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Create a new dataset (new) and read the standard BRUKER parameter set (rpar) to record T1 1H measurements with rpar PROTONT1 all (the pulse program t1ir can be visualized in the PulsProg section or with the edcpul command).MODIFY SPECIFIC PARAMETERSOtherwhise, from the reference 1H spectrum create a new dataset with edc or iexpno and change the pulse program to pulprog t1ir. All required parameters are as described for the 1H spectrum. The inversion-recovery experiment is recorded as a 2D data set in which a delay (vd) is varied over the course of the experiment. For this reason, change parmod to 2D in eda. A 1D 1H spectrum is obtained for each value of vd that can be readed using the corresponding rser command.
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.ACQUISITIONDefine a vd-list by typing, for instance, edlist vd t1delay. Enter the desired delays (in seconds) as, for instance:
10sand include it in the acquisition parameters by typing vdlist t1delay.
5s
4s
3s
3s
2s
1s
0.5s
0.25s
0.1s
0.01sIt is very important to use a long recycle delay, usually d1=5*T1(1H) (d1=10 s), and l4=td1 is the number of experiments (or number of delays in vd-list).
Start acquisition by rga and zg (the expected experimental time is displayed with the expt command). (minimum number of scans ns=8 and ds=4).PROCESSING
The spectra can be processed by the automation program proc_t1 or manually entering xf2. In all cases, set SI1 as a power of two greater than or equal to the number of delays in vdlist (SI1=16). A linebroadening is usually applied (lb=1 Hz). More details in T1 calculation.PLOT
Use the TOPSPIN plot editor (xwinplot)AUTOMATION
It is advisable to store all acquisition and processing parameters (for instance, with the command wpar t1ir all) to be used later. It can be advisable to store all acquisition and processing parameters (with the command wpar) to be used later.OTHER RELATED VERSIONSBoth 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_zg)) 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_2dt1).
This experiment can also by recorded in full automation mode using macros (edmac), BUTTON-NMR (buttonnmr) or ICON-NMR (iconnmr)
The same experiment using a fix interpulse delay is also available (pulprog t1ir1d) to be used by the au-program invrec_au.
Also see: 13C T1 measurements using the Inversion-Recovery experiment
Written by Teodor Parella Copyright © 1998-2008 BRUKER Biospin. All rights reserved. |