Probe Pulse Width Homogeneity Test

Direct-Observe Tests

Tune the probe on the test sample. Collect a spectrum and set the transmitter frequency on the peak to be observed. Measure the 180 degree pulse; divide this value in half to get the 90 degree pulse width. Measure the 450 degree and 810 degree pulse widthsss:
  1. Estimate the 450 and 810 degree pulse widths based upon the 90 degree pulse width
  2. Collect spectra with pulse widths that are shorter and longer than this estimate
  3. The spectrum with the largest peak height was collected with the 450 (or 810) degree pulse.
Nucleus Sample
1H 0.1% chloroform in acetone-d6
19F 0.05% trifluorotoluene in benzene-d6
31P 5mM triphenylphosphate in DMSO-d6
13C 40% p-dioxane in benzene-d6
15N 90% formamide in DMSO-d6
39K 0.2M KF in 10% D2O/90% H2O

Direct-Observe Specifications

Values are in units of microseconds.
Probe 1H 19F 31P13C 15N39K
I-500 HCN tri-axis< 8 --- --- --- --- --- ---
I-500 HCN Z-axis < 8 --- --- --- --- --- ---
I-500 HCX < 10 --- --- --- --- --- ---
I-500 BB --- --- --- --- --- --- ---
I-400 4nuc+ --- --- --- --- --- --- ---
I-400 5mm BB --- --- --- --- --- --- ---
I-400 10mm BB --- --- --- --- --- --- ---
I-400 Inv < 10 < 15 --- --- --- --- ---
Gem-300 quad < 15 < 20 < 12 --- --- --- ---
VXR-400 BB --- --- --- --- --- --- ---

Indirect-Observe Tests

Tune the probe on the test sample. Collect a 1H spectrum and set the transmitter frequency between the X-nucleus-labeled peaks to be observed. Measure the 180 degree pulse; divide this value in half to get the 90 degree pulse width. Perform the following experiment:
90(H) - 1/2JXH - pulse(X) - Acquire Measure the 180 degree pulse; divide this value in half to get the 90 degree pulse width. Measure the 450 degree and 810 degree pulse widthsss:
  1. Estimate the 450 and 810 degree pulse widths based upon the 90 degree pulse width
  2. Collect spectra with pulse widths that are shorter and longer than this estimate
  3. The spectrum with the largest peak height was collected with the 450 (or 810) degree pulse.
Nucleus Sample JXH
13C
15N

Direct-Observe Specifications

Values are in units of microseconds.
Probe 13C 15N
I-500 HCN tri-axis< 13 < 40
I-500 HCN Z-axis < 13 < 40
I-500 HCX < 22 < 30
I-400 Inv < 12 < 25
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Last updated: December 29, 1997
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