0.1505) / 0.9625
Pele800 (RT Probe)
5-16-06
VT = (Temp - 1.9237) / 0.89521
Pele800 (Cold Probe)
4-13-07
VT = (Temp - 0.2738) / 0.9498
*Temperature in degrees Celcius
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Direct and Indirect* Referencing to DSS

Spectrometer
Date
1H
13C*
15N*
2H*
Pele500
6-9-06
tof=-2548.07Hz=0ppm, sfrq=499.725693MHz
dof=0Hz=97.5ppm, dfrq=125.668047MHz
dof2=0Hz=98.1ppm, dfrq2=50.641732MHz
dof3=0HZ=5.1ppm, dfrq3=76.711325MHz
Saturn500
11-3-05
tof=-2554.2 Hz=0ppm, sfrq=499.7602127MHz
dof=0Hz=97.6ppm, dfrq=125.676729MHz
dof2=0Hz=98.1ppm, dfrq2=50.6452312MHz
dof3=0Hz=5.1ppm, dfrq3=76.7166253MHz
Pele600
5-23-06
tof=-3097.5Hz=0ppm, sfrq=599.4476078MHz
dof=0Hz,92.1ppm, dfrq=150.744699MHz
dof2=0Hz=89.1ppm, dfrq2=60.746909MHz
dof3=0Hz,-0.02ppm, dfrq3=92.01933MHz
Apollo
6-8-06
tof=-3072.0Hz=0ppm, sfrq=599.775633MHz
dof=0Hz,92.0ppm, dfrq=150.827182MHz
dof2=0Hz=89.0ppm, dfrq2=60.780148MHz
dof3=0Hz=5.1ppm, dfrq3=92.06968MHz
Artemis
1-28-08
tof=-3083.8Hz=0ppm, sfrq=599.7095005MHz
dof=0Hz=92.0ppm, dfrq=150.8105541MHz
dof2=0Hz=89.1ppm, dfrq2=60.7734475MHz
dof3=0Hz=5.1ppm, dfrq3=92.0595304MHz
Pele800
5-16-06
tof=-4116.5Hz=0ppm, sfrq=800.4738662MHz
dof=0Hz=92.0ppm, dfrq=201.297307MHz
dof2=0Hz=89.1ppm, dfrq2=81.118536MHz
dof3=0Hz=5.1ppm, dfrq3=122.878241MHz
*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

Pele500
Pele600
Pele800
Apollo
Channel Reflected Power
1 7
2 13
3 189
4 25
Channel Reflected Power
1 8
2 33
3 97
4 67
Channel Reflected Power
1 --
2 --
3 --
4 --
Channel Reflected Power
1 1
2 39
3 10
4 43
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

Spectrometer Date S/N Ratio* S/N

Glucose

S/N

Salty Glucose

Line Shape+

55%, 0.55%, 0.11%

Line Shape+

Square Tube

Magnet Drift Rate
Saturn500 4-20-09 874:1 -- -- 0.77, 4.01, 4.53 -- 0.9 Hz/hr (5-3-07)
Artemis 4-21-09 1160:1 -- -- 0.86, 4.55, 7.33 -- 0.2 Hz/hr (1-5-07)
Pele500 (RT Probe) 3-27-08 678:1 -- -- 0.21,2.69,3.07 -- --
Pele500 (Cold Probe) 5-18-09 3258:1 630:1 -- 0.34, 4.77, 9.20 -- --
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) 5-29-09 1687:1 -- -- 0.66, 4.88, 5.35 -- 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 --
*0.1% Ethylbenzene in CHCl3, +1% CHCl3 in d6-Acetone, non-spin
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