Species Distribution in Bicontinuous Phase Systems for Enhanced Oil Recovery Probed by Single-Sided NMR.

Multiphase aqueous-organic systems where a bicontinuous phase is in equilibrium with an excess organic and aqueous phase find various applications in industry. These systems─also known as Winsor III─are complex not only for the different phases that develop therein but also because they are multicomponent systems. In this work, we explore for the first time the use of a benchtop low-field single-sided NMR to determine the species distribution in Winsor III systems.

NMR characterization of structure and moisture sorption dynamics of damaged starch granules.

Among the many biopolymers that constitute food products, starch is one of the most common. Starch granules are often damaged in the milling process, which affects the final product quality, mainly due to changes in water adsorption properties. In this work, the crystallinity degree of wheat starch samples as a function of the mechanical damage is determined by low field H NMR.

Comparison of experimental times in T-D and D-T correlation experiments in single-sided NMR.

Diffusion-relaxation correlation experiments in nuclear magnetic resonance are a powerful technique for the characterization of fluid dynamics in confined geometries or soft matter, in which relaxation may be either spin-spin (T) or spin-lattice (T). The general approach is to acquire a set of bidimensional data in which diffusion is codified by the evolution of the magnetization with either Hahn or stimulated echoes (STE) in the presence of a constant magnetic field gradient. While T is codified by a Carr-Purcell-Meiboom-Gil (CPMG) sequence, T is either encoded by saturation or inversion-recovery methods.

Magnetic Resonance Imaging in Situ Visualization of an Electrochemical Reaction under Forced Hydrodynamic Conditions.

Magnetic resonance imaging (MRI) has proven to be a powerful tool for the characterization and investigation of in situ chemical reactions. This is more relevant when dealing with complex systems, where the spatial distribution of the species, partition equilibrium, flow patterns, among other factors have a determining effect over mass transport and therefore over the reaction rate. The advantage of MRI is that it provides spatial information in a noninvasive way and does not require any molecular sensor or sample extraction.

Single-shot velocity mapping by rewinding of velocity encoding with Echo-Planar Imaging.

The ability of single-shot NMR imaging methods to follow the time evolution of a velocity distribution within an object is strongly limited by the phase errors accumulated as velocity maps are acquired. In the particular case of Carr-Purcell based sequences combined with Echo Planar Imaging acquisition, phase accumulates through subsequent images, hampering the possibility to acquire several velocity maps, which would be useful to determine transient behavior. In this work, we propose the use of a rewinding velocity encoding module applied after the acquisition of each image during the CPMG echo train.

Flow-Pattern Characterization of Biphasic Electrochemical Cells by Magnetic Resonance Imaging under Forced Hydrodynamic Conditions.

The fluid dynamics of a liquid|liquid system inside a four-electrode electrochemical cell were studied by velocimetry magnetic resonance imaging (MRI) and flow propagator measurements. To characterize this system fully, three different cell configurations operating at two rotational frequencies were analyzed. Quantitative information about the stability of the liquid|liquid interface and the dynamics of the organic phase were determined.

Environmental Topology and Water Availability Modulates the Catalytic Activity of β-Galactosidase Entrapped in a Nanosporous Silicate Matrix.

In the present work we studied the catalytic activity of E. coli β-Gal confined in a nanoporous silicate matrix (E) at different times after the beginning of the sol-gel polymerization process. Enzyme kinetic experiments with two substrates (ONPG and PNPG) that differed in the rate-limiting steps of the reaction mechanism for their β-Gal-catalyzed hydrolysis, measurements of transverse relaxation times (T) of water protons through H-NMR, and scanning electron microscopy analysis of the gel nanostructure, were performed.

Enhanced Surface Interaction of Water Confined in Hierarchical Porous Polymers Induced by Hydrogen Bonding.

