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Removal of Paramagnetic Ions Prior to Analysis of Organic Reactions in Aqueous Solutions by NMR Spectroscopy

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journal contribution
posted on 28.05.2021, 19:16 by Rio Febrian, Joseph P. Roddy, Christine H. Chang, Clinton T. Devall, Paul J. Bracher
This article describes a method for improving 1H NMR spectra of aqueous samples containing paramagnetic metals by precipitation of metal cations with a variety of counteranions. The addition of hydroxide, phosphate, carbonate, and arsenate to solutions of transition metals such as Fe2+ and Mn2+ can reduce line broadening and improve the ability of a spectrometer to lock on the signal of deuterium. The method is most effective under strongly alkaline conditions, and care must be taken to observe whether the organic substrates undergo side reactions or are themselves removed from solution upon addition of the precipitating salts. As a demonstration of the practical value of the method, we show that NMR spectroscopy can be used to monitor the transition-metal-mediated hydrolysis of glycylglycine (Gly2).