Single-sided Nuclear Magnetic Resonance Research Articles

Optimization of RF coil geometry for NMR/MRI applications using a genetic algorithm

A simulation method that employs a genetic algorithm (GA) for optimizing radio frequency (RF) coil geometry is developed to maximize signal intensity in nuclear magnetic resonance (NMR)/magnetic resonance imaging (MRI) applications. NMR/MRI has a wide range of applications, including medical imaging, and chemical and biological analysis to investigate the structure, dynamics, and interactions of molecules. However, NMR suffers from inherently low signal intensity, which depends on factors related to RF coil geometry. The investigation of coil geometry is crucial for improving signal intensity, leading to a reduction in the number of scans and a shorter total scan time. We have explored a better optimization method by modifying RF coil geometry to maximize signal intensity. The RF coil geometry comprises wire elements, each of which is a small vector representing the current flow, and GA chooses some of the prepared wire elements for optimization. The optimization of a substrate coil with a surface perpendicular to a static field was demonstrated for single-sided NMR system applications while considering various cylindrical sample diameters. A non-optimized and a GA-optimized substrate coil were compared through simulation and experiment to confirm the performance of the GA simulation. The maximum error between simulation and experiment was below 5%, with an average of less than 3%, confirming simulation reliability. The results indicated that the GA improved signal intensity by approximately 10% and reduced the necessary total scan time by around 20%. Finally, we explain the limitations and explore other potential applications of this GA-based simulation method.

Nondestructive measurement of the capillary water absorption coefficient and water transport behaviors of porous building materials by using single-sided NMR

Capillarity has an important effect on the durability of buildings, and the capillary absorption coefficient is a key parameter to describe the strength of material capillarity. Most of the methods currently used to measure the capillary absorption coefficient of materials can damage the sample or are not accurate enough and need to be improved. This paper proposes a method to measure the capillary absorption coefficient of brick, sandstone, mortar and concrete by using a single-sided nuclear magnetic resonance (NMR) technique, which has the advantages of accuracy, nondestructiveness, continuity and rapidity. The relative error of the capillary absorption coefficient obtained from three repetitions of the experiment ranges from 0 to 5.11%, which is in the range of 0.64%∼1.30% compared with that obtained by the partial impregnation method. This method has great potential for application in in situ testing. This paper also analyzed the water transport behaviors in porous building materials based on the variation in NMR signal intensity in the measured materials and established a water transport model. The model is divided into two stages: the first stage is mainly the one-dimensional rise in moisture in the vertical direction. The second stage is mainly the diffusion of moisture in the horizontal direction, which continuously fills each pore space to saturation. Difficulty in removing air leads to a reduced rate of water absorption in the second stage.

Single-Sided Nuclear Magnetic Resonance (NMR) for the Analysis of Skin Thickness and Collagen Structure in Scarred and Healthy Skin

Monitoring of skin scar thickness and structural properties is desirable when assessing the efficacy of the healing process. In this work, we report the use of single-sided, low-field nuclear magnetic resonance (NMR) for the analysis of the thickness and collagen structure of healthy and scarred skin. Acquisition of T2 relaxation profiles was proven to provide quantification of porcine skin thickness as accurate as standard histological techniques. Subsequent analysis of human participants highlighted the utility of this technique for identifying different types of scar and in identifying differences between the thickness of moderate hypertrophic scars and healthy skin. Using bead packings as a model system, determination of the surface-to-volume (S/V) ratio and tortuosity (k) was successfully measured on the single-sided apparatus based on time-resolved diffusion analysis. Application of this method to human skin was able to detect regional differences in collagen structures, consistent with qualitative expectations. It was also able to differentiate between healthy and scarred skin tissue. Preliminary results indicated that scarred tissue exhibited decreased S/V ratios and tortuosities, which is coherent with the formation of less-aligned collagen within scar tissue and indicated the potential for this technique to differentiate scar types. This novel application of single-sided low-field NMR has the potential to be deployed in clinical settings for the differentiation of scar types and for the assessment and monitoring of skin scarring and healing.

