Wavelength Dispersive X-ray Fluorescence Research Articles

Unified method for the determination of chemical composition in different types of materials using Wavelength Dispersive X-ray Fluorescence Spectrometry

Abstract The aim of the article is to show that determination of the main chemical composition with Wavelength Dispersive X-ray Fluorescence Spectrometry method does not require the use of separate analytical applications and procedures for the tests of materials of different origin. This is however conditioned upon calcination of the tested initial sample at the temperature of 815 °C to remove organic matter and its preparation for X-ray measurements by fusing into a borate bead. Within the framework of the conducted research a special analytical application measuring 10 oxides: SiO2, Al2O3, Fe2O3, CaO, MgO, Na2O, K2O, SO3, TiO2 and P2O5 was developed. Standards and certified reference materials (CRMs) were applied for calibration. Synthetic standards with the use of oxides and salts of purity of 99.99% were also prepared to complete the measuring points on the calibration curves The curves determined based on the measuring points have high correlation coefficients and accuracy. The α empirical correction coefficients were applied to correct matrix effects. The range of the method was confirmed based on the measurements of 13 synthetic standards. The average values of the standard deviations in the lower range of the calibration curves were between 0.0008% for K2O and 0.0056% for Na2O and 0.0054% for MgO. The average values of the relative standard deviation were in the range between 1.81% for K2O and 13.92% for MgO and 11.21% for Na2O, respectively. In the upper range of the calibration curves, the average values of standard deviation were between 0.079% for TiO2 and 0.962% for P2O5, and the relative standard deviation was between 0.05% for SiO2 and 2.39% for P2O5. The accuracy of the developed WDXRF method was assessed based on the measurement of 10 certified reference materials representing all the tested materials (cement, coal ash, slag, fire clay, sediment and soil). Out of 98 conducted measurements (two CRMs did not contain the declared content of P2O5 and SO3 respectively), in 68 measurements, relative errors were below 5%, and, in next 27 measurements, they were between 5% and 10%. The errors were comparable for all the tested materials which confirms that in WDXRF analyses of borax beads the type, kind and origin of a sample do not affect accuracy of the obtained measurements.

Ionosilica-based anion exchangers for low-temperature thermochemical storage of energy under mild conditions of adsorbent regeneration and saturation

Three ionosilica materials have been tested for low-temperature thermochemical storage of energy under mild conditions of adsorbent regeneration and saturation. The previous synthesis procedures were adapted to prepare materials possessing an organosilica framework with silylated cationic blocs and Cl-, HSO4-, SO42- anions in various proportions as extra-framework compensating counter-ions. Transmission and Scanning Electron Microscopy, Wavelength Dispersive X-Ray Fluorescence, Energy Dispersive X-ray Spectroscopy, Thermogravimetric analysis, adsorption of gaseous nitrogen at 77 K, 29Si Solid-State Nuclear Magnetic Resonance spectroscopy were employed to establish the key characteristics of the three ionosilica samples in terms of elemental composition, particle morphology and textural properties, thermal stability and regenerability, or variability of surface activity during repeated hydration-dehydration cycles. Their capacity to adsorb water vapor at cool and moderate ambient temperatures after incomplete surface drying was demonstrated by means of the scanning microscopy operating in low-vacuum mode at 275 K, or more precisely by measuring the water adsorption isotherms at 313 K and the related differential heats under static conditions. Finally, flow calorimetry operating in the moist-gas flow mode was used to measure the integral heat accompanying the adsorption of water vapor at its partial pressure of 2.8 kPa and 296 K as well as the kinetics of heat release in three drying-saturation cycles. After a drying procedure carried out under helium flow at 353 K, the thermal performance of two ionosilica samples containing both HSO4- and SO42- counter-ions was sufficient enough to consider them as potential adsorbents for auxiliary space heating in homes, small businesses, or public buildings.

Characterization of a Jian‐like sherd with the optical microscope, confocal Raman, wavelength‐dispersive X‐ray fluorescence, and portable XRF spectrometers

AbstractThe ceramic masterpieces that belong to the private collections and art galleries are rarely studied with analytical instruments to define the authenticity, provenance, and characteristics of the materials because the scientific investigations are required to be solely noninvasive for characterizing the unfractured genuine objects. A monographic program, Blue Print, which was initiated by a German cultural heritage foundation, Art & Science Endowment Trust (ASET) Stiftung, aims at developing on‐site research protocols for systematic research investigations on the fragmentary samples, with and without verifiable archeological contexts. For that reason, a combination of analytical techniques was carried out on a Jian‐like sherd, which was assumed to be produced either as a genuine artifact between the 11th and late 14th centuries ad or as a Qing Dynasty copy (1644–1911 ad). Before slicing the sherd, confocal Raman microscopy was used to define the red glaze signature and the crystals formed on the glazed surface, whereas portable X‐ray fluorescence (XRF) (pXRF) was used to define the composition of the glaze and body. Afterward, the sherd was cut and polished for the characterization with a zoom microscope, wavelength‐dispersive XRF (WD‐XRF), and Raman. The macroscopic examination revealed the presence of a glassy black colored interface layer, which was detected between the body and red glaze. The composition of the red glaze was determined with XRF and Raman spectrometers, and the presence of cadmium sulfoselenide (CdSxSe1−x, 0 ≤ x ≤ 1) with a high amount of zirconium (WD‐XRF: 2.20 wt.%, pXRF: 1.55‐wt.% ZrO2) was found. Additionally, Raman measurements evidenced the presence of epsilon‐hematite crystals formed on the blackened red glazed surface. Unlike the glaze composition, the elemental content of the body is almost the same (Al2O3: 25.7 wt.%, Fe2O3: 8.19 wt.%, K2O: 2.54 wt.%) with the genuine Jian wares already documented by artistic and scientific examinations.

Daytime concentrations of minor and trace elements in atmospheric aerosols at four sampling sites of Dar es Salaam, Tanzania

Tropospheric aerosols (total suspended particulate, TSP) were sampled at four sampling sites of various anthropogenic impact (industrial, commercial, heavy trafficked, and mixed urban influence), located in Dar es Salaam, the commercial capital of Tanzania. Air concentrations of minor and trace elements (Al, As, Br, Ca, Cd, Cl, Cr, Cu, Fe, K, Mg, Mn, Na, Ni, Pb, S, Si, Sb, and Zn) in TSP were determined by means of wavelength-dispersive X-ray fluorescence (WDXRF) spectrometry and inductively coupled plasma atomic emission spectrometry (ICP-AES). From these data, the main ionic composition of particulate matter was inferred by means of a species correlation/ratio-derived approach, based on former studies of the region. Enrichment factors, bivariate correlations, diagnostic ratios, and chemical mass closures were calculated utilizing the concentration data of TSP constituents for each site in order to reveal the emission sources. A couple of diagnostic ratios (Ni/Cd, Zn/Cd, Br/Ni, Ni/Sb) were useful for source identification, e.g., motor vehicle exhaust and non-exhaust emissions. Significant increases in concentrations of As, Br, Cr, Cu, Mn, Ni, Pb, and Zn were observed, as compared to results for the city before 2010. Moreover, first-time air levels are reported for Cd and Sb, which are important markers of non-exhaust emissions. Air quality indices and calculations with the AIRQ+ model have foreseen increases in the negative health effects of the sensitive groups of the local population at the study areas, especially those with heavy traffic, industrial, and/or mixed urban influence.

An in situ and ex situ study of the microstructural evolution of a novel lithium silicate glass-ceramic during crystallization firing

