Non-destructive Analytical Method Research Articles

Effect of Luting Materials on the Accuracy of Fit of Zirconia Copings: A Non-Destructive Digital Analysis Method.

The marginal accuracy of fit between prosthetic restorations and abutment teeth represents an essential aspect with regard to long-term clinical success. Since the final gap is also influenced by the luting techniques and materials applied, this study analyzed the accuracy of the fit of single-tooth zirconia copings before and after cementation using different luting materials. Forty plaster dies with a corresponding zirconia coping were manufactured based on a single tooth chamfer preparation. The copings were luted on the plaster dies (n = 10 per luting material) with a zinc phosphate (A), glass-ionomer (B), self-adhesive resin (C), or resin-modified glass-ionomer cement (D). The accuracy of fit for each coping was assessed using a non-destructive digital method. Intragroup statistical analysis was conducted using Wilcoxon signed rank tests and intergroup analysis by Kruskal-Wallis and Mann-Whitney U tests (α = 0.05). Accuracy of fit was significantly different before/after cementation within A (0.033/0.110 µm) and B (0.035/0.118 µm; p = 0.002). A had a significantly increased marginal gap compared to C and D, and B compared to C and D (p ≤ 0.001). Significantly increased vertical discrepancies between A and B versus C and D (p < 0.001) were assessed. Of the materials under investigation, the zinc phosphate cement led to increased vertical marginal discrepancies, whereas the self-adhesive resin cement did not influence the restoration fit.

Using MA-rFTIR Mapping as a Tool to Assess the Efficacy of Cleaning Treatments and to Aid in the Restoration Activities of Paintings

The removal of non-original superimposed layers covering the original pictorial layer in paintings is a common practice to restore the authentic appearance of surfaces and mitigate potential risks to artwork preservation. Contemporary assessments of the effectiveness of such cleaning treatments often employ non-destructive analytical methods. However, many existing techniques face limitations, either lacking specificity in compound identification or analyzing very limited areas (&lt;millimeters) through a point-by-point approach. This study introduces the application of a macro Fourier transform infrared scanner, in reflection mode (MA-rFTIR), as an effective tool for supporting restorers during cleaning processes. This method proved successful in addressing challenges related to the removal of calcium oxalate films and non-original superimposed layers on two ancient paintings.

Nondestructive Single-Atom-Thick Crystallographic Scanner via Sticky-Note-Like van der Waals Assembling-Disassembling.

Crystallographic characteristics, including grain boundaries and crystallographic orientation of each grain, are crucial in defining the properties of two-dimensional materials (2DMs). To date, local microstructure analysis of 2DMs, which requires destructive and complex processes, is primarily used to identify unknown 2DM specimens, hindering the subsequent use of characterized samples. Here, a nondestructive large-area 2D crystallographic analytical method through sticky-note-like van der Waals (vdW) assembling-disassembling is presented. By the vdW assembling of veiled polycrystalline graphene (PCG) with a single-atom-thick single-crystalline graphene filter (SCG-filter), detailed crystallographic information of each grain in PCGs is visualized through a 2D Raman signal scan, which relies on the interlayer twist angle. The scanned PCGs are seamlessly separated from the SCG-filter using vdW disassembling, preserving their original condition. The remaining SCG-filter is then reused for additional crystallographic scans of other PCGs. It is believed that the methods can pave the way for advances in the crystallographic analysis of single-atom-thick materials, offering huge implications for the applications of 2DMs.

Non-destructive method of blood serum composition analysis in forensic science

The article is devoted to consideration of non-destructive methods of blood serum composition analysis in forensics, problem solving and their improvement. At the current stage of creating materials and devices of a new generation, the task is not only to manage their properties, but also to effectively use them in various fields, in particular, in forensics. Analysis of the structural evolution of a heteroatomic liquid (in particular, blood) from the standpoint of theoretical and experimental approaches allows us to open new horizons in the practical plane, to determine the phenomenology of the process based on modern research methods. The authors of this work conducted a qualitative and quantitative analysis of experimental data related to the kinetics and mechanisms of structure formation of a multicomponent substance in the liquid state. It should be emphasized that the structural kinetics of a liquid such as blood serum, or blood itself, is a complex multistage process.

