Sample Material Research Articles

Diffusion of radioactive waste elements from underground water and leachates of phosphate waste forms in pore solution of clay materials

Using through diffusion method at room temperature, migration of RW element simulators (P, Se, Br, Mo, Cs, U) in compacted samples of clay materials of various mineral compositions was studied during porous diffusion from model solutions: underground water and leachates of phosphate waste forms having a total salt content of up to 500 mg/L. Based on the results of experiments, effective diffusion coefficients and sorption distribution coefficients of elements in barrier materials were determined. Numerical models are proposed to describe diffusion transfer of selenium, cesium and uranium depending on porosity, mineral composition of materials, and concentration of elements in pore solution. Patterns of diffusion of elements from solutions of different salt composition were revealed.

ITER materials irradiation within the D–T neutron environment at JET: post-irradiation radioactivity analysis following the DTE2 experimental campaign

Abstract This work presents the results following the first irradiation of ITER materials samples in a tokamak D--T plasma environment operating at significant fusion power. The materials exposed to this nuclear environment at the Joint European Torus during the DTE2 experimental campaign that took place in 2021 include representative ITER samples from various components such as poloidal field (PF) coil jacket samples, toroidal field coil radial closure plate steels, EUROFER 97 steel, W and CuCrZr materials from the divertor, Inconel-718, CuCrZr, and 316L stainless steel for blanket modules, as well as vacuum vessel forging samples.

The experimental results discussed include high-resolution gamma spectrometry measurements and analysis conducted with the post-irradiated samples, of which there were 68 in total. These samples were exposed through different experimental campaigns, including deuterium, deuterium--tritium and tritium phases. Supporting the analysis were 25 dosimetry foil-based neutron diagnostics and two 'VERDI' neutron spectrometry diagnostics. A further 12 samples for positron annihilation spectroscopy (PALS) were also irradiated. The irradiation of all these samples took place in a long-term irradiation assembly located near the JET vacuum vessel.

The post-irradiation analysis of the ITER material samples has yielded valuable insights into their material activation levels and radiation fields. Comparative assessments between experimental measurements and comprehensive neutronics simulations have demonstrated a significant level of agreement in this work, while also revealing some discrepancies in specific material instances. The data and interpretation from this work not only serve as a robust experimental foundation for enhancing the precision and predictability of neutronics simulation approaches for ITER and next-step devices but also present some opportunities for the refinement of simulation methodologies. In light of these findings, a series of recommendations have been proposed, aimed at improving confidence in nuclear predictions associated with materials that have been exposed to fusion nuclear environments and advancing understanding in this important domain.

Towards a data platform for multimodal 4D mechanics of material microstructures

This paper presents advances in the data management strategy applied to 4D multimodal mechanics of material sample microstructures. Guidelines to build a data platform allowing for complex workflows, involving several high-throughput experimental and numerical techniques, and complying with FAIR data management principles, are discussed. Next, their implementation within the open-source Python package Pymicro is presented, offering a high-level interface to build complex datasets through multimodal methodologies. Its capability to enable and automate complex workflows by building a digital twin of a commercially pure titanium sample under tension are then demonstrated. The digital twin contains microstructural and mechanical data for thousands of grains gathered on the same sample through synchrotron DCT and in-situ SEM experiments, as well as full-field numerical simulation. Finally, a local and statistical comparison between simulation and measurements of plastic slip and crystal rotation in hundreds of grains is shown, as an example of the contribution of this platform to multimodal data convergence and its importance for the development of a new generation of material models.

Foam density measurement using a 3D scanner

In this work, we used a 3D scanner for the volume measurement of foamed samples, a long-standing problem in the density evaluation of foams. The 3D scanning density measurement method can be selected as an alternative to or in combination with well-established, classical methods that involve the use of instruments like a caliper, a pycnometer, or other devices based on displacement or flotation principles. In particular, the classical methods show some limitations when the foamed sample geometry is irregular, when the polymer is highly hygroscopic, and when it has open porosities. We have tested numerous foamed samples of different sizes, shapes, densities, materials, and morphologies. We utilized different 3D scanner configurations for their volume measurement and compared the results with geometrical and displacement methods, when possible. Results showed that the proposed method is highly accurate, reproducible, and simple, although some specific precautions should be put in place to avoid misinterpretation by the shape-reconstructing software.