ObjectiveTo elucidate the compositional and microstructural developments of a novel lithium silicate glass-ceramic during its crystallization cycle. MethodsBlocks of a lithium silicate glass-ceramic (Obsidian®, Glidewell Laboratories) were cut into 1mm thick plates and polished to 1μm finish. Some of them were crystallized prior to polishing. Firstly, ex situ compositional and microstructural characterizations of both the pre- and post-crystallized samples were performed by wavelength dispersive X-ray fluorescence, field-emission scanning electron microscopy, and X-ray diffractometry. Secondly, the pre-crystallized samples were subjected to in situ compositional and microstructural characterizations under non-isothermal heating by simultaneous thermogravimetry/differential scanning calorimetry, X-ray thermo-diffractometry, and field-emission scanning electron thermo-microscopy. ResultsThe microstructure of pre-crystallized Obsidian® consists of an abundant population of perlitic-like/dendritic lithium silicate (Li2SiO3) nanocrystals in a glass matrix. Upon heating, the residual glassy matrix does not crystallize into any form of SiO2; elemental oxides do not precipitate unless over-heated above 820°C; and the Li2SiO3 nanocrystals do not react with the glassy matrix to form typical lithium disilicate (Li2Si2O5) crystals. Nonetheless, the Li2SiO3 nanocrystals grow and spheroidize through the solution-reprecipitation process in the softened glass, and new lithium orthophosphate (Li3PO4) nanocrystals precipitate from the glass matrix. SignificanceThe identification of compositional and microstructural developments of Obsidian® indicates that, by controlling the firing conditions, it is possible to tailor its microstructure, which in turn could affect its mechanical and optical properties, and ultimately its clinical performance.

Proximate composition and element contents of selected species of Ganoderma with reference to dietary intakes.

Ganoderma is a wood-degrading mushroom that is treasured as a functional food since primitive times. Monitoring of macronutrient and element levels in mushrooms collected from the natural environment provides basic information in terms of safety, regulation, and nutrition. A comparative study was developed on the proximate and element contents of Ganoderma applanatum, G. brownii, G. lucidum, and G. philippii collected from different zones of the natural forests in Uttarakhand, India. These mushrooms revealed high amounts of proteins (9.29-12.4%) and carbohydrates (75.5-80.3%) and low contents of fats (1.62-2.87%), but ash (6.14-8.32%) and fibre (4.92-8.07%) were available in significant amounts. Element concentrations were determined by wavelength dispersive X-ray fluorescence (WDXRF) spectrometry. Calcium (5400-19,250mg/kg) and potassium (2602-5601mg/kg) were the predominant elements in mushrooms. The mushroom samples provided significant percentage contribution to reference recommended dietary intakes (RDIs) of essential elements such as calcium (27.0-96.3%), copper (58.2-95.8%), and manganese (37.3-62.3%), for adult males and females; and iron (35.3-97.1% for males and 28.6-78.6% for females), magnesium (7.06-11.5% for males and 7.74-12.6% for females), and zinc (6.35-19.8% for males and 7.65-23.7% for females). The studied mushrooms have no health risks as toxic metals such as aluminium and lead were detected below the legislated respective provisional tolerable intake values. Nutritional quality index (NQI) values revealed that mushrooms are densely rich in calcium, copper, iron, magnesium, manganese, and zinc.

Determination of chemicals released from single use low density polyethylene plastic bags

The use of plastics has increased manifold, owing to their inexpensive, multipurpose, durable and lightweight nature. Plastics are made with various types of polymer, including Low Density Polyethylene (LDPE). In Myanmar, many foods are packaged in single use LDPE plastics including fresh meat, vegetables, fast foods, and even some hot foods in daily life. Therefore the present study was aimed to determine the chemicals released from single use LDPE plastic bags that were used in direct contact with hot foods. Fourier Transform Infra-Red (FTIR) spectroscopy analysis was done for confirmation of LDPE. Extraction of chemicals from single use plastic bags was carried out by reflux extraction method by using four types of solvents (chloroform, ethanol, distilled water and olive oil). The individual chemicals released from the sample were determined by Gas Chromatography-Mass Spectrometry (GC-MS) with National Institute of Standard and Technology (NIST) library. GC-MS results of different extracts were hexadecanoic acid octyl ester (26.09%), octadecanoic acid octyl ester (19.96%), tetracosane (13.36%) and 9-octadecanoic acid methyl ester (9.28%) from distilled water extract;3-methoxy 2,2-dimethyloxirane (84.26%), 2,3-dihydro-1,4-dioxin (3.77%), 1-ethoxy pantane (2.85%) and tetracosane (2.65%) from ethanolic extract; toluene (69.30%), ethyl benzene (18.11%), 1,1-dipropoxypropane (4.02%) and dipropoxy methane (1.56%) from chloroform extract; and supraene (76.81%), nonanal (3.09%), 2-decenal (2.97%), 2-undecenal (3.05%) and toluene (1.35%) from olive oil extract respectively. According to the Wavelength Dispersive X-ray Fluorescence (WDXRF) analysis of single use plastic bag, the different concentrations of elements were found to be titanium (0.0587 %), chlorine (0.0093 %) and strontium (0.0026 %) and so on. The present study revealed that single use LDPE plastic bags contained some chemicals that are toxic to human beings such as toluene, ethyl benzene, methyl oxirane, supraene and some type of aldehyde, and even carcinogenic substance like dioxin. Therefore it is necessary to limit the use of harmful additives and packaging of hot foods in single use LDPE plastic bags.