Nondestructive Quantification of Isoflavones in Cotyledons by Near-Infrared Spectroscopy and Potential and Limits for Sustainable Soybean Breeding

The isoflavones in the cotyledon of soybean seeds mimic human estrogen in structure, conferring them complex effects on health. Their regulation represents a major challenge for the sustainable breeding of new varieties with lower levels of potential endocrine disruptors. To develop a rapid, nondestructive, and eco-friendly analysis method, this study explores how sample grinding affects the results of near-infrared spectroscopy (NIRS) and the preprocessing methods. The prediction of the daidzein and genistein content would help the specific reduction in isoflavones in the cotyledon without harming seed development. The potential of a nonlinear approach (artificial neural network) is also compared with the more conventional partial least squares (PLS) regression. The isoflavone content of cotyledons from 529 soybean samples (65 genotypes) was quantified by HPLC, and the NIR spectra of these samples were collected using a Brucker multi-purpose analyzer. The spectra of whole and ground cotyledons were also collected for 155 samples. The results show that grain fragmentation improves the model calibration, although spectral preprocessing can harmonize this effect. Although the best PLS regression in cross-validation did not suffice to quantify the daidzein and genistein percentages, the artificial neural network (ANN) approach allowed us to develop much more reliable models than PLS. The performance of ANNs in external validation is remarkable in terms of both precision and applicability (R2 = 0.89 and a ratio of prediction to deviation of 2.92), making ANNs suitable in the breeding context for screening soybean grains regarding their isoflavone content.

Vegan and sugar-substituted chocolates: assessing physicochemical characteristics by NMR relaxometry, rheology, and DSC

The main physicochemical characteristics of novel artisanal chocolates (both dark and milky) intended for vegan consumers or for those requiring assumption of fewer simple sugars, were analysed. Replacement of milk (with coconut copra, almonds, and soy protein isolates), and sucrose (with coconut sugars, stevia and erythritol, respectively) in dark chocolate, were accounted for by means of texture analysis, rheology, water activity, fatty acid composition, differential scanning calorimetry (DSC) and fast field cycling (FFC) nuclear magnetic resonance (NMR) relaxometry. The vegan sample (i.e., the milk-less one) showed lower values of hardness and adhesiveness as well as a larger peak in the melting behavior at the calorimetric evaluation (DSC). Moreover, the absence of milk resulted in the halving of the yield stress and a decrease in both the apparent and Casson’s viscosity. In the sample of chocolate with less sucrose, the peak temperatures measured at the DSC indicate crystallization of cocoa butter in its best form (Vβ2), unlike in dark chocolate, due to the different sugar composition. Similarly, the Casson yield stress (τ0), increased significantly (almost 70%), with the substitution of sugar. Finally, the results of NMR FFC relaxometry made it possible to identify aggregates of different sizes, laying the basis for its use as a rapid, non-destructive method for chocolate analysis.

Probing hydrogen content in steel using the thermoelectric effect

The issue of hydrogenation of steel is a serious technological problem. Due to its small atomic radius, hydrogen is difficult to analyze quantitatively and qualitatively. Non-destructive estimation of hydrogen content would significantly improve the quality control process. In this work, we attempt to develop a new methodology for the determination of hydrogen content in 4340 steel using the thermoelectric effect. For this purpose, we investigated the mechanisms of hydrogenation, structural and microstructural changes caused by hydrogenation, and performed theoretical calculations of the influence of hydrogen on the electronic structure of steel. Measurements of the Seebeck coefficient were performed using the specially developed μm-resolution scanning thermoelectric microscope (SThM). The KKR-CPA calculations show that hydrogen located at T-voids strongly modifies electronic properties and influences the Seebeck coefficient of the material. Ultraviolet photoelectron spectroscopy (UPS) proves that hydrogenated samples exhibit the valence band onset shift towards higher binding energies concerning the non-hydrogenated materials. Theoretical and experimental studies of the Seebeck coefficient dependence on the total hydrogen content confirm a measurable decrease in the Seebeck coefficient (18.5 µV/K for 0.136 ppm and 13.5 µV/K for 1.03 ppm). Plotted calibration curves for 4340 steel were used for preliminary kinetic studies of the spontaneous dehydrogenation in this material. This work demonstrates that the thermoelectric effect can be used as the basis of a new fast and non-destructive analytical method for the determination of the hydrogen content in 4340 steel.

