Nuclear Magnetic Resonance Techniques Research Articles

Enhanced room-temperature Na+ ionic conductivity in Na4.92Y0.92Zr0.08Si4O12

Developing cost-effective and reliable solid-state sodium batteries with superior performance is crucial for stationary energy storage. A key component in facilitating their application is a solid-state electrolyte with high conductivity and stability. Herein, we employed aliovalent cation substitution to enhance ionic conductivity while preserving the crystal structure. Optimized substitution of Y3+ with Zr4+ in Na5YSi4O12 introduced Na+ ​ion vacancies, resulting in high bulk and total conductivities of up to 6.5 and 3.3 ​mS ​cm−1, respectively, at room temperature with the composition Na4.92Y0.92Zr0.08Si4O12 (NYZS). NYZS shows exceptional electrochemical stability (up to 10 ​V vs. Na+/Na), favorable interfacial compatibility with Na, and an excellent critical current density of 2.4 ​mA ​cm−2. The enhanced conductivity of Na+ ​ions in NYZS was elucidated using solid-state nuclear magnetic resonance techniques and theoretical simulations, revealing two migration routes facilitated by the synergistic effect of increased Na+ ​ion vacancies and improved chemical environment due to Zr4+ substitution. NYZS extends the list of suitable solid-state electrolytes and enables the facile synthesis of stable, low-cost Na+ ion silicate electrolytes.

Application of 15N-Edited 1H-13C Correlation NMR Spectroscopy─Toward Fragment-Based Metabolite Identification and Screening via HCN Constructs.

Many key building blocks of life contain nitrogen moieties. Despite the prevalence of nitrogen-containing metabolites in nature, 15N nuclei are seldom used in NMR-based metabolite assignment due to their low natural abundance and lack of comprehensive chemical shift databases. However, with advancements in isotope labeling strategies, 13C and 15N enriched metabolites are becoming more common in metabolomic studies. Simple multidimensional nuclear magnetic resonance (NMR) experiments that correlate 1H and 15N via single bond 1JNH or multiple bond 2-3JNH couplings using heteronuclear single quantum coherence (HSQC) or heteronuclear multiple bond coherence are well established and routinely applied for structure elucidation. However, a 1H-15N correlation spectrum of a metabolite mixture can be difficult to deconvolute, due to the lack of a 15N specific database. In order to bridge this gap, we present here a broadband 15N-edited 1H-13C HSQC NMR experiment that targets metabolites containing 15N moieties. Through this approach, nitrogen-containing metabolites, such as amino acids, nucleotide bases, and nucleosides, are identified based on their 13C, 1H, and 15N chemical shift information. This approach was tested and validated using a [15N, 13C] enriched Daphnia magna (water flea) metabolite extract, where the number of clearly resolved 15N-containing peaks increased from only 11 in a standard HSQC to 51 in the 15N-edited HSQC, and the number of obscured peaks decreased from 59 to just 7. The approach complements the current repertoire of NMR techniques for mixture deconvolution and holds considerable potential for targeted metabolite NMR in 15N, 13C enriched systems.

Quantitative Low-Field 19 F Nuclear Magnetic Resonance Analysis of Carbonyl Groups in Pyrolysis Oils.

Pyrolysis bio-oils, one of the products of lignocellulosic biomass pyrolysis, have the potential to be widely used as fuels. The chemical composition of bio-oils is very complicated as they contain hundreds, if not thousands, of different, mostly oxygen-containing, compounds with a wide distribution of physical properties, chemical structures, and concentrations. Detailed knowledge of bio-oil composition is crucial for optimizing both the pyrolysis processes and for any subsequent upgrading into a more viable fuel resource. Here we report the successful use of low-field, or benchtop, nuclear magnetic resonance (NMR) spectrometers in the analysis of pyrolysis oils. Pyrolysis oils from four different feedstocks were derivatized and analyzed using 19 F NMR techniques. The NMR results compare favorably with titrations for total carbonyl content. In addition, the benchtop NMR spectrometer proves able to reveal key spectral features, thus allowing the quantification of different carbonyl groups, such as aldehydes, ketones and quinones. Benchtop NMR spectrometers are typically compact, cheaper than their superconducting counterparts and do not require cryogens. Their use will make NMR analysis of pyrolysis oils easier and more accessible to a wide range of different potential users.

