SHARPER-DOSY: Sensitivity enhanced diffusion-ordered NMR spectroscopy

Abstract

Since its discovery in mid-20th century, the sensitivity of Nuclear Magnetic Resonance (NMR) has increased steadily, in part due to the design of new, sophisticated NMR experiments. Here we report on a liquid-state NMR methodology that significantly increases the sensitivity of diffusion coefficient measurements of pure compounds, allowing to estimate their sizes using a much reduced amount of material. In this method, the diffusion coefficients are being measured by analysing narrow and intense singlets, which are invariant to magnetic field inhomogeneities. The singlets are obtained through signal acquisition embedded in short (<0.5 ms) spin-echo intervals separated by non-selective 180° or 90° pulses, suppressing the chemical shift evolution of resonances and their splitting due to J couplings. The achieved 10−100 sensitivity enhancement results in a 100−10000-fold time saving. Using high field cryoprobe NMR spectrometers, this makes it possible to measure a diffusion coefficient of a medium-size organic molecule in a matter of minutes with as little as a few hundred nanograms of material.

Advancements in Characterization Techniques for Microemulsions: From Molecular Insights to Macroscopic Phenomena

“…This technology is widely used to determine the structure of microemulsions [ 48 ], study the effects of different components on microemulsions, and assist in constructing phase diagrams, as shown in Figure 5 [ 49 , 50 ]. Here, we explain diffusion nuclear magnetic resonance (dNMR) based on pulsed magnetic gradient techniques, especially pulsed field gradient NMR (PFG NMR) [ 51 ], pulsed-gradient spin-echo NMR (PGSE NMR) [ 52 ], and diffusion-ordered spectroscopy (DOSY) [ 53 , 54 ]. In cases where unexpected diffusion occurs in NMR samples, spatially encoded diffusion NMR (SPEN DNMR) techniques have also been developed [ 55 ].…”