Nondestructive Measurement of the Water Content in Building Materials by Single-Sided NMR-MOUSE

Water has a significant impact on the properties of building materials. A nuclear magnetic resonance (NMR) spectrometer can be used to detect water in materials and measure its distribution nondestructively, rapidly, and accurately. In this paper, a novel method is introduced for using single-sided NMR to measure the water content (WC) of building materials, including brick, sandstone, mortar, and concrete. The NMR signal intensity and water content of these building materials were measured using a single-sided NMR-MOUSE PM25 and a high-precision electronic scale, respectively. A total of 80 groups of NMR signal intensity and water content data were obtained in two different measurement environments. The NMR signal intensity and water content data for each of the four building materials were fitted by the least squares method. The similarity of the coefficients of the determined correlations demonstrated that these relations are universal for building materials and independent of the NMR signal intensity and water content measurement environments.

Real-time in-situ measurement of hydrogel swelling by single sided NMR

Swelling factor and swelling rate are key characteristics of hydrogels. Here, a new method is presented for accurate in-situ monitoring of hydrogel swelling in real-time using single-sided nuclear magnetic resonance (NMR) profiling. The method reduces experimenter bias and uncertainty intrinsic to common weighing and caliper methods. Moreover, NMR allows monitoring of samples that may otherwise be inaccessible to other methods, for instance in opaque or sealed containers. The method is straightforward and does not require deep knowledge of NMR principles from the experimenter. This NMR profiling method estimates similar swelling factors to those using the weigh and caliper method, with precision equivalent to the weigh method and significantly better than with caliper. Unlike weigh and caliper methods, NMR profiling additionally provides dynamic swelling rates over time, without needing to touch or modify the sample.

Low-field, high-gradient NMR shows diffusion contrast consistent with localization or motional averaging of water near surfaces

Nuclear magnetic resonance (NMR) measurements of water diffusion have been extensively used to probe microstructure in porous materials, such as biological tissue, however primarily using pulsed gradient spin echo (PGSE) methods. Low-field single-sided NMR systems have built-in static gradients (SG) much stronger than typical PGSE maximum gradient strengths, which allows for the signal attenuation at extremely high b-values to be explored. Here, we perform SG spin echo (SGSE) and SG stimulated echo (SGSTE) diffusion measurements on biological cells, tissues, and gels. Measurements on fixed and live neonatal mouse spinal cord, lobster ventral nerve cord, and starved yeast cells all show multiexponential signal attenuation on a scale of b with significant signal fractions observed at b × D0 ≫ 1 with b as high as 400 ms/μm2. These persistent signal fractions trend with surface-to-volume ratios for these systems, as expected from porous media theory. An exception found for the case of fixed vs. live spinal cords was attributed to faster exchange or permeability in live spinal cords than in fixed spinal cords on the millisecond timescale. Data suggests the existence of multiple exchange processes in neural tissue, which may be relevant to the modeling of time-dependent diffusion in gray matter. The observed multi-exponential attenuation is from protons on water and not macromolecules because it remains proportional to the normalized signal when a specimen is washed with D2O. The signal that persists to b × D0 ≫ 1 is also drastically reduced after delipidation, indicating that it originates from lipid membranes that restrict water diffusion. The multi-exponential or stretched exponential character of the signal attenuation at b × D0 ≫ 1 appears mono-exponential when viewed on a scale of (b×D0)1/3, suggesting it may originate from localization or motional averaging of water near membranes on sub-micron length scales. To try to disambiguate these two contributions, signal attenuation curves were compared at varying temperatures. While the curves align when normalizing them using the localization length scale, they separate on a motional averaging length scale. This supports localization as the source of non-Gaussian displacements, but this interpretation is still provisional due to the possible confounds of heterogeneity, exchange, and relaxation. Measurements on two types of gel phantoms designed to mimic extracellular matrix, one with charged functional groups synthesized from polyacrylic acid (PAC) and another with uncharged functional groups synthesized from polyacrylamide (PAM), both exhibit signal at b × D0 ≫ 1, potentially due to water interacting with macromolecules. These preliminary finding motivate future research into contrast and attenuation mechanisms in tissue with low-field, high-gradient NMR.