Concentration‐number (C‐N) fractal models reveal the distribution pattern of the elements in ancient nephrite measured by portable X‐ray fluorescence: Based on nephrite objects excavated from different sites in Nanyang, Henan Province

AbstractChanges in the composition of various chemical elements in ancient nephrite artifacts due to prolonged burial are critical factors that should not be underestimated. However, the increasingly stringent heritage management has made many techniques impractical. Consequently, portable X‐ray fluorescence (pXRF) has become an indispensable nondestructive field analysis method. This paper aims to make use of the pXRF dataset to distinguish which elements tested are endogenous or exogenous, as well as to gauge which elements have been affected by stronger burial effects. More specifically, we carry out this work on the example of 103 pieces of nephrite excavated from different cemeteries in the Nanyang area. In addition to traditional statistical techniques, a new tool, the concentration‐number (C‐N) fractal method can shed new light on the analysis of the distribution patterns of different elements in excavated nephrite. The anomalous boundaries generated by the method have clear geochemical significance and can be delineated between background zone and disturbed regions. The degree of resistance of different elements to fluctuations in external factors was assessed, which has a direct relationship with the content of the buried soil. Considering the richness of the model, it has the potential to be used in archaeometrics.

Quantification of bulk elemental composition for C‐type asteroid Ryugu samples with nondestructive elemental analysis using muon beam

AbstractSamples from asteroid Ryugu, brought back by asteroid explorer Hayabusa2, are important for investigating the origin and evolution of the solar system. Here, we report the elemental compositions of a 123‐mg Ryugu sample determined with a nondestructive muon elemental analysis method. This method is a powerful tool for determining bulk chemical composition, including light elements such as C, N, and O. From the muonic x‐ray spectra with three carbonaceous chondrites, the relationship between the elemental composition and muonic x‐ray intensity was determined for each element. Calibration curves showed linearity, and the elemental composition of Ryugu was quantitatively determined. The results reflect the average bulk elemental composition of asteroid Ryugu owing to the large amount of samples. Ryugu has an elemental composition similar to that of Orgueil (CI1) and should be classified as CI1. However, the O/Si ratio of Ryugu is 25% lower than that of Orgueil, indicating that Orgueil may have been seriously contaminated by terrestrial materials after its fall to Earth. These results indicate that the Ryugu sample is more representative than the CI chondrites as a solid material of the solar system.

Local strain distribution analysis in strained SiGe spintronics devices

This paper reports nanobeam X-ray diffraction (nanoXRD) measurement results for strained SiGe spintronics devices grown by MBE. A quantitative nanoXRD analysis verifies that in-plane strain is properly exerted on the SiGe spin channel layer in the device showing enhanced spin diffusion length, whereas overall strain relaxation and local change in crystallinity occur in the sample with unclear spin signals. Crystal defects such as dislocations and stacking faults found in cross-sectional transmission electron microscopy observations are correlated with the results of nanoXRD analysis and their influence on spin transport properties are discussed. The present results demonstrate the capability of the nanoXRD based method for quantitative nondestructive analysis of strain distribution and crystallinity in real device structures.

