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DEPT-135 experiment

PRELIMINARY SET-UP PARAMETER SET
Create a new dataset (new) and read the standard BRUKER parameter set (rpar) to record a DEPT-135 spectrum with rpar C13DEPT135 all (the pulse program dept135 can be visualized in the PulsProg section or with the edcpul command).

MODIFY SPECIFIC PARAMETERS
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.

See  90º 13C observe pulse and 90º 1H decouple pulse calibrations.

By default, the following parameters are set to: ns=128, ds=2, d1=2, d2=3.57ms, sw=331.2 and td=64k. Change them if required.

Optimize the values of o1 and sw from the conventional 13C spectrum if required. o2 must be set to the center of the proton spectrum.

ACQUISITION
Start acquisition by rga and zg (the expected experimental time is displayed with the expt command).
PROCESSING
The recorded data is Fourier transformed with ef (set lb=1) and automatic 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.
PLOT
Use the TOPSPIN plot editor (xwinplot)
OBSERVATIONS
It can be advisable to store all acquisition and processing parameters (with the command wpar) to be used later.

Both acquisition and processing steps can be performed using predefined automated AU programs. In this case, start data acquisition with the xaua command (the program executes the AU program defined in the acquisition parameters AUNM (au_zg135)) and the data can be automatically processed and plotted with the xaup command (the program executes the AU program defined in the processing parameter AUNMP (proc_cpd135).

This experiment can also by recorded in full automation mode using macros (edmac), BUTTON-NMR (buttonnmr) or ICON-NMR (iconnmr) . In automation applications the signal-to-noise ratio can be automatically optimized changing the acquisition AU program to AUNM=au_deptsino.

OTHER RELATED VERSIONS
 
Once the parameter set of the DEPT-355 experiment has been defined, DEPT-90 and DEPT-45 experiments can be run simply changing the pulse program:
  • For instance, to record a DEPT-90 spectrum, read the predefined parameter set of DEPT-135 experiment (rpar dept45 all), change the pulse program (pulprog=dept90) and start the acquisition (check for the number of scans, ns). These parameters can be stored for further use (wpar dept90 all). Process the spectrum as described above.
  • The same procedure should be followed to record a DEPT-45 spectrum: read the predefined parameter set of DEPT-135 experiment (rpar dept135 all), change the pulse program (pulprog=dept45) and start the acquisition (check for the number of scans, ns). These parameters can be stored for further use (wpar dept45 all).
  • Otherwhise, a single parameter set can be defined (wpar dept all) for recording any DEPT experiment. In such case, the pulse program is set to dept and the user must define the corresponding p0 (45, 90 or 135 degree 13C observe pulse) according to the carbon multiplicity selection.
  • Also see:

        1D 1H-decoupled carbon-13 spectrum


    Written by Teodor Parella
    Copyright © 1998-2008 BRUKER Biospin. All rights reserved.