Overlooked Formation of Carbonate Radical Anions in the Oxidation of Iron(II) by Oxygen in the Presence of Bicarbonate

AbstractIron(II), (Fe(H2O)62+, (FeII) participates in many reactions of natural and biological importance. It is critically important to understand the rates and the mechanism of FeII oxidation by dissolved molecular oxygen, O2, under environmental conditions containing bicarbonate (HCO3−), which exists up to millimolar concentrations. In the absence and presence of HCO3−, the formation of reactive oxygen species (O2⋅−, H2O2, and HO⋅) in FeII oxidation by O2 has been suggested. In contrast, our study demonstrates for the first time the rapid generation of carbonate radical anions (CO3⋅−) in the oxidation of FeII by O2 in the presence of bicarbonate, HCO3−. The rate of the formation of CO3⋅− may be expressed as d[CO3⋅−]/dt=[FeII[[O2][HCO3−]2. The formation of reactive species was investigated using 1H nuclear magnetic resonance (1H NMR) and gas chromatographic techniques. The study presented herein provides new insights into the reaction mechanism of FeII oxidation by O2 in the presence of bicarbonate and highlights the importance of considering the formation of CO3⋅− in the geochemical cycling of iron and carbon.

Overlooked Formation of Carbonate Radical Anions in the Oxidation of Iron(II) by Oxygen in the Presence of Bicarbonate.

Iron(II), (Fe(H2 O)6 2+ , (FeII ) participates in many reactions of natural and biological importance. It is critically important to understand the rates and the mechanism of FeII oxidation by dissolved molecular oxygen, O2 , under environmental conditions containing bicarbonate (HCO3 - ), which exists up to millimolar concentrations. In the absence and presence of HCO3 - , the formation of reactive oxygen species (O2 ⋅- , H2 O2 , and HO⋅) in FeII oxidation by O2 has been suggested. In contrast, our study demonstrates for the first time the rapid generation of carbonate radical anions (CO3 ⋅- ) in the oxidation of FeII by O2 in the presence of bicarbonate, HCO3 - . The rate of the formation of CO3 ⋅- may be expressed as d[CO3 ⋅- ]/dt=[FeII [[O2 ][HCO3 - ]2 . The formation of reactive species was investigated using 1 H nuclear magnetic resonance (1 H NMR) and gas chromatographic techniques. The study presented herein provides new insights into the reaction mechanism of FeII oxidation by O2 in the presence of bicarbonate and highlights the importance of considering the formation of CO3 ⋅- in the geochemical cycling of iron and carbon.

1H and 13C NMR spectral assignments for low-concentration bile acids in biological samples

Bile acids are the main body of enterohepatic circulation in vivo. They have essential functions such as emulsifying fat, bacteriostasis and regulating multiple metabolic pathways as signal molecules. However, the assignments of NMR signals for some low-concentration bile acids are still needed. This study combined 1D nuclear magnetic resonance (NMR) and 2D NMR techniques including 1H–1H correlation spectroscopy (COSY), 1H–1H total correlation spectroscopy (TOCSY), 1H J-resolved spectroscopy (J-Res), 1H–13C heteronuclear single quantum coherence spectroscopy (HSQC), and 1H–13C heteronuclear multiple bond correlation spectroscopy (HMBC) to assign the 1H and 13C signals of six bile acids in aqueous solution at physiological pH (∼7.4) and nine bile acids in methanol. These data are of importance to the NMR-based studies on lipid digestion, absorption, and metabolism.

