Matrix-assisted diffusion-ordered spectroscopy: choosing a matrix.
Diffusion-ordered spectroscopy (DOSY) is an important technique for separating the NMR signals of the components in a mixture, and relies on differences in diffusion coefficient. Standard DOSY experiments therefore struggle when the components of a mixture are of similar size, and hence diffuse at similar rates. Fortunately, the diffusion coefficients of solutes can be manipulated by changing the matrix in which they diffuse, using matrix components that interact differentially with them, a technique known as matrix-assisted DOSY. In the present investigation, we evaluate the performance of a number of new, previously used, and mixed matrices with an informative test mixture: the three positional isomers of dihydroxybenzene. The aim of this work is to present the matrix-assisted DOSY user with information about the potential utility of a set of matrices (and combinations of matrices), including ionic and non-ionic surfactants, complexing agents, polymers, and mixed solvents. A variety of matrices improved the diffusion resolution of the signals of the test system, with the best separation achieved by mixed micelles of sodium dodecyl sulfate and cetyl trimethylammonium bromide. The use of mixed matrices offers great potential for the analyst to tailor the matrix to a particular sample under study. © 2016 The Authors Magnetic Resonance in Chemistry Published by John Wiley & Sons, Ltd.
Departamento de Química Orgânica e Inorgânica, Centro de Ciências, Universidade Federal do Ceará, CP 12 200, CEP 60455-970, Fortaleza, Brazil.
Nilce V
NV
Gramosa
Departamento de Química Orgânica e Inorgânica, Centro de Ciências, Universidade Federal do Ceará, CP 12 200, CEP 60455-970, Fortaleza, Brazil.
Nágila M S P
NMSP
Ricardo
School of Chemistry, University of Manchester, Manchester, M13 9PL, UK.
Ralph W
http://orcid.org/0000-0001-8009-5334
RW
Adams
School of Chemistry, University of Manchester, Manchester, M13 9PL, UK.
Gareth A
GA
Morris
School of Chemistry, University of Manchester, Manchester, M13 9PL, UK.
Mathias
M
Nilsson
1H; Brij; CTAB; DOSY; MAD; NMR; SDS; dihydroxybenzene isomers; matrix-assisted DOSY