Magnetic Micro Research Articles

Preparation and Characterization of Magnetic Polymeric Micro- and Nanocomposites for Industrial Applications

ABSTRACT To optimize cost and weight and streamline the manufacturing process of existing soft magnetic components, which currently rely on metallic soft magnetic particles, an innovative approach involving the preparation of high-performance magnetic polymeric composites is proposed. These composites are based on soft magnetic ferrite particles with high Curie temperature and magnetic saturation, along with low coercivity and remanent magnetization, and are used as fillers in thermoplastic polymers. To achieve these goals, cobalt ferrite (CoFe2O4) micro- and nanoparticles were synthesized by two different methos: solid-state reaction and coprecipitation. The as-obtained particles were used to fabricate soft magnetic polymer composites by extrusion and injection molding methods. The successful synthesis of cobalt ferrite was confirmed by X-ray diffraction, Fourier transform infrared spectroscopy (FTIR), and Raman spectroscopy. The magnetic behavior of cobalt ferrites and polymer composites was also investigated by vibrating sample magnetometry (VSM). This study shows that these new high-performance soft magnetic polymer composites can be used as alternative materials for the manufacture of magnetic components such as inductors and transformers and that their low cost and lightweight make them suitable for the manufacture of magnetic components.

Application of magnetic AlFu MOF nanocomposite for the extraction and preconcentration of some pesticides from different distillates

This research used a magnetic AlFu nano-metal-organic framework as an adsorbent for the first time. This approach extracts and preconcentrates eight pesticides from various distillates through a two-step process: magnetic dispersive micro solid phase extraction and dispersive liquid-liquid microextraction. Initially, the nanocomposite is dispersed into a sample solution containing the pesticides and Na2SO4. The target pesticides are then adsorbed onto the nanocomposite, which is subsequently isolated from the aqueous phase using an external magnetic field. Acetonitrile is used to elute the adsorbed analytes pesticides from the nanocomposite surface. The resulting acetonitrile extract, containing the concentrated pesticides, is then mixed with a tiny amount of another solvent and injected into a NaCl solution. Centrifugation allows the organic phase, enriched with the pesticides, to settle down. An aliquot of this organic layer is then analyzed using a gas chromatography-flame ionization detector. Optimization of the procedure led to favorable performance, including good extraction recovery of the pesticides (68–98 %), significant enrichment (enrichment factors of 340–489), a wide range of detectable concentrations (2.90–1400 µg L−1), and low detection (0.15–0.88 µg L−1) and quantification limits. (0.49–2.90 µg L−1)

Clay Minerals and Continental‐Scale Remagnetization: A Case Study of South American Neoproterozoic Carbonates

AbstractThe Neoproterozoic carbonate rocks of the Araras Group (Amazon Craton) and the Sete‐Lagoas and Salitre Formations (São Francisco Craton) share a statistically indistinguishable single‐polarity (reversed) characteristic direction. This direction is associated with paleomagnetic poles that do not align with the expected directions for primary detrital remanence. We employ a combination of classical rock magnetic properties and micro imaging/chemical analysis (in thin sections) using synchrotron radiation to examine these remagnetized carbonate rocks. Magnetic data indicate that most samples lack the anomalous hysteresis properties typically associated with carbonate remagnetization (except for distorted loops). Through a combination of Scanning Electron Microscopy with Energy Dispersive X‐ray Spectroscopy (SEM‐EDS), X‐ray Fluorescence (XRF), and X‐ray Absorption Spectroscopy (XAS), we identified subhedral/anhedral magnetite, or spherical grains with a core‐shell structure of magnetite surrounded by maghemite. These grains are within the pseudo‐single domain size range, as do most of the iron sulfides, and are spatially associated with potassium‐bearing aluminosilicates. While fluid percolation and organic matter maturation play a role, smectite‐illitization appears to be crucial for the growth of these phases. X‐ray diffraction analysis, in addition, identifies these silicates as predominantly highly crystalline illite, suggesting exposure to epizone temperatures. These temperatures were likely reached during the final stages of the Gondwana assembly (Cambrian), but remanence was only locked in afterward, in successive cooling events during the Early Middle Ordovician. This is supported by the carbonates' paleomagnetic pole positions compared to Gondwana's apparent polar wander path, and the absence of reversals, contrasting with the high reversal frequency of the Late Ediacaran/Cambrian.