Determination of trace amounts of uranium in plutonium oxide by wavelength dispersive X-ray fluorescence spectrometry

This paper presents a wavelength dispersive X-ray fluorescence (WDXRF) spectrometry based non-destructive methodology for the determination of trace level uranium in PuO2 powder. The methodology requires pelletization of PuO2 powder standards and samples using a hydraulic press, measuring WDXRF spectra of calibration standards and samples using U Lα X-ray as analytical line and analyzing the samples for trace amounts of uranium. The reproducibility of the analytical results using this methodolgy was found to be better than ± 5% (RSD, n = 5) for uranium in the range of 200–1000 µg g−1. The samples were also analyzed for U by ICP-OES and WDXRF values showed a close agreement with those obtained by ICP-OES.

Determination of sulfur in Soils and Stream Sediments by Wavelength Dispersive X-ray Fluorescence Spectrometry

A simple, rapid and nondestructive wavelength dispersive X-ray fluorescence spectrometry (WD-XRF) was developed for the determination of sulfur in soils and stream sediments. WD-XRF was used to study the spectral line shifts and matrix effects of different inorganic species such as sulfide, elemental sulfur, thiosulfate, sulfite and sulfate. Analysis of the spectral lines in the S Kα wavelength range confirmed that Mo Lα (2θ = 111.799 °) lines interfered with S Kα (2θ=110.683°) lines. Twenty-seven soils and stream sediments reference samples were used to calibrate and evaluate the analytical method and the detection limit for sulfur was 5.43 mg/kg. The relative error (%RE) of the reference samples was −8.3–6.4%, showing good accuracy. However, the single form of sulfur (sulfide, sulfite and sulfate) had a significant matrix enhancement effect in the sodium carbonate matrix, especially for sulfides, and its relative error was 11.9 ~ 26.9%. The results of WD-XRF, inductively coupled plasma emission spectroscopy (ICP-OES) and elemental infrared analyzer were compared. The fitness for purpose of the results was also evaluated by the quality criteria test proposed by the International Geological Correlation Programme (IGCP), from which it can be deduced that the method was adequate considering geochemical mapping application.

Highly Ordered and Crystalline Cu Nanowires in Anodic Aluminum Oxide Membranes for Biomedical Applications

1D metallic nanostructures have become a subject of intensive research due to their potential application in the biomedical field such as sensing, imaging, drug delivery, and biodevices. Herein, anodic aluminum oxide (AAO) template is used to electrochemically grow the highly crystalline Cu nanowires. The electrodeposition potential for copper solution is identified by cyclic voltammetry. The Cu nanowire‐deposited AAO template is further characterized using field emission scanning electron microscope (FESEM), energy dispersive X‐ray (EDX) spectroscopy, wavelength dispersive X‐ray fluorescence (WDXRF) spectroscopy, X‐ray diffraction (XRD), and electrochemical impedance spectroscopy (EIS). The Cu‐deposited AAO template is tested for antibacterial activity against different microorganisms (including both gram positive as well as gram negative). Further, the assessment of the cytotoxic nature of Cu nanowires is a fundamental step for their application in the biomedical field. The favorable properties of Cu‐deposited AAO template in terms of excellent antibacterial effects and low cytotoxicity promote their application in the biomedical field, especially for medical diagnosis.