Hierarchical porous polymer systems are increasingly applied to catalysis, bioengineering, or separation technology because of the versatility provided by the connection of mesopores with percolating macroporous structures. Nuclear magnetic resonance (NMR) is a suitable technique for the study of such systems as it can detect signals stemming from the confined liquid and translate this information into pore size, molecular mobility, and liquid-surface interactions. We focus on the properties of water confined in macroporous polymers of ethylene glycol dimethacrylate and 2-hydroxyethyl methacrylate [poly(EGDMA-co-HEMA)] with different amounts of cross-linkers, in which a substantial variation of hydroxyl groups is achieved.

Structure characterization of the non-crystalline complexes of copper salts with native cyclodextrins.

The characterization of non-crystalline complexes is particularly difficult when techniques like X-ray diffraction or NMR cannot be used. We propose a simple procedure to characterize the physicochemical properties of amorphous new coordination compounds between cyclodextrins (CD) and Cu(2+) salts, by means of the integration of the information provided by several techniques including elemental analysis, flame atomic absorption, TGA, UV-Vis diffuse reflectance, colorimetry, FT-IR and EPR. On the basis of these procedures, we suggest geometrical and structural approximations resulting in an octahedral or distorted octahedral geometry with diverse positions for the metallic centre.

Spatially Resolved Monitoring of Drying of Hierarchical Porous Organic Networks.

Evaporation kinetics of water confined in hierarchal polymeric porous media is studied by low field nuclear magnetic resonance (NMR). Systems synthesized with various degrees of cross-linker density render networks with similar pore sizes but different response when soaked with water. Polymeric networks with low percentage of cross-linker can undergo swelling, which affects the porosity as well as the drying kinetics.

Unusual temperature-induced swelling of ionizable poly(N-isopropylacrylamide)-based microgels: experimental and theoretical insights into its molecular origin.

In the traditional view of temperature-driven volume phase transitions in PNIPAM-based microgel solutions, a monotonic and sharp decrease in the particle size occurs upon heating the solution to above the volume phase transition temperature (VPTT). However, at sufficiently high microgel concentrations and under low salt conditions, our dynamic light scattering experiments reveal an unexpected non-monotonic evolution of the particle size when increasing the solution temperature. These findings show that poly(N-isopropylacrylamide-co-methacrylic acid) (P(NIPAM-co-MAA)) microgels swell upon heating the solution in the temperature range where NIPAM is water-soluble (i.

Evaporation kinetics in swollen porous polymeric networks.

NMR is a fast, nondestructive, and noninvasive technique that can provide information about the pore structure of macroporous polymer beads and the dynamics of liquids confined in them. In this work, we describe the study of the pore structure of the macroporous polymer of ethylene glycol dimethacrylate and 2-hydroxyethyl methacrylate [poly(EGDMA-co-HEMA)] in the dry but also in the swollen state by measuring relaxation times of liquids contained in the polymer network. The results show that the pore architecture differs from the dry to the soaked state.

Synthesis of amphiphilic dendrons and their interactions in aqueous solutions with cetyltrimethylammonium p-toluenesulfonate (CTAT).

In this work, we report synthesis and rheology of an interesting structured fluid based on the self-assembly of amphiphilic dendrons and wormlike micelles. Two amphiphilic dendrons were synthesized by the combination of aliphatic chains and polar dendritic heads. They showed different degrees of hydrophobicity and formed micelles in aqueous solution at critical micelle concentrations (CMC) of 25 and 125 ppm.

Chemical and physicochemical characteristics of humic acids extracted from compost, soil and amended soil.

In order to gain understanding about how "HA-like substances" from organic amendments may change some properties in the soil solution, the knowledge of chemical and physicochemical characteristics (charge development, acid-base behavior and heterogeneity) should be known. The aim of this research were (i) to study the elemental and functional composition, (ii) to determine charge behavior, acid-base properties (apparent dissociation constant and buffer capacity) and (iii) to evaluate heterogeneity of humic acids (HA) isolated from municipal solid waste compost (MWC) and from the corresponding MWC-amended soil, in comparison to those of the unamended soil HA using potentiometric titration and differential scanning potentiometry (DSP). Potentiometric titration and the first derivative of -Q versus pH (negative charge development versus pH) curves could be used to determine proton-affinity distribution and the chemical heterogeneity of the HA as well as the average pK(app) and buffer capacity in a wide range of pH.