Design of Planar Permanent Magnet Array for Remotely Actuated Magnetic Micro Robots

Design of Planar Permanent Magnet Array for Remotely Actuated Magnetic Micro Robots

Electrochemical deposition of cobalt phosphorus for hard magnetic micro devices and the impact on magnetic anisotropy

When fabricating magnetic components for micro-electro-mechanical systems, the intrinsic material properties as well as the magnetic anisotropy of the deposited material and the fabricated devices must be adjusted to the application. This work focuses on electrochemically deposited cobalt phosphorus layers from a sulfate-based electrolyte to be used as hard magnetic scales in position measurement systems. In preliminary tests round discs (5 mm diameter, 20 or 10 μm height) were fabricated, showing the influence of three process parameters (current density, pH-value and temperature) on the chemical composition and the magnetic behavior of the deposited cobalt phosphorus. Hereby deposition parameters to produce hard magnetic cobalt phosphorus are defined. Deposits with up to 6 wt.-% phosphorus show hard magnetic behavior, whereas deposits with more than 6 wt.-% show soft magnetic behavior. This is correlated with a transition from crystalline to amorphous structures. In further investigations arrays of micro scales (40 μm width, 10 μm height) were fabricated to show the influence of direct current and pulsed current on the properties of the deposits. Pulsed current increases coercive field strength by about 40 %, resulting in maximum values of 23 kA/m (in-plane) and 14 kA/m (out-of-plane). Remanence increases by about 30 %, resulting in maximum values of 0.40 T (in-plane) and 0.2 T (out-of-plane). Pulse plating changes preferred orientation from (110) to (100) and slightly increases grain size by about 20 %, resulting in an average grain size of 25 nm.

Enhancing Magnetic Micro- and Nanoparticle Separation with a Cost-Effective Microfluidic Device Fabricated by Laser Ablation of PMMA.

Superparamagnetic iron oxide micro- and nanoparticles have significant applications in biomedical and chemical engineering. This study presents the development and evaluation of a novel low-cost microfluidic device for the purification and hyperconcentration of these magnetic particles. The device, fabricated using laser ablation of polymethyl methacrylate (PMMA), leverages precise control over fluid dynamics to efficiently separate magnetic particles from non-magnetic ones. We assessed the device's performance through Multiphysics simulations and empirical tests, focusing on the separation of magnetite nanoparticles from blue carbon dots and magnetite microparticles from polystyrene microparticles at various total flow rates (TFRs). For nanoparticle separation, the device achieved a recall of up to 93.3 ± 4% and a precision of 95.9 ± 1.2% at an optimal TFR of 2 mL/h, significantly outperforming previous models, which only achieved a 50% recall. Microparticle separation demonstrated an accuracy of 98.1 ± 1% at a TFR of 2 mL/h in both simulations and experimental conditions. The Lagrangian model effectively captured the dynamics of magnetite microparticle separation from polystyrene microparticles, with close agreement between simulated and experimental results. Our findings underscore the device's robust capability in distinguishing between magnetic and non-magnetic particles at both micro- and nanoscales. This study highlights the potential of low-cost, non-cleanroom manufacturing techniques to produce high-performance microfluidic devices, thereby expanding their accessibility and applicability in various industrial and research settings. The integration of a continuous magnet, as opposed to segmented magnets in previous designs, was identified as a key factor in enhancing magnetic separation efficiency.

Magnetically Guided Microcatheter for Targeted Injection of Magnetic Particle Swarms.

