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Standard line shape test sample: 60% benzene/40% p-dioxane.PARAMETER SETInsert the sample (ij). Choose the solvent deuterium signal with the lock command Tune and match the probehead (wobb or atma if required). Optimize the shim procedure (read an optimized shim file with the rsh command or performs a gradshim if required). Record a conventional 1H spectrum. Record a conventional 13C spectrum.
The calibration of the 13C line shape is performed using the standard C13HUMP parameter set (the pulse program is set to pulprog zgcw30). The width of the benzene resonance line is measured at the height of 0.55% and 0.11%.MODIFY SPECIFIC PARAMETERS
The test is usually performed using a sample spinning rate of 20 Hz. Update the corresponding pulses and power levels in the acquisition parameters according to the selected solvent/probehead parameters by executing the getprosol command (pulses and power levels must be correctly set by the edprosol command). If required, any acquisition parameter can be modified manually or in the AcquPars section.ACQUISITIONo1 and o2 are set on resonance of the 13C and 1H benzene resonances, respectively.
Set p1 to the 90º 13C observe pulse and pl14 to the low power level for 1H decoupler pulse decoupler attenuation for continuous wave decoupling.
Start acquisition by rga and zg (the expected experimental time is displayed with the expt command).PROCESSING
The recorded data is Fourier transformed with ft (or ef) and phase and baseline corrections are performed using apk and abs, respectively. Modify processing parameters if required from the ProcPars section or using the ased command.. Reference the benzene line to 0.0 Hz.PLOT
Use the TOPSPIN plot editor (xwinplot) Plot from 7 to -8 Hz with a CX=15 cm (1.0 Hz/cm) and a CY=1000 cm. Determine the lineshape at 5.5 cm and 1.1 cm height. The plot window must also show the spinning sidebands.OBSERVATIONS
Written by Teodor Parella Copyright © 1998-2008 BRUKER Biospin. All rights reserved. |