Development and validation of a method for multielement analysis of apatite by total-reflection X-ray fluorescence spectrometry

Apatite group of minerals incorporates a large range of trace metals such as Sr, Y, U, Th, as well as the rare earth elements, that allows obtaining useful information on their genesis and could be used in several applications in geology and geochemistry. In this study, a new method for the multielement analysis of apatite using total-reflection X-ray fluorescence spectrometry (TXRF) was developed. The acid digestion procedure was chosen as an optimal sample preparation with the capability to analyze a low sample amount (~5–10 mg). The validation of the method passed through the combination of procedures: analysis of Durango and Otter Lake well-known apatite samples; using inductively coupled plasma mass spectrometry and wavelength-dispersive X-ray fluorescence spectrometry as reference analytical methods; assessment of the measurement uncertainty. The proposed TXRF method is advantageous in being fast, cheap and simple for the multielement analysis of apatite with high accuracy.

Particle Induced X-ray Emission spectrometry (PIXE) of Hawaiian volcanics: An analogue study to evaluate the APXS field analysis of geologic materials on Mars

The Alpha Particle X-ray Spectrometer (APXS), a field instrument onboard four martian rovers, measures largely unprepared, in situ samples on Mars. The APXS has high precision that enables the determination of elemental concentrations in a wide range of geologic materials. However, lack of sample preparation can lead to heterogeneous matrix effects, and understanding the associated uncertainty is essential for interpreting APXS data. Here we use Particle Induced X-ray Emission spectrometry (PIXE) to analyze a suite of geologic samples from Hawai'i as an analogue study to better understand APXS analyses of martian samples. Wavelength-Dispersive X-ray Fluorescence (WDXRF) analyses of fused glass beads establish higher-accuracy standards for the Hawaiian samples. Sulfate-silicate mixtures were made to evaluate sulfur analysis by PIXE. Results show that the PIXE concentrations for most major elements have 2–6% accuracy, which is comparable to the APXS. However, the PIXE concentrations are systematically high in Al and low in Mg, resulting in lower accuracy (13% and 20%, respectively). Olivine-phyric lavas and most of their altered products have the largest discrepancies with Al concentrations up to 25% high and Mg up to 35% low. Sulfur is systematically high (up to 30% in a basalt matrix) compared to gravimetric S concentrations in the sulfate-silicate mixtures. These systematic deviations in Mg, Al, and S are linked to heterogeneous matrix effects, because PIXE and APXS analyses assume all atoms in a sample to be homogeneously mixed on the sub-micrometer scale, which is not the case. Two key implications for APXS results are: (1) Olivine-bearing samples likely have reported concentrations of Mg that is too low and Al that is too high. Thus, olivine-phyric basalts in Gusev crater and the basaltic sand and soil at three landing sites may have Mg and Al concentrations closer to those of the olivine-phyric shergottites and modelled martian crust than previously thought. (2) Sulfate-silicate mixtures may have overestimated S concentrations reported, resulting in greater uncertainty in the stoichiometry of Ca-sulfates, which is used to deduce the geochemical associations of sulfur in samples.

The role of surfactants in induced electrodeposition of Zn–Mo layer from citrate solutions

The influence of various additives on the process of electrodeposition of Zn–Mo coatings from citrate solutions was examined. Potentiostatic deposition, Wavelength dispersive X-ray fluorescence (WDXRF), X-ray diffraction and micro-Raman spectroscopy were carried out to analyze the role surfactants of electrodeposition of Zn–Mo layers. Atomic force microscopy was applied to investigate the surface morphologies. The mechanism describing the action of surfactant during the co-deposition process of Zn–Mo has been proposed. It was found that the additive can adsorb specifically on the Inner Helmholtz Plane (IHPs) on the cathode and consequently limiting the approaching of other molecules (complexes) to the surface. Reduction processes are associated mainly with the formation and adsorption of zinc citrate complexes and mixed Zn(I)–Mo(VI)-citrate complexes those further reduce to metallic zinc and metallic zinc-molybdenum alloy (two hexagonal metallic phases). What is remarkable by hindering the reduction of the Zn(I)-citrate complex, the surfactant inhibits the reduction of zinc to metallic zinc and at the same time facilitates (catalyzes) the formation of the Zn(I)–Mo(VI)-citrate complex. The presence of only PEG 20000 in the bath causes deposition of one (Zn,Mo) hcp phase. While the presence in the bath of CTAB, Triton X-100 or D-sorbitol makes that two hcp phases can create: (Zn) and (Zn,Mo) or one hcp phase (Zn) and one oxide phase (MoO2).However, absence of surfactants or not optimal concentration of surfactants in the electrolyte and low ratio of concentrations of Zn(II) to Mo(VI) cause the reduction of molybdenum complexes only to molybdenum oxides which blocked the cathode surface, when in the case of greater ratio of concentrations of Zn(II) to Mo(VI) (increase the reduction rate of zinc citrate complexes in comparison to mixed Zn(I)–Mo(VI)-citrate complexes and molybdate citrate complexes ([(MoO4)H3cit]3-)) the metallic zinc, zinc oxides, and molybdenum oxides can co-deposit on the electrode surface (composite coatings of oxide nanoparticles dispersed within a zinc matrix).