The initial delivery of small-scale magnetic devices such as microrobots is a key, but often overlooked, aspect for their use in clinical applications. The deployment of these devices within the dynamic environment of the human body presents significant challenges due to their dispersion caused by circulatory flows. Here, a method is introduced to effectively deliver a swarm of magnetic nanoparticles in fluidic flows. This approach integrates a magnetically navigated robotic microcatheter equipped with a reservoir for storing the magnetic nanoparticles. The microfluidic flow within the reservoir facilitates the injection of magnetic nanoparticles into the fluid stream, and a magnetic field gradient guides the swarm through the oscillatory flow to a target site. The microcatheter and reservoir are engineered to enable magnetic steering and injection of the magnetic nanoparticles. To demonstrate this approach, experiments are conducted utilizing a spinal cord phantom simulating intrathecal catheter delivery for applications in the central nervous system. These results demonstrate that the proposed microcatheter successfully concentrates nanoparticles near the desired location through the precise manipulation of magnetic field gradients, offering a promising solution for the controlled deployment of untethered magnetic micro-/nanodevices within the complex physiological circulatory systems of the human body.

Separation and purification of hyaluronic acid by [formula omitted] nano and micro particles coated with chitosan and silica

Hyaluronic acid (HA), a glycosaminoglycan, is comprised of alternating units of D-glucuronic acid and N-acetylglucosamine. This compound harbors numerous biomedical applications, including its use in pharmaceuticals, wound healing, osteoarthritis treatment, and drug delivery. Its unique composition and exceptional features, such as its high water-absorbing and retaining capacity, have also led to its use in the cosmetics industry. The employment of this biopolymer has given rise to an escalation in the request for its manufacture. The present investigation has explored the correlation between hyaluronic acid and chitosan and silica for the purpose of separation. Consequently, Iron oxide magnetic nano particles and micro particles were produced via co-precipitation method and were layered with chitosan and silica to purify the hyaluronic acid from the fermentation broth that was generated by Streptococcus Zooepidemicus. The size distribution and zeta potentials of the two kinds of particles were gauged with the aid of a dynamic laser light scattering apparatus and zeta potential meter (Malvern, Zeta master) respectively. The confirmation of the chemical structure of the Fe3O4 nanoparticles and Fe3O4 particles conjugated with chitosan and silica was accomplished through the utilization of Fourier Transform Infrared Spectroscopy (FT-IR). Protein contamination was thoroughly characterized by means of sodium dodecyl-sulfate polyacrylamide gel electrophoresis (SDS-PAGE) and Nanodrop 2000/2000c spectrophotometers protein estimation method. The maximum HA adsorption capacity, under optimal pH conditions of 4, was determined to be 87 mg/g, 112 mg/g, 51 mg/g, and 44 mg/g for Fe3O4 −chitosan nanoparticle, Fe3O4 −chitosan micro particle, Fe3O4 −silica microparticle, and Fe3O4 −silica nanoparticle, respectively.

Simultaneous and Independent Control of Multiple Swimming Magnetic Microrobots by Stabilizer Microrobot

This paper presents a new strategy for simultaneous control of multiple magnetic Micro Robots (MRs) improving stability and robustness with respect to external disturbances. Independent control of multiple MRs, can enhance efficiency and allows for performing more challenging applications. In this study, we present a system consisting of a Helmholtz coil and 2N Permanent Magnets (PMs), rotated by servomotors, to control several MRs. We have also improved the system’s stability by adding a larger MR (stabilizer MR). This MR can be moved all around the workspace and works as a moving internal magnetic field source. Thanks to this moveable magnetic field, other MRs are more stable against environmental disturbances. By simulating simultaneous and independent control of multiple MRs, we demonstrate the advantages of using the stabilizer MR (more than 20 percent reduction in tracking error and control effort). In addition, we evaluate experimentally our proposed method to independently control the position of three MRs using a stabilizer MR demonstrating the efficacy of the strategy.

