It is critical to probe in situ the dynamics and wettability of oil, water, and gas trapped in the complex microstructure of oil-shale rocks. However, usual techniques cannot separate these fluids in shale rocks. Here, we use multifrequency and multidimensional nuclear magnetic relaxation (NMR) techniques for probing these dynamics. The frequency dispersion behaviors of the longitudinal relaxation rates 1/T 1 for oil and water confined in shales are interpreted through a relaxation model showing one-dimensional (oil) and two-dimensional (2D) (water) diffusing phases confined within the organic kerogen and mineral layers, respectively. We probe the average hopping and residence times of these fluids at pore surfaces and assign signals to water and oil at both organic and mineral pore surfaces for characterizing their local wettability. This allows interpreting our 2D T 1 −T 2 correlation spectra that could be made down-hole, thus giving an invaluable tool for investigating oil and gas recovery on these important porous rocks.

A poplar biochar obtained by an industrial gasification process was saturated with water and analyzed using fast field cycling (FFC) NMR relaxometry in a temperature range between 299 and 353 K. Results revealed that the longitudinal relaxation rate increased with the increment of the temperature. This behavior was consistent with that already observed for paramagnetic inorganic porous media for which two different relaxation mechanisms can be accounted for: outer-and inner-sphere mechanisms. The former is due to water diffusing from the closest approach distance to infinity, whereas the second is due to water interacting by nonconventional H-bonds to the porous surface of the solid material. In particular, the inner-sphere relaxation appeared to be predominant in the water-saturated biochar used in the present study. This study represents a fundamental first step for the full comprehension of the role played by biochar in the draining properties of biochar-amended soils.

The field cycling NMR relaxometry method (also known as fast field cycling (FFC) when instruments employing fast electrical switching of the magnetic field are used) allows determination of the spin-lattice relaxation time (T1 ) continuously over five decades of Larmor frequency. The method can be exploited to observe the T1 frequency dependence of protons, as well as any other NMR-sensitive nuclei, such as (2) H, (13) C, (31) P, and (19) F in a wide range of substances and materials. The information obtained is directly correlated with the physical/chemical properties of the compound and can be represented as a 'nuclear magnetic resonance dispersion' curve. We present some recent academic and industrial applications showing the relevance of exploiting FFC NMR relaxometry in complex materials to study the molecular dynamics or, simply, for fingerprinting or quality control purposes. The basic nuclear magnetic resonance dispersion features are outlined in representative examples of magnetic resonance imaging (MRI) contrast agents, porous media, proteins, and food stuffs. We will focus on the new directions and perspectives for the FFC technique. For instance, the introduction of the latest Wide Bore FFC NMR relaxometers allows probing, for the first time, of the dynamics of confined surface water contained in the macro-pores of carbonate rock cores. We also evidence the use of the latest field cycling technology with a new cryogen-free variable-field electromagnet, which enhances the range of available frequencies in the 2D T1 -T2 correlation spectrum for separating oil and water in crude oil. Copyright © 2015 John Wiley & Sons, Ltd.

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An NMR analytical protocol based on complementary high and low field measurements is proposed for blueberry characterization. Untargeted NMR metabolite profiling of blueberries aqueous and organic extracts as well as targeted NMR analysis focused on anthocyanins and other phenols are reported. Bligh-Dyer and microwave-assisted extractions were carried out and compared showing a better recovery of lipidic fraction in the case of microwave procedure. Water-soluble metabolites belonging to different classes such as sugars, amino acids, organic acids, and phenolic compounds, as well as metabolites soluble in organic solvent such as triglycerides, sterols, and fatty acids, were identified. Five anthocyanins (malvidin-3-glucoside, malvidin-3-galactoside, delphinidin-3-glucoside, delphinidin-3-galactoside, and petunidin-3-glucoside) and 3-O-α-l-rhamnopyranosyl quercetin were identified in solid phase extract. The water status of fresh and withered blueberries was monitored by portable NMR and fast-field cycling NMR. (1) H depth profiles, T2 transverse relaxation times and dispersion profiles were found to be sensitive to the withering.