Inline NMR via a Dedicated V-Shaped Sensor.

Process monitoring and control require dedicated and reliable measures which reflect the status of the process under investigation. Although nuclear magnetic resonance is known to be a versatile analytical technique, it is only seldomly found in process monitoring. Single-sided nuclear magnetic resonance is one well known approach for being applied in process monitoring. The dedicated V-sensor is a recent approach that allows the inline investigation of materials in a pipe non-destructively and non-invasively. An open geometry of the radiofrequency unit is realized using a tailored coil, enabling the sensor to be applied for manifold mobile applications in in-line process monitoring. Stationary liquids were measured, and their properties were integrally quantified as the basis for successful process monitoring. The sensor, in its inline version, is presented along with its characteristics. An exemplary field of application is battery production in terms of anode slurries; thus, the first results on graphite slurries will demonstrate the added value of the sensor in process monitoring.

Monitoring cheese ripening by single-sided nuclear magnetic resonance

The noninvasive, longitudinal study of products and food processing is of interest for the dairy industry. Here, we demonstrated that single-sided nuclear magnetic resonance (NMR) can be used for noninvasive monitoring of the cheese ripening process. The maturation of soft-ripened Camembert-like molded cheese samples was monitored for 20 d measuring 1-dimensional and 2-dimensional NMR relaxation and diffusion data at various depths, ranging from the hard surface layer to the soft center. Gelation and gel shrinkage were observed throughout ripening, and a complete loss of free water signal was observed at the cheese rind. Transversal (T2) relaxation distributions include 3 components that evolve with ripening time and position, corresponding to water inside the casein gel network, water trapped in casein, and fat. Two-dimensional T1-T2 relaxation experiments provided enhanced resolution of the 3 components, allowing quantification of the relative proportions of each phase. Furthermore, diffusion (D)-T2 relaxation correlation experiments revealed the bimodal size distribution of fat globules. The study demonstrated that single-sided NMR can provide spatially resolved signal intensity, relaxation, and diffusion parameters that reflect structural changes during the ripening process and can be exploited to understand and monitor the ripening of cheeses.

Effect of shape on depth profile Nuclear Magnetic Resonance data of multilayered composite structure

ABSTRACT Polymer matrix composite structures with adhesively bonded rubber layers are being used for various industrial applications. The adhesive layer thickness (used for bonding composite and elastomer rubber layers) has to be uniform to achieve desired bond strength. However, this cannot be controlled in practical applications in industry as no physical measurements are possible for large structures. This paper reports application of single-sided portable Nuclear Magnetic Resonance (NMR) at a frequency of 12.88 MHz for the study of the adhesive layer thickness measurement as well as qualitative analysis of the adhesive layer used for bonding these materials. The effect of the shape of the sample on the proton NMR signal which is related indirectly to elastic properties was investigated. Results obtained on flat and curved glass fibre reinforced polymer (GFRP) composite samples were compared. Studies showed there is a change in single-sided NMR depth profile data (slope of amplitude versus depth curve) due to changes in the shape of the composite structure. A multilayer sample with rubber and propellant bonded adhesively to the composite structure was also tested to study the effect of shape on the profile NMR data.