Application of non-destructive analysis methods in TENMAK-PAF

Development of non-destructive analysis systems at the R&D beamline of the Proton Accelerator Facility of the Turkish Energy, Nuclear and Minerals Research Agency (TENMAK-PAF) is described in this work. The proton beam from the cyclotron with energy between 15–30 MeV and current between 0.1 μA–1.2 mA is modified with several components and subsystems to be suitable for the application of non-destructive analysis methods. Certified reference materials (CRM) and samples with different properties were irradiated under vacuum in the irradiation chamber with the new system. Particle Induced X-ray Emission (PIXE) and Particle Induced Gamma ray Emission (PIGE) spectra of these samples were obtained with appropriate radiation detectors and measurement systems. The results of PIXE analyses and X-ray fluorescence (XRF) spectrometry were compared. PIXE and PIGE results are in good agreement with the certified values for the CRMs. This work constitutes the first reported application of non-destructive ion beam analysis methods in TENMAK-PAF and in Türkiye.

Analytical method for stable background reduction for Raman spectra of carbon‐containing meteorite and terrestrial samples suffering from intense fluorescence

AbstractChemical states of carbon in terrestrial (meta) sediments and carbonaceous chondrites gather attention as a geothermometer. As a nondestructive analytical method, Raman spectroscopy has been widely used to study their electronic properties, crystallinity, and structural defects through so‐called D and G bands. For the analysis of Raman spectra, a common problem is coexistence of a fluorescence background, which should be subtracted prior to the peak‐fitting analysis. However, we recently faced a problem that the band shape noticeably changed depending on the background function assumed although the background seemed to be well subtracted at a first glance regardless of the choice of the background function. For the application of the Raman spectroscopy as a geothermometer, a standard background subtraction method must be established to suppress the arbitrariness. In the present study, Raman spectra of seven carbon‐containing natural samples, whose background intensities were significantly different, were measured, and their background shape was evaluated by first‐, second‐, and third‐order polynomials. The results indicated that the third‐order polynomial was necessary and sufficient as a standard background function. Importantly, although lower order polynomials seem to successfully fit the background at a first glance, they falsely caused dispersion of the shoulder band shape.

A Green Raman Spectroscopic Assay Method for The Quantification of Tranexamic Acid in Pharmaceutical Formulations

Tranexamic acid (TXA) is a widely used antifibrinolytic agent that is used to prevent and treat excessive bleeding. Current analytical methods for TXA are often time-consuming and require the use of toxic solvents. Raman spectroscopy has the ability to measure TXA because it is a fast and non-destructive analytical method. This research established and validated a green Raman spectroscopic test for TXA measurement. There was no need for harmful solvents because the technique relied on a basic aqueous solution of TXA. Results demonstrated that the technique was linear across the 0.7% to 13.0% concentration range. The method was also shown to be accurate, with results comparable to the orthogonal techniques. The green Raman spectroscopic assay method was applied to the quantification of TXA in pharmaceutical formulations. The results obtained were comparable to those obtained using reference methods. To quantify TXA quickly and accurately, one can use the green Raman spectroscopic test. Since no harmful chemicals are needed for the procedure, it is also eco-friendly. Method has the potential to be used in a variety of settings, including pharmaceutical quality control and research laboratories.

Poor Cycling Performance of Rechargeable Lithium–Oxygen Batteries Under Lean-Electrolyte and High-Areal-Capacity Conditions: Role of Carbon Electrode Decomposition