Source Identification of Trace Elements in PM2.5 at a Rural Site in the North China Plain

An intensive sampling of PM2.5 was conducted at a rural site (Gucheng) in the North China Plain from 22 October to 23 November 2016. A total of 25 elements (Al, Na, Cl, Mg, P, S, K, Ca, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Se, Br, Sr, Cd, Ba, Pb, and Sb) from PM2.5 filter samples collected daily were measured using a wavelength dispersive X-ray fluorescence spectrometer. Cl, S, and K were the most abundant elements, with average concentrations of 2077.66 ng m−3 (range 118.88–4638.96 ng m−3), 1748.78 ng m−3 (range 276.67–4335.59 ng m−3), and 1287.07 ng m−3 (range 254.90–2748.63 ng m−3), respectively. Among noncrustal trace metal elements, the concentration of Zn was the highest, with an average of 397.74 ng m−3 (range 36.45–1602.96 ng m−3), followed by Sb and Pb, on average, of 299.20 ng m−3 and 184.52 ng m−3, respectively. The morphologies of PM2.5 samples were observed using scanning electron microscopy. The shape of the particles was predominantly spherical, chain-like, and irregular. Positive matrix factorization analysis revealed that soil dust, following by industry, secondary formation, vehicle emissions, biomass and waste burning, and coal combustion, were the main sources of PM2.5. The results of cluster, potential source contribution function, and concentration weighted trajectory analyses suggested that local emissions from Hebei Province, as well as regional transport from Beijing, Tianjin, Shandong, and Shanxi Province, and long-range transport from Inner Mongolia, were the main contributors to PM2.5 pollution.

In-line characterization of ultrathin transition metal dichalcogenides using X-ray fluorescence and X-ray photoelectron spectroscopy

Industry-scalable fabrication methods of sulfur-based transition metal dichalcogenides are being developed, which puts strong requirements on the characterization of these mono- and few-layer materials in a cleanroom environment. In this paper, we show that the stoichiometry of ultrathin molydbenum disulfide layers can be determined by inline X-ray photoemission spectroscopy and wavelength-dispersive X-ray fluorescence, within the uncertainty provided by reference-free X-ray fluorescence in grazing incidence performed at the Physikalisch-Technische Bundesanstalt. In addition, we demonstrate that automated inline wavelength-dispersive X-ray fluorescence analysis can accurately determine the mass deposition of molybdenum and sulfur. Such information is crucial to support and accelerate the development of multi-parametric sulfur-based transition metal dichalcogenides processes, for instance by careful adjustment of the mass deposition per deposition cycle, both on samples and full wafers.

Analysis of elements secreted by CHO-K1 cells exposed to gamma radiation under different treatments