Magnetic Micro and Nano Sensors for Continuous Health Monitoring

Magnetic micro and nano sensors can be used in a broad variety of applications, e.g., for navigation, automotives, smartphones and also for health monitoring. Based on physical effects such as the well-known magnetic induction, the Hall effect, tunnel magnetoresistance and giant magnetoresistance, they can be used to measure positions, flow, pressure and other physical properties. In biomedicine and healthcare, these miniaturized sensors can be either integrated into garments and other wearables, be directed through the body by passive capsules or active micro-robots or be implanted, which usually necessitates bio-functionalization and avoiding cell-toxic materials. This review describes the physical effects that can be applied in these sensors and discusses the most recent micro and nano sensors developed for healthcare applications.

Synthesis, Characterization, and Electrochemical Study of Novel Porphyrin Derivatives as Corrosion Inhibitors for Carbon Steel in HCl Solutions

This study involves the synthesis of some porphyrins derivatives, these are termed as 4,4',4'',4'''-(porphyrin-5,10,15,20-tetrayl)tetrakis(N-(6-aminoacridin-3-yl)benzamide) (3a), 4,4',4'',4'''-(porphyrin-5,10,15,20-tetrayl)tetrakis(N-(5-methoxybenzo[d]thiazol-2-yl)benzamide) (3b), 4,4'-(10,20-bis(3-hydroxyphenyl)porphyrin-5,15-diyl)bis(N-(6-aminoacridin-3yl)benzamide) (5a), and 4,4'-(10,20-bis(3-hydroxyphenyl)porphyrin-5,15-diyl)bis(N-(benzo[d]thiazol-2-yl)benzamide) (5b). These derivatives were synthesized using open circuit potential (OCP) and potentiodynamic polarization (PDP) in 0.1 M HCl solution methods. These derivatives were characterized using nuclear magnetic resonance (1H- and 13C-NMR) spectroscopy, mass spectra (ESI), and micro elemental analysis (CHN). The activity of these synthesized materials was investigated as a corrosion inhibitor using carbon steel (CS) as a model for corroded materials. The obtained results showed that the synthesized porphyrins derivatives were effective corrosion inhibitors to 0.1 M HCl solution for CS. In the case of the derivative 3a, a maximum inhibition efficiency (IE%) was recorded and it was around 74%. The derivative 3b showed an IE% of around 68.11%, while the %IE of 5a and 5b were around 18.98% and 45.16%, respectively. The best IE% value that was recorded for the derivative 3a has the potential to be effective anticorrosive coatings for industrial applications and act as mixture inhibitor because their ΔEcorr values are less than 85 mV. On the CS surface following treatment with compound 3a, the inhibitor mechanism for acidic medium (HCl) was investigated.

Semi–Bone Tunnel Technique Using Double-Row Suture Bridge Combined With Platelet-Rich Plasma Hydrogel for Rotator Cuff Repair in a Rabbit Model

Background: The approach to managing the footprint area and reconstructing the tendon-bone interface (TBI) is critical for optimal healing. Purpose: To evaluate the outcomes of the semi–bone tunnel (SBT) technique using a double-row suture bridge combined with platelet-rich plasma (PRP) hydrogel for rotator cuff repair in a rabbit model. Study Design: Controlled laboratory study. Methods: A total of 48 New Zealand White rabbits were divided into 4 groups. The supraspinatus tendons were severed at the footprint to create a rotator cuff tear model in the surgical groups. Rabbits were treated with the traditional onto-surface repair (control group), SBT technique (SBT group), and SBT technique combined with PRP hydrogel implantation (SBT+PRP group). The rabbits without surgery were the normal group. At 8 weeks after surgery, macroscopic observation, magnetic resonance imaging (MRI) and micro–computed tomography (μCT) examinations, histological evaluations, and biomechanical tests were performed to assess the curative effects of the given treatments. Results: The MRI results showed that the repaired supraspinatus tendon presented a uniform signal, minimal inflammatory response, and the lowest signal-to-noise quotient value in the SBT+PRP group. The μCT results suggested that the SBT technique did not reduce the local bone mineral density in the TBI area compared with the onto-surface repair technique. The histological staining results showed that the regenerated TBI in the SBT+PRP group had a 4-layer structure similar to the natural tissue. The highest values for biomechanical properties were observed in the SBT+PRP group, and there was no significant difference between the SBT+PRP group and normal group. Conclusion: The SBT technique presented a better tendon-bone healing effect for rotator cuff tear in the rabbit model compared with the traditional onto-surface repair technique. The specimens in the SBT+PRP group had a similar TBI structure and biomechanical properties to the natural tissue. Clinical Relevance: The SBT technique can be an alternative surgical approach for rotator cuff repair, especially for moderate to large tears and cases requiring scaffold implantation.