There has been considerable interest in developing rechargeable lithium oxygen batteries (LOBs) that have the potential to significantly exceed the energy density limit of a Li ion battery (approximately 300 Wh/kg). Although 500 Wh/kg LOB has been demonstrated and exhibited stable discharge/charge cycle at room temperature condition1, their cyclability remains less than 10 cycle. For realizing the LOB with practically high energy density and long cycle life, the deep understanding of complicated reaction in LOBs has been highly demanded. Especially, the problems specifically associated with the limited electrolyte (“lean-electrolyte”) conditions need to be taken into account in LOBs.Although the importance of investigating negative lithium electrodes in lean-electrolyte systems has been recognised in recent years2,3, specific problems associated with the negative lithium electrode in a LOB has not been investigated so far. In particular, chemical crossover from the positive electrode to the negative electrode is a crucial factor that needs to be taken into consideration. Actually, recent studies have shown that LiOH is formed on the surface of a lithium-metal electrode through reaction with H2O in the electrolyte4,5. This H2O is generated by the decomposition of the tetraethylene glycol dimethyl ether (TEGDME) solvent at the positive oxygen electrode, which then migrates to the negative electrode side to react with the lithium-metal electrode. Consequently, problems related to chemical crossover are prominent in lean-electrolyte LOBs, where the effective water concentration in the electrolyte is much higher than that in an excess electrolyte system.Despite the importance of investigating the reaction of negative lithium electrodes in LOB with appropriate technological parameters, mechanistic details remains unclear due to the technical difficulty for applying non-destructive analytical methods. In the present study, we investigated the reaction of a negative lithium electrode in a lean-electrolyte LOB operating under high areal capacity conditions. The use of advanced non-destructive analytical methods, including three-electrode electrochemical techniques and an in-situ analytical setup revealed that the reaction efficiency of the lithium electrode mostly decreases through chemical crossover from the positive oxygen electrode6. In particular, the H2O generated as a side-product at the positive oxygen electrode crosses over to the negative electrode side and reacts with the lithium-metal electrode to form a porous LiOH/Li2CO3 layer on the electrode surface. LiOH and Li2CO3 accumulates, and the porous layer thickens through repeated discharge/charge cycling, which supresses efficient Li-ion transport through the layer.Furthermore, using a solid-state ceramic-based separator to protect the lithium-metal negative electrode, the side reaction with the negative electrode was considerably suppressed, which helped exclusively assess the degradation phenomena occurring in the oxygen positive electrode. By series of in-situ and ex-situ analysis revealed the following points: (i) Although the electrolyte degradation intensified with increasing repeated discharge/charge cycling, the scarcity of the electrolyte minimally influenced the cycle life of the LOBs. (ii) Most of the Li2CO3-like solid-state side products decomposed during charging at voltages higher than 3.8 V. (iii) Severe decomposition of the carbon electrode occurred during cycling, and an equivalent amount of CO2 was generated during charging at voltages higher than 3.8 V. Because the carbon electrode used in these experiments merely decomposed via simple electrochemical oxidation at voltages up to 4.5 V, the carbon electrode was considered to deteriorate through the decomposition of its solid-state side products. The findings of this study are anticipated to guide future investigations on the advancement of LOBs. In particular, detailed understanding of the reaction at the interface between the carbon electrode and solid-state products is crucial for realizing practical high-energy-density LOBs with long cycle life.

Confocal micro-X-ray fluorescence analysis for difference identification of ceramic samples.

A nondestructive analytical method for difference identification is required in the research fields such as forensic science or archeology. An X-ray fluorescence (XRF) analysis is one of feasible techniques for this purpose. Micro-XRF using an X-ray micro-beam gives elemental distributions by scanning the samples. A confocal micro-XRF (CM-XRF) technique is a unique analytical technique to analyze limited volume. CM-XRF enables elemental depth imaging and elemental profiling in depth nondestructively. Therefore, CM-XRF has been applied for various samples such as industrial samples, paintings, forensic samples, food materials, and human hairs. CM-XRF technique would be a suitable method for difference identification because the CM-XRF gives detailed information on elemental distribution not only on the surface of the sample but also in depth. We developed CM-XRF instrument in the laboratory and applied to two very similar ceramics samples. It showed differences in the intensity profiles of Fe and Mn for blue paintings on the ceramics. In addition, depth elemental analysis revealed different depth profiles especially of Co and Zn for both samples. These results suggest that CM-XRF provides useful information for the identification of ceramic samples.

An irradiation system for nuclear and materials research in a medical cyclotron

Development and commissioning of an irradiation system and experimental setup for nuclear research and materials analysis in a medical cyclotron facility is described. The setup, Low Energy in-Vacuum Irradiation System-LEVIS, is installed at the end of the existing R&D beamline. The components of LEVIS and their functions are explained and the characteristics such as energy, current and profile of the beam are measured. Different types of radiation detectors are installed and tested in the chamber for future applications of non-destructive analysis methods.