Evaluation of single-sided nuclear magnetic resonance technology for usage in geosciences

Because of its mobility and ability to investigate exposed surfaces, single-sided (SiS) nuclear magnetic resonance (NMR) technology enables new application fields in geosciences. To test and assess its corresponding potential, we compare longitudinal (T 1) and transverse (T 2) data measured by SiS NMR with those of conventional geoscientific laboratory NMR. We use reference sandstone samples covering a broad range of pore sizes. Our study demonstrates that the lower signal-to-noise ratio of SiS NMR data generally tends to slightly overestimated widths of relaxation time distributions and consequently pore size distributions. While SiS and conventional NMR produce very similar T 1 relaxation data, unbiased SiS NMR results for T 2 measurements can only be expected for fine material, i.e. clayey or silty sediments and soils with main relaxation times below . This limit is given by the diffusion relaxation rate due to the gradient in the primary magnetic field associated with the SiS NMR. Above that limit, i.e. for coarse material, the relaxation data is strongly attenuated. If considering the diffusion relaxation time of 0.2 s in the numerical data inversion process, the information content is blurred over a range larger than that of conventional NMR. However, our results show that principle range and magnitudes of the relaxation time distributions are reconstructed to some extent. Regarding these findings, SiS NMR can be helpful to solve geoscientific issues, e.g. to assess the hydro-mechanical properties of the walls of underground facilities or to provide local soil moisture data sets for calibrating indirect remote techniques on the regional scale. The greatest opportunity provided by the SiS NMR technology is the acquisition of profile relaxation data for rocks with significant bedding structures at the μm scale. With this unique feature, SiS NMR can support the understanding and modeling of hydraulic and diffusional anisotropy behavior of sedimentary rocks.

Detection of Planar Defects in Multilayered GFRP Composite Structures Using Low-Field Nuclear Magnetic Resonance

Adhesively bonded interfaces of glass fiber– reinforced plastics (GFRP) composite to rubber and rubber to propellant were investigated for planar interfacial defects with a spatial resolution of 100 μm. Single-sided low-field nuclear magnetic resonance (NMR) with a magnetic field strength of 0.3 T (12.88 MHz proton frequency) has been used for noninvasive inspection of planar defects in GFRP-based multilayered composite structures. Further, in this paper, the application of low-field NMR for adhesive liner thickness measurement is also demonstrated. The investigation revealed applicability of single-sided low-field NMR for onsite field applications. Results were compared with other nondestructive evaluation (NDE) techniques: acousto-ultrasonic and radiographic testing (RT). It is observed that single-sided low-field NMR is an excellent NDE tool to study adhesive bonds and defects such as debonding, variations in thickness to accuracies ranging from 50 to 200 μm, and degradation. In comparison with the acousto-ultrasonic technique and RT, single-sided low-field NMR is observed to be more sensitive.

A single-sided magnet for deep-depth fat quantification

Early detection of fatty-liver disease is important before further aggravations of the disease, such as cirrhosis, can develop. In this study, we developed a low-cost, movable single-sided magnet for in vivo liver fat quantification. A gradient field of 73.5 G/cm and a field strength of 0.0725 T were obtained by structurally optimizing the concave U-shaped magnet, on which the region of interest (ROI) was a curved shape about 0.4 mm thick, 8 cm above the surface of the radiofrequency (RF) coil. We constructed a prototype nuclear magnetic-resonance (NMR) relaxometry system based on this optimized magnet. Subsequent phantom experiments demonstrated the effectiveness of the single-sided magnet in evaluating different proton density fat fraction (PDFF) phantoms. As expected, the results of the six phantoms showed good positive correlation between PDFF and the fitted fat amplitude, which suggested that single-sided NMR relaxometry could be used to quantify liver fat in vivo.

Characterization of Structural Bone Properties through Portable Single-Sided NMR Devices: State of the Art and Future Perspectives.