Determination of Aloin A, Aloin B, and Aloe-Emodin in Raw Materials and Finished Products Using HPLC Multi-Laboratory Validation Study, AOAC 2016.09, Final Action Status.

A multi-laboratory validation study was performed on AOAC Official Method of Analysis (OMA) 2016.09, for final action. Eight different laboratories throughout the world participated in the study tested the same set of 6 different laboratory samples of raw materials (commercial) and formulated products (commercial), and all the laboratories successfully generated results within the acceptance criteria. The intention of the study was to evaluate specificity, precision (variation), linearity/range, system suitability, limit of detection (LOD), and limit of quantitation (LOQ) by multiple laboratories to satisfy the requirement of moving the OMA 2016.09 to the final action status. Accuracy and ruggedness were already validated in earlier work of single laboratory validation (1), and it was not necessary to include these validation parameters in the multi-laboratory validation study. Laboratory samples containing Aloe were sent out to participating laboratories. Each lab followed AOAC 2016.09 (First Action status) to analyze contents of aloin A, aloin B, and aloe emodin using high performance liquid chromatography (HPLC) instrument. The results generated by each laboratory were collected and evaluated. The specificity results show that blank and matrix chromatograms do not contain major interfering peaks on the retention time of aloin A, aloin B, and aloe-emodin. The precision (variation) results of duplicated preparations are not more than 0.05 parts per million (ppm) different. The linearity/range results from six standards (10 parts per billion (ppb), 20 ppb, 40 ppb, 80 ppb, 160 ppb, and 500 ppb) have correlation coefficient (R) value of ≥ 0.999. The system suitability results meet the acceptance criteria to show the instrument validity. The limit of detection (LOD) results show that the signal-to-noise (S/N) ratio of 10 ppb standards for all three components are about 3. The limit of quantitation (LOQ) results show that the S/N ratio of 20 ppb standards for all three components are about 10. The validation parameters (specificity, precision (variation), linearity/range, system suitability, LOD, and LOQ) have been successfully analyzed, and it shows that the test method is suitable for its intended use. The test method has been successfully validated by the eight different laboratories around the world (US, UK, Germany, and Canada). Each of the laboratory is managed independently by the site lab management team. This multi-lab study validated the method of Determination of Aloin A, Aloin B, and Aloe-Emodin in Raw Materials and Finished Products Using high performance liquid chromatography (HPLC), and the method fits for its intended purpose.

On the determination of charge and nitrogen content in cellulose fibres modified to contain quaternary amine functionality

Research interest in quaternization of cellulose fibres has increased considerably over the past decades. However, there is little or no consensus regarding how to characterize the material in terms of degree of substitution (DS), and the literature suggests a range of different methods focusing on charge determination as well as nitrogen content quantification. This work aims to fill the knowledge gap regarding how the different methods perform in relation to each other, and for what cellulosic systems each method has advantages, disadvantages and even potential pitfalls. FT-IR and NMR measurements are used to establish successful modification and determine the relative number of substituent groups. Another six methods are compared for the determination of the DS of cellulosic fibres and nanofibrils. The methods include Kjeldahl measurements, nitrogen determination by chemiluminescence, determination of molecular nitrogen by the Dumas method, colloidal titration, conductometric titration and polyelectrolyte adsorption. It can be concluded that most techniques investigated are reliable within certain ranges of DS and/or when using appropriate post-treatment of the quaternized material and suitable sample preparation techniques. The results from the present work hence provide recommendations to make an educated choice of method, and experimental protocol, based on the technique at hand.

Molten Aluminum-Induced Corrosion and Wear-Resistance Properties of ZrB2-Based Cermets Improved by Sintering-Temperature Manipulation.

