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Bruker has put together a calibration routine which (1) automates the determination of the optimal O1 and P1, and (2) records a 1D proton spectrum of the sample (using the zgesgp pulse program). The AU program to launch is called calibo1p1. The program will run

• o1calib
• pulsecal
• run a 1-minute excitation sculpting 1D proton experiment (zgesgp)

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Then the values of O1 and P1 can be transferred retrieved by looking at the recording parameters in the resulting experiment (eda). Write them down and transfer them to the following experiments. You need to make sure you execute getprosol in the other experiments to calculate all the pulses based on P1.

getprosol 1H [P1 value in µs] [PLW1]W

For example, if the P1 value was determined to be 8.60 µs, you can use the following command (assuming that its corresponding power level is 12.614W): getprosol 1H 8.60 12.614W614W

Another advantage of the calibo1p1 program is that you can assess the quality of your sample by looking at the 1D proton spectrum it produces (see above). Well dispersed peaks, particularly in the amide protons region (6-10 ppm) are indicative of a diverse chemical environment around these hydrogen atoms, which typically correlates with the presence of structural elements.

Data acquisition

Once everything is locked, tuned, matched, shimmed and calibrated for optimal signal intensity and quality, it is time to load a new experiment. In the case of a 1D proton experiment, the default acquisition parameters for a protein sample are saved as PROT_1DESNIG. To load them in a new experiment, first create a new experiment using the new command. In the dialog box, select the acquisition parameters PROT_1DESNIG s

Processing

References

Benjamin Görling (Bruker) - 1D Acquisition