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note
-
Before any experiments could be run, all four lines had to be calibrated with respect to one another. All lines were calibrated by pushing 500, μL of water through the empty lines at a flow rate of 0.48 mL/min while acquiring spectra every 0.125 s corresponding to a spectrum every 1 μL. The spectrum with the first evidence of the water peak for each line was recorded and compared for all lines. The experiment was run 7 times for each line, and the lines were cut until the spectral appearances which occurred were within one unit (1 μL) of each other. The standard deviation of 7 runs was 2 μL units.
-
-
-
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37
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0141883644
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note
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2O was used as the sample because it has one, singlet peak from which the line width at half-height is easily measured. The line width of the glycine peak was used to gauge whether the sample was centered around the coil. If the sample was not centered and the air bubble on either end of the sample was within 0.5 cm of the coil, then the line width would broaden from its normal value of 1-2 Hz until the peak disappeared into the baseline. With a 25 μL sample, it was found that the push volume could fall within an 8 μL window, and the glycine line width would still be < 2 Hz for each coil. The windows for each line overlapped in the range of 121-128 μL. Thus, 125 μL of push solvent was used to center the samples.
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38
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58149365344
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Smallcombe, S. H.; Patt, S. L.; Keifer, P. A. J. Magn. Reson. A 1995, 117, 295-303.
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Keifer, P.A.3
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39
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0141952567
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note
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The Gaussian pulse width, transmitter power, and gradient strengths were determined. The pulse width and transmitter power were chosen to give a 90 degree pulse with a 1350 Hz excitation width at half-height and 8200 Hz at 1% height. The gradient was chosen to separate the centers of the spectral windows of neighboring coils by 9000 Hz. The reverse gradient strength was chosen to give the best S/N for each coil.
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-
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40
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0141918179
-
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note
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Currently, when the shim values are arrayed, an internal delay between scans results with the Varian INOVA spectrometer. The delay is 4-6 s/scan. When this problem is circumvented, the number of scans that can be performed for each sample in the 69 s window of analysis time can be increased from 1 to 5 without adding time to the automation method.
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41
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