During the hot dip aluminum plating process, components such as sinking rollers, pulling rollers, and guide plates will come into long-term contact with high-temperature liquid aluminum and be corroded by the aluminum liquid, greatly reducing their service life. Therefore, the development of a material with excellent corrosion resistance to molten aluminum is used to prepare parts for the dipping and plating equipment and protect the equipment from erosion, which can effectively improve the production efficiency of the factory and strengthen the quality of aluminum-plated materials, which is of great significance for the growth of corporate profits. With AlFeNiCoCr as the binder phase and ZrB2 as the hard phase, ZrB2-based ceramic composites were prepared by spark plasma sintering (SPS). SEM, EDS and XRD were used to characterize the microstructure and properties of the sintered, corroded, and abraded material samples. The density, fracture toughness, corrosion rate and wear amount of the composite material were measured. The results show that ZrB2-AlFeNiCoCr ceramics have compact structure and excellent mechanical properties, and the density, hardness and fracture toughness of ZrB2-AlFeNiCoCr increase with the increase in sintering temperature. However, when the composite material is at 1600 °C, the relative density of the sintering at 1600 °C decreases due to the overflow of the bonding phase. Therefore, when the sintering temperature is 1500 °C, the high entropy alloy has the best performance. The average corrosion rate of ZrB2-1500 at 700 °C liquid aluminum is 1.225 × 10-3 mm/h, and the wear amount in the friction and wear test is 0.104 mm3.

Heat capacity measurements by a Setaram μDSC3 evo microcalorimeter: estimation of deviation in the measurement, advanced data analysis by mathematical gnostics, and prediction by the artificial neural network

AbstractThe aim of the work is to study the variation in the isobaric heat capacity measurement due to changes in the amount of sample and the calibration standard using a Setaram $$\mu$$ μ DSC3 evo microcalorimeter batch cells to provide a guideline toward the selection of the sample amount to minimize heat capacity measurement error in $$\mu$$ μ DSC. Moreover, overall variation, variation due to the sample amount, and variation due to the calibration standard (reference) amount in heat capacity measurement were estimated for different amounts of the sample or/and the calibration standard material. In the present work, heat capacity measurements were taken for [C4mim][Tf2N] (1-butyl-3-methylimidazolium bis[(trifluoromethyl)sulfonyl]imide) ionic liquid as a sample material and 1-butanol as a calibration standard. A novel non-statistical approach, mathematical gnostics (MG), was used for data analysis of measured heat capacities data. Moreover, the artificial neural network (ANN) model was developed to predict the deviation in the heat capacity measurement with 99.83% accuracy and 0.9939 R2 score. The Python package PyCpep based on the trained ANN model was developed to predict the deviation in the heat capacity measurement.

Studying the Influence of some Technological Factors on the Properties of Nitrocellulose-cellulose Material Sheets

This study presents the results of manufacturing cellulose-cellulose nitrate materials using paper-making equipment in the laboratory Rapid-Kothen. Determine the influence of the ratio of components, pulp grinding, additives, and lamination technology on the properties of cellulose-cellulose nitrate materials. Using chemical analysis, the technical specifications of some UKP pulps were analyzed and US softwood UKP pulps were selected for use in research. Through SEM images and experiments, it is shown that the morphology of NC greatly affects the remaining nitrate cellulose content in the material. NC-C material samples with different mixing ratios, using pulp with different grinding degrees were also investigated for mechanical properties and the degree of preservation of materials on the mesh. The influence of additives such as cationic starch and carboxymethyl cellulose (CMC) on the mechanical properties of the material was also investigated. Lamination using nitrate cellulose glue or alcohol:ether solvent mixture can significantly increase the mechanical properties of the material.

Enhanced Scratch Detection for Textured Materials Based on Optimized Photometric Stereo Vision and Fast Fourier Transform–Gabor Filtering

In the process of scratch defect detection in textured materials, there are often problems of low efficiency in traditional manual detection, large errors in machine vision, and difficulty in distinguishing defective scratches from the background texture. In order to solve these problems, we developed an enhanced scratch defect detection system for textured materials based on optimized photometric stereo vision and FFT-Gabor filtering. We designed and optimized a novel hemispherical image acquisition device that allows for selective lighting angles. This device integrates images captured under multiple light sources to obtain richer surface gradient information for textured materials, overcoming issues caused by high reflections or dark shadows under a single light source angle. At the same time, for the textured material, scratches and a textured background are difficult to distinguish; therefore, we introduced a Gabor filter-based convolution kernel, leveraging the fast Fourier transform (FFT), to perform convolution operations and spatial domain phase subtraction. This process effectively enhances the defect information while suppressing the textured background. The effectiveness and superiority of the proposed method were validated through material applicability experiments and comparative method evaluations using a variety of textured material samples. The results demonstrated a stable scratch capture success rate of 100% and a recognition detection success rate of 98.43% ± 1.0%.

