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I need to set up 2H NMR on a Bruker 600 MHz BBO probe for the first time. Can anyone give me a set of instructions? Do I run in protonated or deuterated solvent? How do I tune 2H on the BB channel? What 2H values do I need in the edprosol table? What pulse program? What hardware connections or disconnections, e.g. removing the 2H stop filter.... |
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Hi, if you want to measure 2H you should use a protonated solvent, otherwise you will get a huge solvent peak in your 2H spectrum and your (presumably) tiny substance signals will suffer from the small dynamic range that is left for them. For shimming purposes you could manually lock on the signal of the deuterons in your sample. Once you have shimmed your sample you should turn off lock and sweep and remove the 2H stop filter from the preamplifier. Change the nucleus in edasp to 2H and tune the BB channel to 2H. If the tune/match settings for 2H are not indicated on your probe, you should tune to the indicated values of a nucleus close in frequency to 2H and then change the tuning/matching gradually until you reach the final 2H frequency. There should be no need to change anything in the edprosol table. After you successfully matched/tuned your probe, you determine the pulse lengths for a given powerlevel and use these values in your pulse program. For 2H, the procedure to do this is not different than for any other nucleus. The same is true for the pulse program. For a normal single-pulse and acquisition experiment you simply use "zg". If the experiment time is rather long, please bear in mind that due to the absence of the lock your frequencies might drift. This will decrease the quality of those spectra. Another tip: If the line-width is not of concern and you simply want a 1D 2H spectrum, you could also just acquire a spectrum via the lock channel. Then no retuning of the BB channel is necessary. |
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Use the lock channel is the easiest way to start, in this case you should use zg2h pulse prog instead of zg |
