title: Solid-state natural abundance 25Mg NMR studies of Na2MgEDTA x 4 H2O--a possible new reference compound for 25Mg NMR spectroscopy.
abstract: Natural abundance solid-state (25)Mg NMR measurements were made of the disodium salt of magnesium ethylenediaminetetraacetate tetrahydrate (Na(2)MgEDTA x 4 H(2)O). Both magic angle spinning (MAS) and static experiments were employed to determine the quadrupole coupling constant (C(q)) and the asymmetry parameter (eta(q)) of the electric field gradient (EFG) tensor associated with (25)Mg in this compound, giving the values C(q) = 1.675(5) MHz and eta(q) = 0.15(1). The isotropic chemical shift was determined to be delta(iso) = 0.25(10) ppm (relative to 11 M MgCl(2) aqueous solution) and a small chemical shift anisotropy (CSA) contribution (approximately -13 ppm) was detected, one of the first CSA reports in (25)Mg NMR. This compound exhibited remarkably good (25)Mg NMR sensitivity, due to its fast spin-lattice relaxation and modest quadrupole coupling, which allowed its use as a secondary shift reference and as a test sample for the implementation and optimisation of signal-enhancement methods in (25)Mg NMR spectroscopy, such as double frequency sweeps (DFS) and the use of adiabatic hyperbolic secant (HS) and WURST pulses.
authors.affiliation: Departamento de Física, Universidade Federal do Espírito Santo, 29075-910 Vitória, ES, Brazil. jair@npd.ufes.br
authors.forename: Jair C C
authors.initials: JC
authors.lastname: Freitas
authors.forename: Alan
authors.initials: A
authors.lastname: Wong
authors.forename: Mark E
authors.initials: ME
authors.lastname: Smith
mesh_terms: D004492:Edetic Acid; D007554:Isotopes; D008274:Magnesium; D009682:Magnetic Resonance Spectroscopy / Q000379:methods* / Q000592:standards; D012015:Reference Standards
chemical_list: D007554:Isotopes; D004492:Edetic Acid; D008274:Magnesium