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Standard 15N sensitivity test sample: 90% formamide in DMSO-d6.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 1H-decoupled 15N spectrum.
The calibration of the 15N sensitivity test is performed using the standard 1H-decoupled 15N parameter set (the pulse program is set to pulprog zgig). This test is performed using the inverse gated decoupling scheme in order to avoid the build up of NOE.MODIFY SPECIFIC PARAMETERS
It is very important to use a long recycle delay, usually d1=5*T1(15N) (for instance d1=500 s). Use a single scan (ns=1).ACQUISITIONSet p1 to the 90º 15N observe pulse at high power level pl1. This pulse is calibrated reaching the maximum signal for 90º and null point in 180º.
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 line to 0 ppm and plot the full spectrum.PLOT
Use the TOPSPIN plot editor (xwinplot) Plot the noise with a minimum amplitude of 1.5 cm over a minimum of 100 Hz.OBSERVATIONS
Written by Teodor Parella Copyright © 1998-2008 BRUKER Biospin. All rights reserved. |