Nuclear Magnetic Resonance (NMR) is a well-suited methodology to study bone composition and structural properties. This is because the NMR parameters, such as the relaxation time, are sensitive to the chemical and physical environment of the 1H nuclei. Although magnetic resonance imaging (MRI) allows bone structure assessment in vivo, its cost limits the suitability of conventional MRI for routine bone screening. With difficulty accessing clinically suitable exams, the diagnosis of bone diseases, such as osteoporosis, and the associated fracture risk estimation is based on the assessment of bone mineral density (BMD), obtained by the dual-energy X-ray absorptiometry (DXA). However, integrating the information about the structure of the bone with the bone mineral density has been shown to improve fracture risk estimation related to osteoporosis. Portable NMR, based on low-field single-sided NMR devices, is a promising and appealing approach to assess NMR properties of biological tissues with the aim of medical applications. Since these scanners detect the signal from a sensitive volume external to the magnet, they can be used to perform NMR measurement without the need to fit a sample inside a bore of a magnet, allowing, in principle, in vivo application. Techniques based on NMR single-sided devices have the potential to provide a high impact on the clinical routine because of low purchasing and running costs and low maintenance of such scanners. In this review, the development of new methodologies to investigate structural properties of trabecular bone exploiting single-sided NMR devices is reviewed, and current limitations and future perspectives are discussed.

Single-Sided Portable NMR Investigation to Assess and Monitor Cleaning Action of PVA-Borax Hydrogel in Travertine and Lecce Stone.

In this work, we investigated the potential of PVA-borax hydrogel for cleaning limestones and the dependence of the cleaning on the porosity of the rock and on the action time of the hydrogel treatment. Towards this goal, we used a nuclear magnetic resonance (NMR) spectrometer, developed for non-invasive and non-destructive applications on cultural heritage. T2-NMR parameters were quantified on different samples of Lecce stone and Travertine cut perpendicular (Pe) and parallel (Pa) to the bedding planes under different experimental conditions: untreated samples, treated with Paraloid B72 and cleaned with PVA-PEO-borax hydrogel applied for 4 min and 2 h. The T2 results suggest that the effectiveness of the cleaning strongly depended on the porosity of the stones. In Lecce stone, the hydrogel seemed to eliminate both the paramagnetic impurities (in equal measure with 4 min and 2 h treatment) and Paraloid B72. In Travertine Pe, characterized by a smaller pore size compared to Lecce stone, no significant effects were found regarding both the cleaning and the treatment with Paraloid B72. In Travertine Pa, characterized by a larger pore size than the other two samples, the hydrogel seemed to clean the paramagnetic agents (it worked better if applied for a longer time) but it did not appear to have any effect on Paraloid B72 removal.

Application of low field magnetic resonance for defect detection in multi-layered cylindrical composite structures

ABSTRACT Polymer-based Glass composite cylindrical structures consisting of multi-layered configuration for special applications were tested with low magnetic field nuclear magnetic resonance (NMR) technique. Relaxation times of chemical species at the interface of adhesive bond were investigated. Studies indicated that the single-sided NMR inspection of such composite structures is a feasible non-destructive evaluation technique to study the adhesive bond interface properties. Results of single-sided inspection over cylindrical surface using low field NMR having magnetic field strength of 0.3 T (12.88 MHz RF frequency) indicated distinct signal intensity values for different constituent materials. Interfacial defects such as de-bond and voids were detectable through the multi-layers of the structure. Overlapping defects at multiple interfaces have no bearing on the signal as well as relaxation times of constituent materials.

The Use of Single-Sided NMR to Study Moisture Behaviour in an Activated Carbon Fibre/Phenolic Composite

Nuclear Magnetic Resonance (NMR) has been shown to be a useful technique to study the form and content of water in polymer composites. Composites using activated carbon fibres with phenolic resin have complex water absorption behaviour which would benefit from such investigation; however, the presence of the conductive fibres can make NMR problematic. In this study, single-sided NMR has been successfully used on such material by developing a method for sample-to-sample compensation for the effect of conductivity. Transverse relaxation curves showed water to be primarily in two states in the resin, corresponding to "bound" and "mobile" molecules. In addition, two much less bound states were identified in the composite, associated firstly with water adsorbed on to the fibre surface and secondly with clusters of water molecules moving more freely within the fibre pores.