Purpose: The aim of the study was to determine the concentration of elements using the two methods: total reflection X-ray fluorescence (TXRF) and wavelength dispersive X-ray fluorescence (WD-XRF) in two media, DMEM + and PBS+.Materials and methods: Tests were carried out at 37 and 0 °C, irradiated by gamma radiation doses of 0, 0.25, 0.5, 5 Gy, both with and without contact with CHO-K1 cells. The survival of non-irradiated CHO-K1 cells was determined after transmission of media from irradiated CHO-K1.Results: Normalized concentrations of elements as a percentage of control data (i.e. 0 Gy dose) for Al, P, S, Cl, K, Ca, Zn, Br, were determined using the TXRF method and for Na, P, S, Cl, K, Ca determined using the WD-XRF method in DMEM + and PBS + without and with contact with cells at two temperatures, 37 and 0 °C, and three absorbed doses of 0.25, 0.5 and 5 Gy. Concentration of elements, presented on the coordinates of the two principal components (PC) for media without contact with cells, determined by the TXRF method and in contact with cells, determined by the TXRF and WD-XRF methods were presented. Treatments to which the media were subjected, presented as co-ordinates determined by the first two PC when media were without and in contact with cells (TXRF method) and for media in contact with cells (WD-XRF method) were shown.Conclusions: The results showed that a statistically significant difference occurred in elemental concentrations for media in contact with the cells at the temperatures used. From principal component analysis (PCA), it was observed that the concentrations of elements such as Al, K, Ca, Zn, Br were similar to each other, in contrast to the concentrations of P, Cl, S, both with contact and without contact with cells. A high correlation between the treatment of media within the group at doses of 0.25 Gy and for the group with 0.5 and 5 Gy doses was confirmed. Numerous correlations were observed between the concentrations of elements for media that were in contact with cells, which were not observed in media without contact with cells. The survival of non-irradiated CHO-K1 cells, was determined after transmission of media from irradiated CHO-K1 cells showing no statistically significant differences.

Chemical and Mineralogical Characterization of Malaysian Monazite Concentrate

Chemical and mineralogical characterization of Malaysian monazite, a phosphate mineral, bearing rare earth elements separated from the tin tailings originated from Ipoh, Perak, Malaysia, was performed in this paper. The study aims to collect detailed information on the chemical composition, crystal phases, and microstructure of the mineral monazite concentrate that would aid to optimize the subsequent hydrometallurgical processes for high-efficient separation of thorium and other associated rare earth elements. A systematic characterization study of the concentrate was conducted using techniques such as optical microscopy (OM), scanning electron microscopy (SEM) equipped with energy-dispersive X-ray spectroscopy (EDS), and Fourier-transform infrared spectroscopy (FTIR). These techniques analyzed the morphological details on the surface, elemental analysis, and mineral association assessment and identified the surface functionalization groups. The bulk composition and the mineral phases in which the elements are present were studied by wavelength-dispersive X-ray fluorescence (WD-XRF) and X-ray diffraction (XRD) studies respectively. The XRF analysis confirmed the presence of Ce, La, Nd, Pr, and Y (rare earth oxides: REO’s ~ 60 wt.%) while thorium dioxide (ThO2) accounted for 7 wt.% of the total composition. Traces of Ca, K, Al, Fe, Ti, and Mn were also confirmed by SEM elemental mapping. The XRD results confirmed that the concentrate was primarily composed of monazite (Ce, La, Nd, Th (PO4)) along with minor impurity phases of quartz. Automated mineralogical analysis was used as a confirmatory tool to corroborate the preliminary evidences. Based on the particle size distribution analysis supported by SEM, the majority of monazite grains were found to be present in the size range of 170–210 μm. Strong bands of PO4 and SiO4 were observed in the IR spectra corresponding to the phospho-silicate matrix of the REE mineral.

Laser-induced breakdown spectroscopy (LIBS) and wavelength dispersive X-ray fluorescence (WDXRF) data fusion to predict the concentration of K, Mg and P in bean seed samples

The present study aims to develop a fast and simple method for the determination of potassium (K), magnesium (Mg) and phosphor (P) in bean seed samples employing a data fusion strategy in the low-level with laser-induced breakdown spectroscopy (LIBS) and wavelength dispersive X-ray fluorescence (WDXRF) techniques combined with direct solid sample analysis. Univariate and multivariate (multiple linear regression, MLR) calibration and leave-one-out cross validation strategies were evaluated to build the calibration models correlated with reference values obtained by inductively coupled plasma optical emission spectrometry (ICP OES) after microwave-assisted acid digestion. The proposed calibration models for WDXRF and LIBS were tested using 14 samples, where the best results were obtained using the data fusion of both techniques. The standard error of cross validation (SECV) obtained were: 0.12% for K, 0.019% for Mg and 0.10% for P, and the trueness ranged between 89 and 124% for K, 82 to 125% for Mg and 73 to 128% for P. These values showed a good accuracy, precise and robustness of the method and a greater reliability of the results. In addition, the predicted concentrations ranged from 0.97 to 1.55% for K, 0.14 to 0.28% for Mg, and 0.27 to 0.82% for P.