Afforestation Alters the Molecular Composition of Soil Organic Matter in the Central Loess Plateau of China

Many studies have been conducted on organic carbon changes under different land use patterns, but studies and data concerning changes in the molecular composition of soil organic matter (SOM) during land use conversion are scarce. In this work, we studied the chemical composition of SOM on two Robinia pseudoacacia L. plantations and their adjacent croplands in the Loess Plateau using biomarker and nuclear magnetic resonance (NMR) techniques. Experimental data on the molecular composition of SOM showed that the soil microbial biomass carbon content initially decreased and then returned to the original level gradually after afforestation, while the SOM content and stocks increased over time. At the initial stage of afforestation, the content of total solvent extracts did not change significantly but changed slowly over time in the plantations without artificial disturbance. With an increase in restoration time, the concentrations of both the microbial- and plant-derived solvent extracts increased. Moreover, the concentrations of plant-derived solvent extracts were consistently lower than those of microbial-derived solvent extracts. Afforestation also significantly increased the lignin-derived phenol content in the surface soil layer (0–10 cm). However, no obvious change was observed in the lignin-derived phenols of the two adjacent croplands. These results indicate that the accumulation of aboveground litter and underground roots has the strongest effects on the lignin-derived phenol content. In contrast to cropland, the two plantations exhibited a high degree of degradation of lignin-derived phenols in the surface soil, but this remained almost unchanged over time. Moreover, in contrast to 20 years after the establishment of the R. pseudoacacia plantation, the low alkyl/O-alkyl carbon ratio of the 8-year R. pseudoacacia plantation indicated that more easily degradable components accumulated during the initial stage of afforestation. Therefore, the proportion of the unstable carbon pool was relatively high and the SOM content may decline in the early stage of afforestation. These results provide evidence illustrating the detailed changes in the chemical composition of SOM during the ecological restoration process.

Dose response assessment of conventional Fricke: a relationship between UV-Visible and nuclear magnetic resonance techniques

Conventional Fricke is an aqueous ferrous sulfate solution that has been widely studied in the field of chemical dosimetry. The feasibility of its use has become attractive for high dose measurements that are of clinical interest in the field of radiotherapy and for industrial purposes, in the irradiation of blood bags and the sterilization of surgical material. The derivation of the absorbed dose of Fricke depends on the radiation-induced oxidation of iron (II) ions (Fe2+) present in the aqueous solution to iron (III) ions (Fe3+), which occurs after exposure to ionising radiation. In this paper, it is proposed to evaluate the dose response of the Fricke dosimeter using two different analytical techniques, ultraviolet-visible spectrophotometry (UV-Vis) and nuclear magnetic resonance spectroscopy (NMR). Twelve groups of samples were analysed in triplicate, irradiated with doses between 0 and 800 Gy, using a cobalt-60 source (60Co). The dose rate of Fricke dosimeters was evaluated against the practical values obtained. The different methods allowed an analytical correlation of the species of oxidised iron (Fe3+) using a linearity curve as a function of the applied radiation dose.

In Situ Copolymerization Studies of Lignin, Acrylamide, and Diallyldimethylammonium Chloride: Mechanism, Kinetics, and Rheology.

In this work, free-radical polymerization of kraft lignin, acrylamide (AM), and diallyldimethylammonium chloride (DADMAC) was studied in detail. In situ nuclear magnetic resonance (NMR), rheological analysis, and particle size techniques were conducted to understand the physicochemical characteristics of this copolymerization system. The copolymerization of lignin-AM and lignin-DADMAC had activation energies of 65.7 and 69.3 kJ/mol, respectively, and followed the first-order kinetic model, which was monitored by in situ H1 NMR results. The highest conversions of AM and DADMAC were 96 and 68%, respectively, in the copolymerization of lignin, AM, and DADMAC at the molar ratio of 5.5:2.4:1, pH 2 and 85 °C. The results illustrated that the participation of AM in the reaction was essential for polymerizing DADMAC to lignin due to less steric hindrance of AM than DADMAC facilitating its bridging performance. The monomer conversion ratio and dynamic rheology of the reaction system indicated that lignin acted as an inhibitor in the copolymerization reaction. The particle size analysis of the reaction mixtures reflected the alteration in the size of particles from coarse particles (>300 μm) to fine particles (<10 and 10-50 μm) and suspension to colloidal systems when the reaction progressed. The oscillation study of the reaction media confirmed the gradual increase in the viscosity of the reaction media, illustrating the crosslinking of lignin, AM, and DADMAC.