Failure analysis of a frangible cover made of short‐cut basalt fiber reinforced epoxy composites

AbstractThe frangible cover made of continuous fiber reinforced composites has become widely used structure for the new generation launch canisters. However, destroying the continuity of fibers is needed during the hand lay‐up process to make the frangible cover fail in predetermined patterns. In this article, composite frangible covers were fabricated with short‐cut basalt fiber reinforced epoxy(BF/Epoxy) composites instead of continuous fiber‐reinforced composite materials, reducing the strength redundancy in the local structure of the frangible covers. Tensile tests were firstly conducted on material samples to obtain the stress–strain characteristics of the short‐cut BF/Epoxy composites. The constitutive model and failure criterion of the short‐cut BF/Epoxy composites material were established. Then failure pressure and failure mode of the frangible covers were predicted by finite element method. Two frangible covers with different geometric parameter were fabricated and subjected to static bursting strength tests. The influence of structure parameter on the bursting pressure of the frangible cover was investigated in detail. it was found that the bursting pressure of the BF/Epoxy composite fragile cover can be tailored by adjusting the geometry size of the weak zones on surface of the cover. Meanwhile, Failure modes and the bursting pressure of the BF/Epoxy composite fragile covers are highly consistent with the predictions.Highlights A frangible cover made of the short‐cut basalt fiber reinforced epoxy(BF/Epoxy) composites was fabricated. The constitutive model and failure criterion were established based on the mechanical properties of the short‐cut BF/Epoxy composites. The static burst strength of the short‐cut BF/Epoxy composite frangible cover subjected to uniform pressure was investigated via both theoretical and experimental approaches. The short‐cut BF/Epoxy composite frangible cover eventually failed in accordance with the predetermined pattern. The simulation error of the failure pressure of the short‐cut BF/Epoxy composite frangible cover was less than 20%.

Optimizing Skin Surface Metabolomics: A Comprehensive Evaluation of Sampling Methods, Extraction Solvents, and Analytical Techniques

Characterizing the metabolite fingerprint from the skin surface provides invaluable insights into skin biology and microbe-host interactions. To ensure data accuracy and reproducibility, it is essential to develop standard operating procedures for skin surface metabolomics. However, there is a notable lack of studies in this area. In this study, we thoroughly evaluated different sampling materials, extraction solvents, taping methods (frequency and number of tapes), and analytical techniques to optimize skin surface metabolomics. Our results showed that the combination of D-Squame D100 tape with a methyl tert-butyl ether/methanol extractant is optimal for skin surface lipidomics. Performing the skin-taping procedure 5 times with 1 tape yields sufficient biomass for lipid analysis, whereas the optimal taping procedure varies for water-soluble compounds. In addition, our study identified associations among the skin surface metabolites, some of which potentially underlie the formation of microbial cutotypes and offer insights into host-microbe interactions.

Accelerating whole-sample polarization-resolved second harmonic generation imaging in mammary gland tissue via generative adversarial networks.

Polarization second harmonic generation (P-SHG) imaging is a powerful technique for studying the structure and properties of biological and material samples. However, conventional whole-sample P-SHG imaging is time consuming and requires expensive equipment. This paper introduces a novel approach that significantly improves imaging resolution under conditions of reduced imaging time and resolution, utilizing enhanced super-resolution generative adversarial networks (ESRGAN) to upscale low-resolution images. We demonstrate that this innovative approach maintains high image quality and analytical accuracy, while reducing the imaging time by more than 95%. We also discuss the benefits of the proposed method for reducing laser-induced photodamage, lowering the cost of optical components, and increasing the accessibility and applicability of P-SHG imaging in various fields. Our work significantly advances whole-sample mammary gland P-SHG imaging and opens new possibilities for scientific discovery and innovation.