What shall we put in the grave? Archaeometric analyses of ceramics from a late Pre-Roman, Roman and Migration period cemetery in Malbork-Wielbark, northern Poland

AbstractThe necropolis at Malbork-Wielbark was excavated from 1927 to 1936 and 2008 to 2019. This burial ground is the eponymous site of the Wielbark culture. To date, over 2000 burials, both inhumation and cremation (pit and urn graves), have been recorded at this site, attesting to its continuous use from the Early Pre-Roman Iron Age (phase A1) to the early Migration Period (phase D1), with particular emphasis on the Roman Period. The cemetery site partially overlies and damages an earlier Iron Age settlement of the Pomeranian culture.Laboratory analyses were carried out on 113 pottery sherds. The series of samples chosen for analysis reflected, as far as was possible, all relative chronological phases and vessel shapes. The pottery was analysed using a step by step strategy built on the results of MGR-analysis (i. e. the classification of samples based on their matrix type) and on a macroscopic assessment of clastic material. In addition, an estimation of chemical composition by portable energy-dispersive X-ray fluorescence (pXRF) was available for each sample. After they had been classified, samples were selected for chemical analysis by wavelength-dispersive X-ray fluorescence (WD-XRF), estimation of physical ceramic properties (open porosity, water absorption and apparent density), Kilb-Hennike analysis (K-H analysis), thin-section studies using a polarising microscope, a study of surface phenomena by RTI (Reflectance Transformation Imaging), thermal analysis (TG-DTG-DTA), X-ray diffraction analysis and functional properties analysis (water permeability and thermal shock resistance), as well as experimental estimation of magnetic properties.The results of MGR-analysis carried out on ceramic samples taken from 113 potsherds revealed that all of the pottery was made from various non-calcareous clays with fine-grained iron compounds homogeneously distributed in the matrix. It was decided not to carry on determining/using MGR-groups, as nearly every sherd represents a different MGR-group. This means that these vessels were made during different production cycles. The differences in thermal behaviour between samples were attributed only to matrix-type groups. It can be concluded that 85 % of the total sherds were made from plastic raw materials of the same provenance, and that the same matrix-type groups occurred in all chronological phases. The percentage of vessels made of particular raw materials indicates a significant difference in the preferences of Pomeranian Culture potters and those of Pre-Roman Iron Age, Early Roman Period and those of the Late Roman Period, when one type of raw material disappears from use. This last period is also characterized by an increase in the number of vessels fired in a reducing atmosphere. Standardization is also evident in vessel-wall thickness, which falls within a narrow range of values, on the other hand combined with a large variety in grain sizes up to very large ones and with a wide range of open porosity values, which in turn points to a lack of care in the preparation of the ceramic body. Vessels that may have been non-local origin are noted in all chronological phases. Analysis of functional properties (water permeability and thermal shock resistance) revealed that the pottery deposited in graves included fully functional wares, such as cooking pots, as well as vessels intended solely as grave goods.More than a few samples evidence the use of a slow-rotating potter’s wheel, and it is also possible that a template was used for forming vessel rims. However, there are very few examples of truly technologically advanced vessels. The technology is generally tailored to the desired type or form of vessel.

The Effect of a Substrate Material on Composition Gradients of Fe-Ni Films obtained by Electrodeposition

The electrodeposition of FeNi alloy films was performed galvanostatically in the sulfate solution (Fe2+/Ni2+ mass ratio 1:2) in order investigate their co-deposition mechanism. The FeNi layers were deposited at variable substrates (copper, brass, silver) under the same chemical (electrolyte composition) and electric plating (current density value) conditions. After applying various time, substrates and external magnetic field orientation, the quality of the obtained film was examined. The surface morphology and crystallographic texture variation were investigated by the Scanning Electron Microscope (SEM), Energy Dispersive X-ray Spectroscopy (EDX), Wavelength Dispersive X-ray Fluorescence (WDXRF) and Laser Confocal Scanning Microscope (LCSM). The anomalous co-deposition of iron group metals is evidently dependent on the substrate.