I have deuterated ferrocene and wish to find out the D content of my product. Can I use HR-ESI MS data for this purpose directly? Or, should I use some kind of internal standard? If yes, what would be most suitable?
HR-ESI MS is a good option. You may directly check the mass difference of 1 or multiples of 1 depending on the number of deuterium atoms that were exchanged. If you are not able to differentiate, you may better try MALDI-TOF MS. Here the things will be much more clear. If you still fail to observe a difference, you may finally check with EDX analysis. Still if you dont see it, it means your sample has not been deuterated.
I assume it shouldn't be straightforward to characterize it with ESI-MS. Of course you should able to compare the isotope pattern of the deuterated ferrocene with regular ferrocene and see how many amu it is bigger. But for that you need to ensure that there is not H/D scrambling between the ferrocene and your solvent. So you need a completely deutrated solvent. But, if by any chance your ferrocene is not 100% deutrated, again any likely H in it may replace by D from solvent (the same problem can happen in 1H NMR). Overall, I don't know how conclusive the result of ESI will be. I think MALDI is a better choice.
I completely agree with Dr. Pach. ESI is much too soft to characterize ferrocene for deuteration, not to mention just absolutely the wrong technique. Proton NMR is clearly the best choice in this case
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