Evaluation of a novel N-(Hydroxymethyl) acrylamide polymer gel dosimeter formulation with organic glucose additive for radiotherapy

In this study, the first evaluation of organic sensitizer material on N-(Hydroxymethyl) acrylamide (NHMA) polymer gel dosimeter was presented. A novel tissue-equivalent polymer gel formula composed of NHMA containing different concentrations of organic glucose additive (GL-NHMA) was developed and evaluated for its potential use to measure 3D dose distributions to compare with treatment planning system. The new polymers of GL-NHMA were irradiated using a linear accelerator (LINAC) with a megavolt X-ray photon beam over a dose range of 2–20 Gy, energies of 6, 10, and 15 MV, and dose rates of 50, 200, and 500 cGy/min. The samples were evaluated using 0.5 T nuclear magnetic resonance (NMR) technique in terms of spin-spin relaxation rate (R2). Comparing with the conventional NHMA composition (i.e., 0 wt% GL concentration), the sensitivity of the GL-NHAM was improved by 53%, 68%, 89%, and 115% with 10, 15, 20, and 25 wt% GL, respectively, with an excellent linear dose response up to 8 Gy. There were no observable effects on the R2 dose response induced by varying the dose rate, photon energy, and irradiation temperature. The polymerization was stable after irradiation for a period of 10 days. Additionally, the R2 values decreased with increasing the scanning temperature. The dosimeter is water equivalent and is energy-independent from 0.1 to 20 MeV when considering the optimum composition. The gel dosimetry accuracy was evaluated in this study by calculating the overall uncertainty and found to be 4.64% (2σ, 95% confidence level). The GL additive acts as an excellent organic sensitizer in the GL-NHMA system, suggesting that this improved polymer formulation may be a useful tool for measuring dose distributions in radiotherapy at clinically relevant dose levels.

Exploring Metabolomic Patterns in Type 2 Diabetes Mellitus and Response to Glucose-Lowering Medications-Review.

The spectrum of information related to precision medicine in diabetes generally includes clinical data, genetics, and omics-based biomarkers that can guide personalized decisions on diabetes care. Given the remarkable progress in patient risk characterization, there is particular interest in using molecular biomarkers to guide diabetes management. Metabolomics is an emerging molecular approach that helps better understand the etiology and promises the identification of novel biomarkers for complex diseases. Both targeted or untargeted metabolites extracted from cells, biofluids, or tissues can be investigated by established high-throughput platforms, like nuclear magnetic resonance (NMR) and mass spectrometry (MS) techniques. Metabolomics is proposed as a valuable tool in precision diabetes medicine to discover biomarkers for diagnosis, prognosis, and management of the progress of diabetes through personalized phenotyping and individualized drug-response monitoring. This review offers an overview of metabolomics knowledge as potential biomarkers in type 2 diabetes mellitus (T2D) diagnosis and the response to glucose-lowering medications.

Engineering Properties of Novel Vertical Cutoff Wall Backfills Composed of Alkali-Activated Slag, Polymer-Amended Bentonite and Sand.

The workability, hydraulic conductivity, and mechanical properties are essential to contaminant containment performance of cementitious backfills in vertical cutoff walls at contaminated sites. This study aims to investigate the engineering properties of a novel vertical cutoff wall backfill composed of reactive magnesia (MgO)-activated ground granulated blast furnace slag (GGBS), sodium-activated calcium bentonite amended with polyacrylamide cellulose (PAC), and clean sand (referred to as MSBS-PAC). Backfills composed of MgO-activated GGBS, sodium-activated calcium bentonite, and clean sand (referred to as MSBS) were also tested for comparison purposes. A series of tests were conducted which included slump test, flexible-wall hydraulic conductivity test, and unconfined compression test. The pore size distributions of two types of backfills were investigated via the nuclear magnetic resonance (NMR) technique. The results showed the moisture content corresponding to the target slump height was higher for MSBS-PAC backfill than that for MSBS backfill. The MSBS-PAC backfill possessed lower pH, dry density, and higher void ratio at different standard curing times as compared to MSBS backfill. The unconfined compressive strength and strain at failure of the MSBS-PAC backfill were noticeable lower than those of the MSBS backfill. In contrast, the hydraulic conductivity of MSBS-PAC backfill was approximately one order of magnitude lower than that of the MSBS backfill, which was less than 10-9 m/s after 28-day and 90-day curing. Lower hydraulic conductivity of MSBS-PAC backfill was attributed to the improvement of pore structure and pore fluid environment by PAC amendment.

Tautomerism and Rotamerism of Favipiravir and Halogenated Analogues in Solution and in the Solid State.

Favipiravir is an important selective antiviral against RNA-based viruses, and currently, it is being repurposed as a potential drug for the treatment of COVID-19. This type of chemical system presents different carboxamide-rotameric and hydroxyl-tautomeric states, which could be essential for interpreting its selective antiviral activity. Herein, the tautomeric 3-hydroxypyrazine/3-pyrazinone pair of favipiravir and its 6-substituted analogues, 6-Cl, 6-Br, 6-I, and 6-H, were fully investigated in solution and in the solid state through ultraviolet-visible, 1H nuclear magnetic resonance, infrared spectroscopy, and X-ray diffraction techniques. Also, a study of the gas phase was performed using density functional theory calculations. In general, the keto-enol balance in these 3-hydroxy-2-pyrazinecarboxamides is finely modulated by external and internal electrical variations via changes in solvent polarity or by replacement of substituents at position 6. The enol tautomer was prevalent in an apolar environment, whereas an increase in the level of the keto tautomer was favored by an increase in solvent polarity and, even moreso, with a strong hydrogen-donor solvent. Keto tautomerization was favored either in solution or in the solid state with a decrease in 6-substituent electronegativity as follows: H ≫ I ≈ Br > Cl ≥ F. Specific rotameric states based on carboxamide, "cisoide" and "transoide", were identified for the enol and keto tautomer, respectively; their rotamerism is dependent on the tautomerism and not the aggregation state.

Multiscale Fine Characterization of a Coal Pore–Fracture System Based on SEM, CT, and NMR in the Jingbian Block, Ordos Basin

To achieve an accurate and comprehensive characterization of the multiscale pore–fracture characteristics of Permian coal in the Jingbian Block, Ordos Basin, a combination of scanning electron microscopy (SEM), X-ray computed tomography (CT), and nuclear magnetic resonance (NMR) techniques was utilized. With these experiments, the mineral composition, pore size distribution (PSD), porosity, and connectivity of pores in coal samples were characterized through qualitative and quantitative methods. The results show that the SEM experiments enabled qualitative identification of pores and mineral types. The coal samples primarily contained gas pores, cell pores, intercrystalline pores, and moldic pores, and clay minerals were the predominant fracture fillings. The 3D reconstruction of the CT experiments shows that the pores and fractures generally expand horizontally, while the minerals show obvious bedding expansion characteristics. Moreover, the estimation of full-size porosity in coal samples can be achieved by combining CT and NMR experiments. The full-size porosity of samples G11-5-1, G11-5-6, G11-5-9, and G11-5-11 was 8.93%, 9.11%, 10.45%, and 11.63%, respectively. The connectivity differences are primarily determined by the throat development degree and the connected pore–fracture count. Samples with more connected pores and larger throat radii exhibit excellent connectivity.

Experimental investigation of hydrocarbon-ion interaction in water-oil emulsions: A new insight into asphaltene structure and chemistry

Emulsification has been proved as one of the mechanisms contributing to improving oil recovery. Regarding the amphiphilic nature of the asphaltene and other polar hydrocarbons, their role should be understood. This research aims to investigate the chemistry and structure of the asphaltene molecules in the emulsions generated by the oil and ion-tuned water. The static bottle tests, containing the aqueous, emulsion, and bulk oil phases, were generated to study the emulsification. To have a mechanistic insight into the participation of asphaltene molecules in the emulsion phase, two oil samples of crude oil and asphaltene-rich toluene were used to generate the emulsions. After extracting the asphaltene from the bulk phases, the analytical techniques of Nuclear Magnetic Resonance (NMR), Fourier transform infrared (FTIR), and Energy-dispersive X-ray (EDX) were employed to study the asphaltene structural parameters, functional groups, and elemental content, respectively. Based on the NMR technique, the asphaltenes with smaller aromatic cores and shorter aliphatic chains, which contain polar functional groups have more tendency to adsorb onto the emulsion phase. It was shown that the magnesium and calcium ions have stronger electrostatic interactions with the asphaltene, leading to more attraction of the asphaltenes in the emulsion phase. In contrast, the sulfate ions showed a weaker attraction force to adsorb the asphaltenes in the emulsion phase. Based on the EDX spectroscopy, the heteroatom (oxygen, nitrogen, and sulfur) contents of the crude asphaltene is more than the bulk one, representing more affinity of the polar asphaltenes toward the emulsion phase. According to the FTIR spectroscopy of the bulk oil, while the aromatic hydrocarbons have a lower affinity toward the emulsion phase, the longer alkanes have more affinity to adsorb onto the emulsion phase. It should be mentioned that the chemistry and structural parameters of the bulk asphaltenes in the emulsions, which were generated by crude oil and asphaltene-rich toluene, were different. This observation indicated that the chemistry of the asphaltenes participating in the emulsion phase is influenced by the presence of other amphiphilic hydrocarbons. In this study, it was shown that chemical functional groups and structural parameters of asphaltene affect the emulsification process. Hence, studying the chemistry of asphaltene and other polar hydrocarbons is a vital step for the formulation of optimum ion-tuned water.

Experimental Study on the Grouting Diffusion Process in Fractured Sandstone with Flowing Water Based on the Low-Field Nuclear Magnetic Resonance Technique

Experimental Study on the Grouting Diffusion Process in Fractured Sandstone with Flowing Water Based on the Low-Field Nuclear Magnetic Resonance Technique

Preparation of 2-Nitrocacalol Acetate From a Sesquiterpene Isolated From Roots of Psacalium decompositum. Evaluation of α-Glucosidase and Acetylcholinesterase Inhibition

Objective To introduce a nitrogen atom into the structure of the cacalol acetate and to evaluate the change in its ability to inhibit enzymes of therapeutic importance such as α-glucosidase and acetylcholinesterase (AChE), which are targeted in the development of drugs for the treatment of diabetes and Alzheimer’s disease (AD), respectively. Methods Cacalol acetate was obtained by subjecting the hexane and ethyl acetate extracts from the roots of Psacalium decompositum to acetylation conditions. Subsequently, the cacalol acetate was brought under nitration conditions using cerium (IV) ammonium nitrate and acetic anhydride to obtain 2-nitrocacalol acetate; this compound was characterized by nuclear magnetic resonance, mass spectrometry, and X-ray diffraction techniques. Additionally, the inhibitory activity of the ethyl acetate extract, the cacalol acetate, and the 2-nitrocacalol acetate was evaluated on the enzymes α-glucosidase and AChE. Finally, the possible mode of ligand–enzyme binding through molecular docking was established. Results The 2-nitrocacalol acetate was obtained with a 20% yield. Its crystallographic structure was obtained, to our knowledge, for the first time, corroborating the S configuration in C5, showing a mostly planar molecule, in which the C6, C7, and C14 atoms and the acetyl group leaving the plane. The ethyl acetate extract was that which significantly inhibited the α-glucosidase (95.8% at 100 μg/mL), while the 2-nitrocacalol acetate exhibited the highest inhibitory activity of the AChE (69.9% at 10 µg/mL). The 2-nitrocacalol acetate presented a favorable interaction energy with the AChE (−8.68 kcal/mol), highlighting the formation of two hydrogen bonds and hydrophobic interactions. Conclusions The 2-nitrocacalol acetate and its crystallographic structure were obtained, to our knowledge, for the first time providing a new modification to this sesquiterpene by introducing a nitro group, which was favored its ability to inhibit AChE. These structural modifications encourage future research in these sesquiterpenes as targets for the development of novel drugs that would be useful in clinical practice.

Characterization and bioactivities of exopolysaccharide produced from Azotobacter salinestris EPS-AZ-6

This study involved the extraction of an exopolysaccharide (EPS) from Azotobacter salinestris AZ-6, which was isolated from soil cultivated with leguminous plants. In a medium devoid of nitrogen, the AZ-6 strain displayed a maximum EPS yield of 1.1 g/l and the highest relative viscosity value of 3.4. The homogeneity of the polymer was demonstrated by the average molecular weight of 1.61 × 106 Da and a retention time of 17.211 min for levan. The presence of characteristic functional groups and structural units of carbohydrate polymers has been confirmed through spectroscopic analyses utilizing Fourier-transform infrared (FT-IR) and nuclear magnetic resonance (NMR) techniques. Thermogravimetric analysis (TGA) revealed a noteworthy decrease in weight (74 %) in the temperature range spanning from 260 to 350 °C. X-ray diffraction (XRD) was utilized to verify the crystalline and amorphous characteristics of EPS-AZ-6. The EPS-AZ-6 exhibited significant cytotoxicity against the MCF-7 tumor cell line, as evidenced by an IC50 value of 6.39 ± 0.05 μg/ml. It also demonstrated a moderate degree of cytotoxicity towards HepG-2 cell line, as indicated by an IC50 value of 29.79 ± 0.41 μg/ml. EPS-AZ-6 exhibited potent antioxidant and in vitro antibacterial properties. These characteristics suggest the potential application value of EPS-AZ-6 in the food industry and pharmaceutical applications.

Dynamic and static imbibition characteristics of tight sandstone based on NMR

The study of the imbibition characteristics is significant as the main means of tight sandstone reservoir development. Static imbibition and dynamic imbibition displacement experiments were carried out with the cores of the Yanchang formation in the Ordos Basin. We studied the effects of the permeability on the imbibition recovery and analyzed the forces of the static imbibition and dynamic imbibition displacement. Finally, combined with the nuclear magnetic resonance technique, the fluid distributions in the core pores and the changes in the fluid signals in the processes of dynamic and static imbibition were analyzed, and the effects of pores of different scales on the static imbibition and displacement recovery were explored. The results showed that the static imbibition and dynamic imbibition displacement recovery increased with the increase in the permeability. Finally, using nuclear magnetic resonance analysis, it was found that dynamic imbibition displacement is an imbibition process driven mainly by the displacement pressure, and its recovery, about 24.20%, is mainly determined by macropores. Static imbibition is an imbibition process driven mainly by capillary forces. The recovery, about 31.15%, is also determined by macropores, but the effects of mesopores and micropores cannot be ignored. In addition, through the comparative analysis of different pores, it was found that the effects of the displacement pressure and capillary forces in different pores were different. Therefore, the displacement pressure of dynamic imbibition and the capillary forces of static imbibition should be reasonably used to improve the recovery degree of tight reservoirs.

Structural analysis of non-stoichiometric lithium cuprates, Li2+2xCu1-2xO2-x. Effects of lithium content and thermal treatments

Lithium cuprate (Li2CuO2) is being used for a wide range of applications due to its high lithium diffusion through the layer structure. Moreover, Li2+2xCu1-xO2-x non-stoichiometric material shows enhanced physicochemical properties. Therefore, lithium location understanding is highly important for lithium cuprate applications. This paper reports the structural coherence analysis, local and long atomic arrangement of Li2+2xCu1-xO2-x using X-ray diffraction (XRD), pair distribution function (PDF) and solid-state nuclear magnetic resonance (NMR) techniques. Li2CuO2, containing different excess quantities of lithium (from 0 to 60 at%), were synthesized by solid-state reaction. The synthesized ceramics presented nonstoichiometric structures, with Li2CuO2 type-structure. Two structural models were proposed to explain the high enhancement physicochemical properties of these ceramics; (i) the extra lithium atoms substitute copper sites, and (ii) lithium species occupy interstitial sites in the crystalline structure. Additionally, further thermal treatments rearrange the non-stoichiometric crystalline structures into the stable Li2CuO2 phase.