Synthesis of the magnetic composite of Ni-MOF-I in aqueous medium and its application in magnetic dispersive micro solid phase extraction of plasticizers from pharmaceutical samples

For the first time, this research presents the synthesis procedure and analytical application of Ni-MOF-I magnetic composite. The synthesis method was green and done in an aqueous medium. The composite was employed as an adsorbent in a magnetic dispersive solid phase extraction process followed by dispersive liquid–liquid microextraction for the extraction and preconcentration of some plasticizers from pharmaceutical samples stored in plastic containers. The Ni-MOF-I magnetic composite was characterized by applying Fourier transform infrared spectrophotometry, vibrating sample magnetometry, scanning electron microscopy, energy-dispersive X-ray, X-ray diffraction, and nitrogen adsorption/desorption analyses. For operating the extraction procedure, initially, the plasticizers were adsorbed onto the adsorbent particles by vortexing. Then, the plasticizers were desorbed from the adsorbent surface using a mL volume of 2-proponal. Subsequently, the obtained eluate phase was mixed with a mixture of 1,2-dibromoethane and 1,1,2-trichloroethane and then injected into deionized water using a glass syringe. Afterward, centrifugation was done to isolate the extractant from the aqueous phase. Eventually, one microliter of the sedimented phase was injected into gas chromatography-flame ionization detection. Acceptable analytical results such as high enrichment factors (355–415) and extraction recoveries (71–83 %), low limits of quantification (0.76–1.08 μg L−1) and detection (0.23–0.33 μg L−1), wide linear ranges (1.08–300 μg L−1), and satisfactory relative standard deviation values of 4.0–6.3 % (intra-day precision, n = 5) and 4.9–7.4 % (inter-day precision, n = 5) were achieved. The suggested procedure was used as a productive analytical method based on the Ni-MOF-I magnetic composite for the extraction and determination of some plasticizers from different pharmaceutical samples filled in plastic containers. Elimination of centrifugation, using 2-propanol as a green desorption/disperser solvent, detection of di-(2-ethylhexyl) phthalate in boric acid alcohol drop, and applying µL-level of the extraction solvent are the advantages of this proposed method.

Development of real-time navigation system for laparoscopic hepatectomy using magnetic micro sensor

Background We report a new real-time navigation system for laparoscopic hepatectomy (LH), which resembles a car navigation system. Material and methods Virtual three-dimensional liver and body images were reconstructed using the “New-VES” system, which worked as roadmap during surgery. Several points of the patient’s body were registered in virtual images using a magnetic position sensor (MPS). A magnetic transmitter, corresponding to an artificial satellite, was placed about 40 cm above the patient’s body. Another MPS, corresponding to a GPS antenna, was fixed on the handling part of the laparoscope. Fiducial registration error (FRE, an error between real and virtual lengths) was utilized to evaluate the accuracy of this system. Results Twenty-one patients underwent LH with this system. Mean FRE of the initial five patients was 17.7 mm. Mean FRE of eight patients in whom MDCT was taken using radiological markers for registration of body parts as first improvement, was reduced to 10.2 mm (p = .014). As second improvement, a new MPS as an intraoperative body position sensor was fixed on the right-sided chest wall for automatic correction of postural gap. The preoperative and postoperative mean FREs of 8 patients with both improvements were 11.1 mm and 10.1 mm (p = .250). Conclusions Our system may provide a promising option that virtually guides LH.