Review of the use of NMR spectroscopy to investigate structure, reactivity, and dynamics of lead soap formation in paintings.

Heavy metal carboxylate or soap formation is a widespread deterioration problem affecting oil paintings and other works of art bearing oil-based media. Lead soaps are prevalent in traditional oil paintings because lead white was the white pigment most frequently chosen by old masters for the paints and in some cases for the ground preparations, until the development of other white pigments from approximately the middle of the 18th century on, and because of the wide use of lead-tin yellow. In the latter part of the 19th century, lead white began to be replaced by zinc white. The factors that influence soap formation have been the focus of intense study starting in the late 1990s. Since 2014, nuclear magnetic resonance (NMR) studies have contributed a unique perspective on the issue by providing chemical, structural, and dynamic information about the species involved in the process, as well as the effects of environmental conditions such as relative humidity and temperature on the kinetics of the reaction(s). In this review, we explore recent insights into soap formation gained through solid-state NMR and single-sided NMR techniques.

Effect of Initial Conformation on the Starch Biopolymer Film Formation Studied by NMR.

The formation of a rigid porous biopolymer scaffold from aqueous samples of 1% w/v (suspension) and 5% w/v (gel) corn starch was studied using optical and nuclear magnetic resonance (NMR) techniques. The drying process of these systems was observed using a single-sided NMR scanner by application of the Carr–Purcell–Meiboom–Gill pulse sequence at different layer positions. The echo decays were analyzed and spin–spin relaxation times (T2) were obtained for each layer. From the depth dependent T2 relaxation time study, it was found that the molecular mobility of water within the forming porous matrix of these two samples varied notably at different stages of film formation. At an intermediate stage, a gradual decrease in mobility of the emulsion sample towards the air–sample interface was observed, while the gel sample remained homogeneous all along the sample height. At a later stage of drying, heterogeneity in the molecular dynamics was observed in both samples showing low mobility at the bottom part of the sample. A wide-angle X-ray diffraction study confirmed that the structural heterogeneity persisted in the final film obtained from the 5% corn starch aqueous sample, whereas the film obtained from the 1% corn starch in water was structurally homogeneous.

A phenomenological approach on the influence of paramagnetic iron in cement stone on 2D T1-T2 relaxation in single-sided 1H nuclear magnetic resonance

In recent years, there has been an increasing interest in 1H nuclear magnetic resonance (NMR) relaxometry to obtain information on the hydration and porosity of cement stone. By spin-spin (T2), spin-lattice (T1), and combined relaxation studies, new insights were gained on liquid and crystal bound water as well as pore water exchange. A conversion of relaxation times to pore sizes has been developed and shown to give consistent results. In this study, we use single-sided 1H NMR to obtain two-dimensional T1-T2 relaxation distributions on systematically varied cement stone samples as well as hydrated and solid cement phases. Results show a richness in features beyond past studies and are interpreted qualitatively in terms of water found in chemically different pore environments. Both T1 and T2 surface relaxivity of calcium silicate surrounded liquid water linearly correlate with the cement's Fe2O3 content. Results are discussed based on a theory of interacting surface relaxation mechanisms.

Non-Destructive Quantification of Lipid and Water in Fresh Tuna Meat by a Single-Sided Nuclear Magnetic Resonance Scanner

ABSTRACTA portable single-sided nuclear magnetic resonance (NMR) surface scanner was applied to the non-destructive quantification of lipid and water in meat block samples of farmed bluefin tuna (Thunnus thynnus). Proton NMR relaxation measurements of the fresh meat block samples were performed at room temperature in a laboratory. Totally, 34 tuna meat block samples were measured; the required measurement time was approximately 70 s for each sample. The results yielded estimation errors of 3.7 and 2.7 g/100 g for the lipid and water weight fractions, respectively. The investigation depth of the sensor was as deep as 3 cm, which enables the non-destructive quantification of the meat of the intact whole tuna beneath the thick scales, skin, and subcutaneous fat in markets and seafood factories.