Evaluating Non-destructive Analysis and Sampling Methods for Identifying Plant and Animal Imprints in Late Pre-contact Wattle and Daub Rubble from the Yazoo Basin, Mississippi

ABSTRACT Past analyses of burned wattle and daub rubble from Native American house excavations have shown that plant and animal-related imprints sometimes occur in daub fragments. This paper evaluates the use of non-destructive analysis and sampling methods from a region-wide assemblage of burned daub recovered from a group of Pre-Contact Mississippian Period village and settlement sites in the Yazoo Basin of northwestern Mississippi, U.S.A. The quality and occurrence of imprints from this assemblage will be assessed, and how they may be considered in both future paleoenvironmental research and curation practices.

Application of X-ray computed tomography in soil and plant -a review

X-ray computed tomography (X-ray CT) is a non-destructive method of soil analysis which can provide three-dimensional (3D) view, quantitative information of the internal organization of the soil. In this paper, we discuss the potential application of X-ray CT in characterization of soil properties like porosity and pore size distribution (PSD), root architecture, soil phase classification, water and solute transport in soil, and highlight the research during last 10–15 years. Here, we review the recent development of X-ray CT in soil science, use of artificial intelligence and machine learning in image analysis, point out the major challenges associated with its use, discuss few improvements to overcome these difficulties and elaborate the possible future technological developments for non-invasive/destructive soil characterization by integrating X-ray CT with recently available complementary techniques.

Nondestructive volumetric optical analysis of corroded copper oxidation using 1700nm swept-source optical coherence microscopy.

This study presents a novel nondestructive analysis method for precise characterization of corroded copper oxidation using optical coherence microscopy (OCM). By exploiting the partial light transmission through metallic oxide layers, we employed a specialized OCM system with a wavelength of 1700nm and enhanced the analysis accuracy compared to conventional optical coherence tomography (OCT). The developed OCM system featured a numerical aperture (NA) of 0.15, providing improved surface profiling and higher lateral resolution than OCT. we developed a peak-finding algorithm to accurately determine the thickness of the copper oxide layer from the acquired interference data with zero padding. Our method was validated by comparing the measured thickness profiles with those obtained from scanning electron microscope (SEM) images of corroded metals. The copper oxidation specimens were prepared after heat treatment for 1, 2, 4, and 8 h in an alumina tube furnace at a temperature of 900 °C to find the correlation between the OCM thickness measurement. Additionally, the acquired enface 3D images enabled the identification of local corrosion distribution within a 4 mm × 4 mm area. The en-face mapping images are utilized to analyze the uniformity of the metal oxidation process across the imaging area of the copper oxidation specimens. With an increase in heat treatment time, the median value of the thickness histogram for the copper oxide within the area consistently remained around 10 µm. However, the thickness variation ranged from -2 µm to 5 µm. This indicates that as the heat treatment time progresses, the thickness of the copper oxide becomes more non-uniform. Our technique holds great potential for nondestructive and noncontact detection of metal corrosion and assessment of corrosion rates in various industrial applications. Future research efforts could focus on expanding the application of OCM to different metals and exploring its commercialization prospects for practical implementation in diverse industries.

Non-Destructive Discrimination of Blue Inks on Suspected Documents through the Combination of Raman Spectroscopy and Chemometric Analysis

Increasingly sophisticated techniques for falsifying and forging legal documents demand non-destructive and accurate analysis methods. Researchers have extensively investigated ink discrimination through an interdisciplinary analysis involving Raman spectroscopy and chemometrics, which is now regarded as a leading forensic document analysis approach. In this study, a groundbreaking method was developed to identify the specific origin of blue-ink pens used in written documents. By employing Raman spectroscopy in conjunction with principal component analysis (PCA), we successfully differentiated between 45 different blue-ink pens used on various documents. The Raman spectroscopy analysis provided a visual examination of each blue ink’s unique Raman signature, and PCA was then applied to the processed spectral data. Moreover, we successfully distinguished highly similar ink types in documents through the combined use of Raman spectroscopy, Pearson’s correlation analysis, and a statistical approach (PCA).