Influence on the properties of TMCs of ceramic and intermetallic composite reinforcements (B4C, TixAly and TixSiy) fabricated by inductive hot pressing

Ambitious and competitive, the aerospace industry continuously demonstrates to be one of the leading engineering sectors either at exigence and new technologies development. As lightning the weight of aircrafts is one of the main targets, the spotlight is usually on material research by which new ones may be produced to pursue this aim and still offer the necessary performances. The combination of the properties of titanium and other materials as reinforcements provides really interesting results as titanium matrix composite materials, also known as TMCs. Various samples of titanium matrix composite materials with different reinforcements have been under study to determine the influence of the reinforcements and their respective proportions on the properties of the material. These samples composed of grade 1 commercially-pure titanium as matrix and B4C, TixAly and TixSiy as reinforcements, have been manufactured through powder metallurgy in the same conditions of temperature and pressure via Inductive Hot Pressing (IHP). A total of eight composite materials have been arranged in several different groups to confront their compositions. Thus, this analysis reports results for the influence of the powder size of the matrix and the ceramic reinforcement, the effect of varying the volumetric composition of B4C, and the selection of different intermetallic reinforcements. These tests and the obtained information serve for a project in which the main goal is to determine which compositions of the studied composite materials reach a high enough specific stiffness for a suitable application in the aerospace industry.

Microalgal Diversity and Molecular Ecology: A Comparative Study of Classical and Metagenomic Approaches in Ponds of the Eifel National Park, Germany

While molecular methods have begun to transform ecology, most algal biodiversity is still studied using the classical approach of identifying microalgae by light microscopy directly in sample material or using cultures. In this study, we compare both approaches (light microscopy and metagenomics as a molecular approach) using the freshwater ponds of the Eifel National Park in Germany as a case study. The ponds were found to be rich in desmids by light microscopy. A total of 299 species representing 81 genera were identified by light microscopy. While the molecular method does not currently allow species identification in most cases, we were able to identify 207 different algal genera. In total, 157 genera were detected only by metagenomics, 50 genera were found with both methods, and 31 genera were found by light microscopy, highlighting the need to continue using light microscopy in addition to a molecular approach. The metagenomics method has several advantages over the light microscopy method: (1) deeper assessment of alpha biodiversity, (2) better abundance numbers, and (3) complete coverage of all living matter. The latter is also a significant improvement over metabarcoding, as universal PCR primers are not available.

THE CONCENTRATION OF NATURAL RADIATION SOURCES (NRS), MAINLY 238U, 232Th, and 40K, IN BUILDING MATERIALS (SAND, CLAY BRICKS, AND CONCRETE BLOCKS) USED ALONG KANGUNDO ROAD, NAIROBI KENYA

This research aimed at assessing the concentration of Natural Radiation Sources (NRS), mainly 238U, 232Th, and 40K, in building materials (sand, clay bricks, and concrete blocks) used along Kangundo Road in Nairobi City County. Human exposure to ionising radiation is largely due to Natural Radiation Sources (NRS). These radioactive elements with long half-lives are found in the Earths lithosphere and in construction materials with radiation levels varying due to their geology. A purposive random sampling method was deployed in this work to collect samples of building materials for analysis. The radioactivity concentration levels in the sampled building materials were determined using a NaI (TI) spectrometer at Kenyatta University laboratory. The activity concentration of 40K varied from 151 ± 8 to 2392 ± 120 Bq/kg, 238U varied from 27 ± 2 to 412 ± 21 Bq/kg and 232Th ranged from 54 ± 3 to 612 ± 31Bq/kg. More than 70 per cent of the samples analysed had activity concentration surpassing the world permissible limits of 420 Bq/kg, 33 Bq/kg, 45 Bq/kg for 40K, 238U and 232Th respectively. The study therefore recommended that assessment of radioactivity concentration for samples with high radioactivity values.

Analytical methodological adaptations for sampling ancient pigments in provenance research

Mineral pigment provenance is a promising direction in cultural heritage particularly in ancient polychromy research. The analysis of trace elements and Pb-isotopes can provide clues about the origin of pigment raw materials. While previous investigations already showed great potential for provenancing archeological-historical mineral pigments, sampling methods and reference data collections need to be developed further to evaluate the potential and limitations of this type of research. This work tests a new sampling method for pigment provenance research that collects sample material with easily available (suffused) cotton swabs for analysis by mass spectrometry. Three artifacts decorated with Egyptian blue and red pigments were selected for comparing sampling with cotton swabs to sampling with a scalpel. All three artifacts date to the 1st century BCE: The first is a colossal marble head from Lazio, Italy, which probably belonged to a seated cult statue of Zeus, and with extensive remains of ancient red paint. The two artifacts (a slag and a fragment of a terracotta vessel) were recovered during Petrie's excavations of an Egyptian blue production facility in Memphis, Egypt. The new results are consistent with previous studies, which provides the necessary quality control for the cotton swab sampling method. This work contributes to improving sampling methods for pigment provenance analysis as well as to a better understanding of past pigment production and trade networks.

Materials characterization for Refuse Derived Fuel (RDF) production as renewable energy resources

This study offers a comprehensive analysis of key parameters—volatile matter, carbon content, ash content, and gross energy—across various material samples intended for Refused Derived Fuel (RDF) briquette production. Through meticulous examination, promising trends emerge, highlighting optimal material combinations for efficient combustion and heat generation. Samples rich in volatile matter and carbon content, notably those incorporating wood powder, demonstrate elevated calorific values, indicating their potential for effective energy production. Conversely, material combinations with low ash content suggest cleaner combustion and reduced environmental impact. The gross energy analysis further validates the substantial heat generation potential of specific sample combinations, rendering them suitable for diverse heating applications. These findings emphasize the critical role of precise raw material selection and meticulous manufacturing process optimization in producing RDF briquettes with desirable properties. Such briquettes not only offer economic viability but also contribute to environmental sustainability by providing an alternative fuel source with reduced emissions. This research underscores the importance of continued exploration and refinement in the development of RDF briquettes, aiming to meet growing energy demands while mitigating environmental concerns.

Machine-learning-based sampling inspection under OQC capacity for real-time quality monitoring in the TFT-LCD industry

ABSTRACT In the thin film transistor-liquid crystal display (TFT-LCD) industry, the competition is fierce, and the external failure cost is high. To improve the quality of released products, sampling inspection under outgoing quality control (OQC) is conducted before products are released. Owing to the variety and complexity of inspection items, the task must be carried out manually while realising automation is difficult. Traditional random sampling inspection is limited by sampling quantity, manpower, and material resources. To effectively improve acceptable quality levels, this paper proposes a quality predictive monitoring framework tailored to the production and inspection characteristics of the TFT-LCD industry. This framework includes real-time automatic quality monitoring based on an optimal machine learning prediction model with two-phase feature creation, and it also addresses OQC inspection capacity constraints. Experimental results show the prediction performance based on proposed model is better than the traditional random sampling process. In practice, superior average outgoing quality improves by more than 70% at the same sampling level. In addition, the features of the process can be further controlled and managed based on the prediction model to monitor the key parameters in real time and respond to abnormalities quickly, thereby further improving the quality of released products.

Fixative or Finish? Identifying the Surface Coating on John Constable’s Drawings Using Peptide Mass Fingerprinting

ABSTRACT A survey of graphite drawings by the English painter John Constable revealed that in many cases the artist applied a coating overtop of the media. This thin, clear, glossy coating was characterized on over thirty drawings where it appeared to be the same material although employed in different ways. Several attempts were made to identify the material with minimal success until peptide mass fingerprinting (PMF) was used, and a minimally invasive sampling method involving vinyl eraser cubes proved to be a very easy and effective technique to collect sufficient sample material for the analysis. The results of testing samples from seven drawings conclusively identified the coating as isinglass, which Constable was using in other preparations of support materials for painting. As part of this work, putative markers for the identification of isinglass by PMF were developed.