A novel deep eutectic solvent modified magnetic covalent organic framework for the selective separation and determination of trace copper ion in medicinal plants and environmental samples

BackgroundPretreatment techniques should be introduced before metal ion determination because there is very low content of heavy metals in Chinese medicinal plants and environmental samples. Magnetic dispersive micro solid phase extraction (MDMSPE) has been widely used for the separation and adsorption of heavy metal pollutants in medicinal plants and environmental samples. However, the majority of MDMSPE adsorbents have certain drawbacks, including low selectivity, poor anti-interference ability, and small adsorption capacity. Therefore, modifying currently available adsorption materials has gained attention in research. ResultsIn this study, a novel adsorbent MCOF-DES based on a magnetic covalent organic framework (MCOF) modified by a new deep eutectic solvent (DES) was synthesized for the first time and used as an adsorbent of MDMSPE. The MDMSPE was combined with inductively coupled plasma optical emission spectrometry (ICP-OES) for selective separation, enrichment, and accurate determination of trace copper ion (Cu2+) in medicinal plants and environmental samples. Various characterization results show the successful preparation of new MCOF-DES. Under the optimal conditions, the enrichment factor (EF) of Cu2+ was 30, the limit of detection (LOD) was 0.16 μg L−1, and the limit of quantitation (LOQ) was 0.54 μg L−1. The results for the determination of Cu2+ were highly consistent with those of inductively coupled plasma mass spectrometry (ICP-MS), which verified the accuracy and reliability of the method. SignificanceThe established method based on a new adsorption material MCOF-DES has achieved the selective separation and determination of trace Cu2+ in medicinal and edible homologous medicinal materials (Phyllanthus emblica Linn.) and environmental samples (soil and water), which provides a promising, selective, and sensitive approach for the determination of trace Cu2+ in other real samples.

The simultaneous measurement of atomoxetine, venlafaxine, and duloxetine in actual water and biological samples requires the creation of a unique magnetic dispersive micro solid phase extraction sorbent based on MOF-on-MOF

ABSTRACT Atomoxetine, venlafaxine, and duloxetine are three antidepressant drugs widely prescribed to treat this disorder. Determining these drugs is a major challenge due to their low concentration and high matrix effects on biological samples. Dispersive micro solid phase extraction was developed as a sample preparation strategy to extract these drugs in real water and biological samples. A novel sorbent containing a magnetic MOF-on-MOF was prepared to extract these drugs using Fe3O4 nanoparticle and Sol-gel technique. The microextraction procedure was optimised under two steps using experimental design. Three factors, including pH, sorbent amount, and desorption solvent volume, significantly affected the extraction of analytes and optimised using a central composite design. The optimum value of pH, sorbent amount, and desorption solvent volume was 29 mg, 6.5, and 150 µL. Under optimum conditions, the linear ranges for measuring atomoxetine, venlafaxine, and duloxetine in water samples were 1.42–496, 0.43–472, and 0.73–459 ng mL−1, respectively. The detection limits of atomoxetine, venlafaxine, and duloxetine were 0.4, 0.1, and 0.2 ng mL−1. High and proper preconcentration factors ranged from 462.4–511.4 in distiled water samples and 450.7–489.8 in urine samples were obtained to determine atomoxetine, venlafaxine, and duloxetine with three concentrations of 5.0, 20.0, and 100.0 ng mL−1, respectively. Inter-day and intra-day RSD% were calculated by triplicate determination of atomoxetine, venlafaxine, and duloxetine at three concentrations of 10.0, 50.0 and 100.0 ng mL−1 and were between 3.2–4.3% and 3.8–4.6% in distiled water samples, and 4.8–5.7% and 5.0–5.8% in urine samples, respectively. Analysis of tap, river water, and two urine samples as real water and biological samples under optimum conditions exhibited recovery and standard deviation in the ranges of 90.2–96.9% and 3.84–5.74%, respectively, confirmed the proper ability of the method to determine atomoxetine, venlafaxine, and duloxetine in natural water and biological samples.

Natural ferromagnetic resonance in microwires and its applications. Brief review

The paper analyzes technological aspects of the Taylor–Ulitovsky method used to produce microwires of various structures. Natural ferromagnetic resonance (NFMR) in cast glass-coated amorphous magnetic micro- and nanowires was theoretically and experimentally studied. The NFMR phenomenon is due to the large residual stresses appearing in the core of the microwire during the casting process. These stresses, along with magnetostriction, determine magnetoelastic anisotropy. Besides residual stresses, the NFMR frequency is influenced by externally applied stresses on the microwire or the composite containing the so-called stress effect (SE). The dependence of the NFMR frequency on the deformation of microwires and the external stresses on them is proposed to be used for remote diagnostics in medicine

Studying water infiltration on bentonite/sand blocks with MRI and X-Ray μCT techniques

Radioactive waste management agencies all around the world are focusing their efforts to provide a reliable technical solution to the Deep Geological Disposal (DGD) concept, in order to store high level (HLW) and intermediate level long lived (IL-LLW) radioactive waste. The protection and isolation of radionucleides is guaranteed by a set of barriers. Bentonite/sand blocks -in proportion of 40/60 on dry mass of the mixture- constitute the main core of the sealing barrier in the French concept run by the French National Radioactive Waste Management Agency (Andra). Its high swelling potential (>2MPa) during hydration, its low hydraulic permeability (<10-11 m/s) and its gas entry pressure (<2MPa) make it ideal to seal the DGD galleries excavated inside the host rock used as geological barrier. Bentonite/sand blocks are placed at unsaturated state during construction. Afterwards, water migration –in both liquid and vapour states- from the saturated host rock to the blocks will induce the humidification of the blocks until hydraulic equilibrium is reached, hypothetically reaching the saturation state. As this natural process will take hundreds of years, a multitude of experimental devices have been reported at laboratory [3, 5] and real scale [4] to understand the evolution of water transfer in bentonite mixtures and support the predictions of numerical models [1]. In laboratory experiments, samples made of a compacted bentonite mixture are usually placed inside a rigid cell connected to a water source. The infiltration of water is not measured directly but deduced by relative humidity gradients measured along the specimen height.
 Numerical models and experimental results have not yet reached accurate predictions of how long it takes for bentonite mixtures to hydrate until complete saturation or how the unsaturated hydraulic permeability evolves. In this context, there is a motivation to study this phenomena by advanced techniques able to capture, image and quantify water transfer through porous media. Thus, an experimental campaign based on Magnetic Resonance Imaging (MRI) and 3D X-Ray micro computed tomography (µCT) is proposed to analyze water infiltration in bentonite/sand blocks. MRI is extensively used in health sciences to create images where the contrast is given by the water’s hydrogen proton content in the different tissues of the body. For geological media, where water content is much smaller than in biological tissues and relaxation times of the porewater are shorter -from 0.1 to 2 ms for compacted bentonite/sand [2]- the experimental requirements are different and less documented. On the other hand, µCT scanning provides high spatial resolution images based on the contrast between the X-Ray absorption properties of the constitutive phases observed. Its temporal variations, in a bentonite/sand mixture, might be the result of concurrent phenomena, namely, porosity and saturation changes together with heterogenous motions induced by hydromechanical couplings -the swelling of bentonite solids when they absorb water-.
 On going MRI and µCT experimental campaigns on a PEEK cell aim at proving the suitability of these techniques to track the evolution of water infiltration in compacted bentonite/sand mixtures, characterizing the water front and the water content along the specimen in function of time. At this stage, preliminary MRI tests have shown the potential of Single Point Imaging (SPI) sequence to quantify, with one-dimensional images, the water content along the bentonite/sand specimen based on a linear correlation with its signal intensity. Preliminary X-Ray radiography tests (Figure 1) run on a cylindric cell of PMMA filled with small blocks of 12 mm in diameter and 10 mm high, prove that X-Ray radiography image analysis gives access to observable and quantifiable increase of absorption associated to the measured decrease in grey level at different transversal sections of the sample. This evolution is linked to the increase of apparent density of the solids -that indeed are absorbing the water-, as described by the Beer-Lambert equation. Even though apparent density increase is goverened by the augmentation of water content, changes in porosity due to the hydromechanical coupling along the sample cannot be neglected. Thus, observing the liquid phase evolution (hydraulics) by MRI, as well as the evolution of the solid/liquid phase (hydromechanics) by 3D-µCT imaging, will potentially provide complementary insight into the mechanisms governing water infiltration in bentonite/sand mixtures.

