|
The relaxation delay is the first step in any NMR experiment in which the initial equilibrium state is prepared to be modified by the effect of pulses and other delays. This period also defines the repetition rate of the experiment and must be taking in account when quantitative NMR work is required.REQUIREMENTS
Delays are executed by the pulse program commands d0-d31, defined in seconds. In particular, d1 is always used as the relaxation period.EXPERIMENTAL DETAILS
d1 is usually set to 1-5*T1 of the nuclei to be perturbated. Thus, in experiments starting from a 90º 1H pulse, d1 is set to 1-5*T1(1H). Usually d1 is set to 1-1.5 seconds for routine applications. On the other hand, in experiments starting from a 90º 13C pulse, d1 is set to 1-5*T1(13C) which can be longer when quaternary carbons are involved. The duration of d1 is very important to define the total experimental time of the NMR experiment to be recorded.SYNTAX
The standard way to implement the relaxation delay in a pulse program is very simple:RELATED TOPICSHowever, during the relaxation delay a series of specific settings are applied in order to achieve an specific goal. For instance:
...
d1
...In all these cases, the overall pre-scan duration will be defined by the addition of all delays existing between the end of the FID acquisition (see the go command in any pulse program) and the first pulse creating transverse magnetixation to be applied.
- Specific power levels, transmitter or decoupler offsets, lists definitions, ... to be used later can be defined during the relaxation period. Such settings only require minimum delays (often defined by the d12 command, 20 us).
- Specific perturbations as, for instance, Solvent presaturation.
- Broadband or selective 1H decoupling before a 90º 13C (or X) pulse, to improve sensitivity by means of heteronuclear NOE effects in heteronuclear experiments.
Some examples: