Search Results (45)

Nuclear Magnetic Resonance (NMR) and Magnetic Resonance Imaging (MRI) are powerful techniques that have been employed to analyze foodstuffs comprehensively. These techniques offer in-depth information about the chemical composition, structure, and spatial distribution of components in a variety of food products. Quantitative NMR is widely applied for precise quantification of metabolites, authentication of food products, and monitoring of food quality. Low-field ¹H-NMR relaxometry is an important technique for investigating the most abundant components of intact foodstuffs based on relaxation times and amplitude of the NMR signals. In particular, information on water compartments, diffusion, and movement can be obtained by detecting proton signals because of H₂O in foodstuffs. Saffron adulterations with calendula, safflower, turmeric, sandalwood, and tartrazine have been analyzed using benchtop NMR, an alternative to the high-field NMR approach. The fraudulent addition of Robusta to Arabica coffee was investigated by ¹H-NMR Spectroscopy and the marker of Robusta coffee can be detected in the ¹H-NMR spectrum. MRI images can be a reliable tool for appreciating morphological differences in vegetables and fruits. In kiwifruit, the effects of water loss and the states of water were investigated using MRI. It provides informative images regarding the spin density distribution of water molecules and the relationship between water and cellular tissues. ¹H-NMR spectra of aqueous extract of kiwifruits affected by elephantiasis show a higher number of small oligosaccharides than healthy fruits do. One of the frauds that has been detected in the olive oil sector reflects the addition of hazelnut oils to olive oils. However, using the NMR methodology, it is possible to distinguish the two types of oils, since, in hazelnut oils, linolenic fatty chains and squalene are absent, which is also indicated by the ¹H-NMR spectrum. NMR has been applied to detect milk adulterations, such as bovine milk being spiked with known levels of whey, urea, synthetic urine, and synthetic milk. In particular, T2 relaxation time has been found to be significantly affected by adulteration as it increases with adulterant percentage. The ¹H spectrum of honey samples from two botanical species shows the presence of signals due to the specific markers of two botanical species. NMR generates large datasets due to the complexity of food matrices and, to deal with this, chemometrics (multivariate analysis) can be applied to monitor the changes in the constituents of foodstuffs, assess the self-life, and determine the effects of storage conditions. Multivariate analysis could help in managing and interpreting complex NMR data by reducing dimensionality and identifying patterns. NMR spectroscopy followed by multivariate analysis can be channelized for evaluating the nutritional profile of food products by quantifying vitamins, sugars, fatty acids, amino acids, and other nutrients. In this review, we summarize the importance of NMR spectroscopy in chemical profiling and quality assessment of food products employing magnetic resonance technologies and multivariate statistical analysis. Full article

Determining the technological quality of fresh meat pieces is essential in the meat industry to ensure the production of high-quality products. For this purpose, nuclear magnetic resonance (NMR) is a non-destructive and non-invasive technique that appears as an alternative to traditional methodologies. The objective of this work is to determine the potential of magnetic resonance imaging (MRI) and time-domain (TD-NMR) relaxometry for determining the physicochemical characterization of fresh hams with different industrial destinations (both fresh and cured products, such as dry-cured ham). For this study, the biceps femoris, semimembranosus, and semitendinosus muscles of 20 fresh hind legs from white pigs, classified into four categories according to their fat content, were analyzed. The semitendinosus muscle was selected as a model, and positive and negative correlations were obtained between different physicochemical parameters and the longitudinal (T1) and transverse (T2) relaxation times obtained by MRI and TD-NMR. Regression models using T1 and T2 were also developed to predict the muscle water-holding capacity (WHC) and drip loss, using high, medium, and low magnetic field NMR (R² > 0.80). Therefore, MRI and TD-NMR could be considered as highly suitable and accurate non-destructive techniques for the WHC determination in the meat industry. Full article

Concrete printing technologies play a key role in the modernization of construction practices. One factor that mitigates their progress is the development of standards and characterization tools for concrete during printing. The aim of this work is to point out correlations between some printability descriptors of mortars and the data obtained from low-field nuclear magnetic resonance (NMR) relaxometry techniques. In this context, the superposed effects of an acrylic-based superplasticizer and calcium nitrate accelerator were investigated. The mortars under study are based on white Portland cement, fine aggregates, and silica fume at fixed ratios. Extrusion tests and visual inspection of the filaments evaluate the extrudability and the printing window. The selected compositions were also investigated via transverse $\left(T_2\right)$ and longitudinal $\left(T_1\right)$ NMR relaxation times. The results indicate that both additives increase the printing window of the mortar, while the accelerator induces a faster increase in specific surface area of capillary pores $\left(S/V\right)$ only after 30–60 min of hydration. Some correlations were found between the printing window and the range where the transverse relaxation rates $\left(1/T_2\right)$ and the pore surface-to-volume ratios $\left(S/V\right)$ increase linearly. This suggests some promising connections between NMR techniques and the study of structural buildup of cementitious materials. Full article

Objectives: Hydrogels produced using the freeze–thaw method have demonstrated significant potential for wound management applications. However, their production requires precise control over critical factors including freezing temperature and the choice of matrix-forming excipients, for which no consensus on the optimal conditions currently exists. This study aimed to address this gap by evaluating the effects of the above-mentioned variables on cryogel performance. Methods: Mechanical properties, absorption capacity, and microstructure were assessed alongside advanced analyses using differential scanning calorimetry (DSC) and low-field nuclear magnetic resonance relaxometry (LF TD NMR). Results: The results demonstrated that fully hydrolyzed polyvinyl alcohol (PVA) with a molecular weight above 61,000 g/mol is essential for producing high-performance cryogels. Among the tested formulations, an 8% (w/w) PVA_56–98 solution (Mw~195,000; DH = 98.0–98.8%) with 10% (w/w) propylene glycol (PG) provided the best balance of stretchability, durability, and low adhesion. Notably, while −25 °C is often used for cryogel preparation, freezing the gel precursor at −80 °C yielded superior results, producing materials with more open, interconnected structures and enhanced mechanical strength and elasticity—deviating from conventional practices. Conclusions: The designed cryogel prototypes exhibited functional properties comparable to or even surpassing commercial wound dressings, except for absorption capacity, which remained lower. Despite this, the cryogel prototypes demonstrated potential as wound dressings, particularly for use in dry or minimally exuding wounds. All in all, this study provides a comprehensive analysis of the physicochemical and functional properties of PVA cryogels, establishing a strong foundation for the development of advanced wound dressing systems. Full article

Using liquid crystals in near-infrared applications suffers from effects related to processes like parasitic absorption and high sensitivity to UV-light exposure. One way of managing these disadvantages is to use deuterated systems. The combined ¹H and ²H nuclear magnetic resonance relaxometry method (FFC NMR), dielectric spectroscopy (DS), optical microscopy (POM), and differential scanning calorimetry (DSC) approach was applied to investigate the influence of selective deuteration on the molecular dynamics, thermal properties, self-organization, and electric-field responsiveness to a 4′-pentyl-4-biphenylcarbonitrile (5CB) liquid crystal. The NMR relaxation dispersion (NMRD) profiles were analyzed using theoretical models for the description of dynamics processes in different mesophases. Obtained optical textures of selectively deuterated 5CB showed the occurrence of the domain structure close to the I/N phase transition. The dielectric measurements showed a substantial difference in switching fields between fully protonated/deuterated 5CB and selectively deuterated molecules. The DSC thermograms showed a more complex phase transition sequence for partially deuterated 5CB with respect to fully protonated/deuterated molecules. Full article

Ferroelectric and antiferroelectric smectic liquid crystalline (LC) phases are still at the center of investigations and interests for both their fundamental properties and variety of technological applications. This review aims to report the main contributions based on different nuclear magnetic resonance (NMR) techniques to the study of chiral liquid crystalline calamitic mesogens forming smectic phases, such as the SmA, the SmC* (ferroelectric), and the SmC*_A (antiferroelectric) phases. ²H NMR and ¹³C NMR techniques and their combination were of help in clarifying the local orientational properties (i.e., the molecular and fragments’ main orientational order parameters) at the transition between the SmA and the SmC* phases, and in the particular case of de Vries liquid crystals, NMR studies gave important clues regarding the actual models describing the molecular arrangement in these two phases formed by de Vries LCs. Moreover, this review describes how the combination of ²H NMR relaxation times’ analysis, ¹H NMR relaxometry, and ¹H NMR diffusometry was successfully applied to the study of chiral smectogens forming the SmC* and SmC*_A phases, with the determination of relevant parameters describing both rotational molecular and internal motions, collective dynamics, and translational self-diffusion motions. Several cases will be reported concerning NMR investigations of chiral ferroelectric and antiferroelectric phases, underlining the great potential of combined NMR approaches to the study of supramolecular, conformational, and dynamic properties of liquid crystals. Full article

Asphalt binders in pavements lose their stability through aging and eventually fail in the field. Using nuclear magnetic resonance (NMR) to monitor the primary longitudinal relaxation time of asphalt samples and the ratio of material that carries this primary relaxation time has been shown to indicate the impact of ultraviolet (UV) radiation on the aging of asphalt pavements. Longitudinal NMR relaxation was used to investigate two types of proposed asphalt rejuvenators, a bio-oil-based rejuvenator and a crude-oil-based rejuvenator. Two different binders with the performance grades (PG) 64-22 and 76-22 were considered for their interactions with the rejuvenators. After 72 h of exposure to intense UV radiation, specifically designed NMR relaxometry experiments were applied to compare the rejuvenation capabilities of the two rejuvenator samples. The crude oil-based rejuvenator was found to exhibit relaxation times similar to the binder samples while the bio-based material showed relaxation times that pointed to different nuclear hydrogen environments. Both rejuvenators reduced the primary relaxation time of the PG 76-22 binder, which indicates that their stiffness was reduced. Both types of rejuvenators also seemed to prevent the effects of UV aging. Two mechanisms of rejuvenation were identified by NMR relaxometry. The primary relaxation time can be used to indicate a change in stiffness while the primary ratio of the material is tied to oxidative aging. Oxidative aging creates distinct hydrogen environments due to asphaltene aggregation. The bio-based rejuvenator only reduced the binder’s stiffness, while the crude oil-based rejuvenator also reduced the aggregation of asphaltenes. Consequently, the bio-based rejuvenator could be classified as an asphalt softener, while the oil-based material acted like a true rejuvenator. Full article

Advanced ¹H Nuclear Magnetic Resonance (NMR) relaxometry and diffusometry methods and VIS-nearIR spectroscopy combined with pH, electrical conductivity (EC) and totally dissolved solids (TDSSs) measurements were used to assess the properties of wastewater collected from a chicken slaughterhouse in each step of the treatment process (wastewater before treatment, biologically treated wastewater, chemically treated wastewater and discharged wastewater) and from sludge. The ¹H NMR Carr–Purcell–Meiboom–Gill (CPMG) and Pulsed-Gradient-Stimulated-Echo (PGSE) decay curves recorded for all samples of wastewater were analyzed by inverse Laplace transform (ILT) to obtain the distributions of transverse relaxation times T₂ and diffusion coefficient D. The VIS-nearIR total absorbance, T₂-values, D-values, pH, EC and TDSS parameters were used for statistical analysis in principal component (PCA). The ¹H T₂-distributions measured for the slaughterhouse wastewater lie in two main regions reflecting the number of dissolved solids or the distribution of undissolved solids. The PCA analysis successfully differentiates between polluted and less polluted wastewaters and sludge. The wastewater treatment applied by the slaughterhouse is efficient. The recommended methods for wastewater monitoring are the NMR T₂- and D-distributions and EC, TDSSs and NMR-D diffusion coefficient. Finally, Machine Learning algorithms are used to provide prediction maps of wastewater treatment stage. Full article

Fast-Field-Cycling (FFC) Nuclear Magnetic Resonance (NMR) relaxometry is a powerful, non-destructive magnetic resonance technique that enables, among other things, the investigation of slow molecular dynamics at low magnetic field intensities. FFC-NMR relaxometry measurements provide insight into molecular motion across various timescales within a single experiment. This study focuses on a model-free approach, representing the NMRD profile $R_1$ as a linear combination of Lorentzian functions, thereby addressing the challenges of fitting data within an ill-conditioned linear least-squares framework. Tackling this problem, we present a comprehensive review and experimental validation of three regularization approaches to implement the model-free approach to analyzing NMRD profiles. These include (1) MF-UPen, utilizing locally adapted $L_2$ regularization; (2) MF-L1, based on $L_1$ penalties; and (3) a hybrid approach combining locally adapted $L_2$ and global $L_1$ penalties. Each method’s regularization parameters are determined automatically according to the Balancing and Uniform Penalty principles. Our contributions include the implementation and experimental validation of the MF-UPen and MF-MUPen algorithms, and the development of a “dispersion analysis” technique to assess the existence range of the estimated parameters. The objective of this work is to delineate the variance in fit quality and correlation time distribution yielded by each algorithm, thus broadening the set of software tools for the analysis of sample structures in FFC-NMR studies. The findings underline the efficacy and applicability of these algorithms in the analysis of NMRD profiles from samples representing different potential scenarios. Full article

The demand for effective asphalt additives is growing as road infrastructure ages and more sustainable pavement solutions are needed. Tire pyrolysis oil (TPO) is an example material that has been gaining attention as a potential asphalt additive. While physical performance grade (PG) temperatures are the predominant performance requirements for asphalt binders, chemical properties are also significant in the evaluation of asphalt performance. There is a need to chemically characterize the aging of asphalt binders modified with TPO and link chemical changes in binder components to binder performance. This study compares 2%, 4%, and 8% TPO and asphalt binder blends via dynamic shear rheometry (DSR), Fourier-transform infrared (FTIR) spectroscopy, and nuclear magnetic resonance (NMR) relaxometry. The variability in the modified blends was seen by both physical and chemical testing during four different blending times (1, 60, 120, and 240 min). After blending, high and intermediate PGs were determined by physical testing. The 8% TPO blend reduced the high PG of the binder from 64 °C to 58 °C. This effect was confirmed by chemical testing through changes in carbonyl indices and NMR relaxation times. With more oil present in the binder matrix, the binder’s resistance to rutting was reduced. While the high PG was hindered, the intermediate PG remained unchanged for all TPO blends. This physical similarity was mirrored in chemical testing. The chemical and physical variability along with the hindrance of the high PG temperature indicate that more treatment may be needed before TPO can be effectively applied to asphalt binders. This study suggests a correlation between physical performance and key chemical indicators. Full article

Calcium phosphate cements are widely used biomaterials for bone regeneration due to their biological properties, such as biocompatibility, biodegradability, and bioactivity. The presence of chitosan in cement composition influences the resorption rate of the material and its mechanical properties. In the present work, the water absorption and solubility of a tricalcium phosphate bone cement, prepared with and without chitosan addition, was comparatively evaluated. The absorption and solubility properties were monitored for 21 days by immersing the samples in water at room temperature and then weighing them. A morphological analysis of the samples was carried out via scanning electron microscopy (SEM). The absorption dynamics and pore evolution were investigated with low-field nuclear magnetic resonance (NMR) relaxometry. It was demonstrated that the presence of chitosan accelerates the hardening dynamics, reduces water absorption, and influences the solubility and degradation behavior of the cement. It was also observed that, independent of the presence of chitosan, the polymerization process is not completed even after one hour, which influences the solubility process. It was also shown that the presence of chitosan reduces the amount of microcracks and improves the functional properties of the hardened cement. Full article

Incorporating blast furnace slag into the composition of paving concrete can be one of the cost-effective ways to completely eliminate by-products from the pig iron production process (approximately 70% granulated slag and 30% air-cooled slag). The possibility to reintroduce blast furnace slag back into the life cycle will provide significant support to current environmental concerns and the clearance of tailings landfills. Especially in recent years, granulated and ground blast furnace slag (GGBS) as a substitute for cement and air-cooled blast furnace slag (ACBFS) aggregates as a substitute for natural aggregates in the composition of concretes have been studied by many researchers. But concrete compositions with large amounts of incorporated blast furnace slag affect the mechanical and durability properties through the interaction between the slag, cement and water depending on the curing times. This study focuses on identifying the optimal proportions of GGBS as a supplementary cementitious material (SCM) and ACBFS aggregates as a substitute to natural sand such that the performance at 90 days of curing the concrete is similar to that of the control concrete. In addition, to minimize the costs associated with grinding GGBS, the hydration activity index (HAI) of the GGBS, the surface morphology, and the mineral components were analyzed via X-ray diffraction, scanning electron microscopy (SEM), energy dispersive spectrometry (EDX), and nuclear magnetic resonance relaxometry (NMR). The flexural strength, the basic mechanical property of road concretes, increased from 28 to 90 days by 20.72% and 20.26% for the slag concrete but by 18.58% for the reference concrete. The composite with 15% GGBS and 25% ACBFS achieved results similar to the reference concrete at 90 days; therefore, they are considered optimal percentages to replace cement and natural sand in ecological pavement concretes. The HAI of the slag powder with a specific surface area equivalent to that of Portland cement fell into strength class 80 at the age of 28 days, but at the age of 90 days, the strength class was 100. The results of this research present three important benefits: the first is the protection of the environment through the recycling of two steel industry wastes that complies with European circular economy regulations, and the second is linked to the consequent savings in the disposal costs associated with wastefully occupied warehouses and the savings in slag grinding. Full article

This work aims to show the advantages of using GGBS (Ground Granulated Blast Furnace Slag) and ACBFS aggregate (Air-Cooled Blast Furnace Slag) on the tensile strength and durability properties of infrastructure concrete at the reference age of 28 days. Three concrete mixes were prepared: the first one was a control sample; the second one had 15% GGBS (instead of Portland cement) and 25% ACBFS (instead of natural sand); and the third had 15% GGBS (instead of Portland cement) and 50% ACBFS (instead of natural sand). The studies on mortars focused on the ratio of compressive strength (CS) in correlation with the specific surface area (obtained by the Blain method). The microstructure of the prepared mortars was examined at the age of 28 days by X-ray diffraction, SEM electron microscopy with an energy-dispersive EDX spectrometer, and NMR nuclear magnetic resonance relaxometry. The results of the tests carried out afterwards on the concretes containing slag (15% GGBS and 25% or 50% ACBFS) showed values that met high-quality criteria for exfoliation (S₅₆ < 0.1 kg/m²), carbonation, and gelling G100 (with a loss of resistance to compression η < 25%). The slag concretes showed a degree of gelation of G100 (with a loss of compressive strength below 25%), low volume losses below 18,000 mm³/5000 mm² (corresponding to wear class 4, grade I), and moderate penetration of chlorine ions (according to the RCPT test). All of these allow the concrete with slag (GGBS/ACBFS) to be recommended as an ecological road concrete. Our study proved that a high-class road concrete of BcR 5.0 can be obtained, with tensile strengths of a minimum 5 MPa at 28 days (the higher road concrete class in Romania, according to national standards). Full article

Nuclear Magnetic Resonance (NMR) spin relaxation times have been an instrumental tool in deciphering the local environment of ionic species, the various interactions they engender and the effect of these interactions on their dynamics in conducting media. Of particular importance has been their application in studying the wide range of electrolytes for energy storage, on which this review is based. Here we highlight some of the research carried out on electrolytes in recent years using NMR relaxometry techniques. Specifically, we highlight studies on liquid electrolytes, such as ionic liquids and organic solvents; on semi-solid-state electrolytes, such as ionogels and polymer gels; and on solid electrolytes such as glasses, glass ceramics and polymers. Although this review focuses on a small selection of materials, we believe they demonstrate the breadth of application and the invaluable nature of NMR relaxometry. Full article

‘Tonda Gentile Romana’ and ‘Tonda di Giffoni’ (Corylus avellana L.) are two Italian hazelnut cultivars, recognized under the quality labels “Protected Designation of Origin” (PDO) and “Protected Geographical Indication” (PGI), respectively. Hazelnut seeds are characterized by a complex microstructure and the presence of different physical compartments. This peculiarity has been studied and evidenced by Time Domain (TD) Nuclear Magnetic Resonance (NMR) experiments. This technique allowed the assessment of the presence of different diffusion compartments, or domains, by evaluating the distribution of the spin–spin relaxation time (T₂).The aim of this research was to develop a method based on ¹H NMR relaxometry to study the mobility in fresh hazelnut seeds (‘Tonda di Giffoni’ and ‘Tonda Gentile Romana’), in order to determine differences in seed structure and matrix mobility between the two cultivars. TD-NMR measurements were performed from 8 to 55 °C in order to mimic post-harvest processing as well the microscopic textural properties of hazelnut. The Carr–Purcell–Meiboom–Gill (CPMG) experiments showed five components for ‘Tonda Gentile Romana’ and four components for ‘Tonda di Giffoni’ relaxation times. The two slowest components of relaxation (T_2,a about 30–40% of the NMR signal, and T_2,b about 50% of the NMR signal) were attributed to the protons of the lipid molecules organized in the organelles (oleosomes), both for the ‘Tonda Gentile Romana’ and for the ‘Tonda di Giffoni’ samples. The component of relaxation T_2,c was assigned to cytoplasmic water molecules, and showed a T₂ value dominated by diffusive exchange with a reduced value compared to that of pure water at the same temperature. This can be attributed to the water molecules affected by the relaxation effect of the cell walls. The experiments carried out as a function of temperature showed, for ‘Tonda Gentile Romana’, an unexpected trend between 30 and 45 °C, indicating a phase transition in its oil component. This study provides information that could be used to strengthen the specifications underlying the definitions of “Protected Designation of Origin” (PDO) and “Protected Geographical Indication” (PGI). Full article