Synthesis of Prussian blue-embedded magnetic micro hydrogel for scavenging of cesium from aqueous solutions; Batch and dynamic investigations

A magnetic micro porous structure composite based on alginate and Prussian blue (M-SA-PB) was simply prepared for cesium removal from the aqueous solutions. The gelation and formation of PB proceeded through the same step, which made the PB homogenously distributed and firmly attached to the alginate matrix. The homogenizer was applied to break down the bulky gel structure into micro-ones, and the lyophilizer will provide the porous structure. Batch cesium sorption experiments showed that the adsorption kinetics and isotherms were attributed to the pseudo-second-order model and Langmuir isotherm. Moreover, the Cs-ion is favorably adsorbed on the M-SA-PB composite surface as a monolayer towards Cs, with a maximum adsorption capacity reach of 191.0 mg/g. Furthermore, the M-SA-PB adsorbent showed excellent adsorption selectivity of Cs from multiple-ion solutions. Our work was extended to use the M-SA-PB composite in dynamic cesium sorption. The column studies showed that the removal efficiency of Cs+ increased with increasing bed depth as well as the initial cesium concentration. Finally, as previously mentioned, the M-SA-PB could be considered an excellent Cs+ scavenger employing both batch and dynamic approaches, which makes it a promising adsorbent for practical investigations.

Carbon nanotubes/metal-organic framework based magnetic dispersive micro-solid phase extraction for the determination of triazole fungicides in wastewater and soil samples

In this research, the magnetic dispersive micro solid phase extraction (M−D-µ-SPE) method was used for pre-concentration and trace detection of triazole fungicides in agricultural wastewater and soil samples. The nano sorbent used for M−D-µ-SPE is based on a magnetic carbon nanotubes/Cu-based MOF (M−MWCNT−Cu−BDC) nanocomposite, which was synthesized and characterized by X-ray diffraction, Fourier-transform infrared spectroscopy, field emission scanning electron microscopy, energy-dispersive X-ray spectroscopy, vibrating-sample magnetometer, and Nitrogen adsorption-desorption analysis. The effective parameters on the extraction performance were optimized, and under the optimized conditions (pH value: 7.0; the amount of sorbent: 30 mg; extraction time: 30 min; desorbing agent: ethanol; the volume of desorbing solvent: 500 μL and desorption time: 5 min), the limits of detection (LOD) was 0.45 ng mL−1, and the linear range was 1.50 to 750 ng mL−1 with a correlation coefficient higher than 0.993. The repeatability (RSD%) of the method for five replicates ranged from 2.8 to 5.5%. High recoveries (91–94%) and excellent preconcentration factor (PF = 91–94) were also obtained. Finally, this method was applied to determine triazole fungicides in agricultural wastewater and soil samples.