EDXRF Techniques Research Articles

Pottery Production Changes During the Transition from Byzantine to Umayyad Rule

Pottery is the most affected tool by the changes in human societies; this is due to its flexibility during forming. In order to estimate the effect of the transition of inhabitants of the urban center of Umm Qais (Gadara), north Jordan, from Byzantine (Christianity) to Umayyad (Islam) rule on pottery production traditions, a total of 29 cooking pots and sherds of pottery jars were selected. The samples were dated according to stratigraphy, archaeological context, and parallel examples to the proposed periods. The samples were investigated following the typological and archaeometric approaches. The raw materials and firing technology of the pottery during the two periods were determined following chemical and mineralogical methods using petrography, XRD, ED-XRF, and EDX-SEM techniques. The results revealed that many styles and forms of pottery continued to be produced and some new styles emerged at the urban center of Gadara. Technically, the potters inherited the knowledge of selecting the available raw materials and firing conditions of pottery during the Byzantine and Umayyad periods. During these periods, Umm Qais potters used the local raw materials—non-calcareous ferruginous illite clays mixed with medium to high amounts of coarse quartz grains and fired at temperatures around 1000° in an oxidizing atmosphere to produce cooking pots. They used the available medium to highcalcareous ferruginous illite clays and fired them at temperatures between 850° and 950° in an oxidizing atmosphere to produce the jars. Importing fine fabric jars and cooking pots during the seventh century from Jarash are indicated too. Thus, the types and forms of everyday use pottery were more affected by the political and religious changes than the technical aspects.

The concentration influence of multi-walled carbon nanotubes coating on fatigue edge crack growth and other mechanical properties of Al 7075-T6 thin plates

In the current study, the incline edge crack growth behavior in an aluminum alloy 7075-T6 specimens (which were coated using nickel-carbon nanotubes electroless coating) has been investigated undergoes uniaxial tensile fatigue loading. High purity multi walled carbon nanotubes have been used in nano-coating solutions with various concentrations (1 g/l, 2 g/l and 3 g/l) to examine the improvement extent of fatigue crack growth resistance and other mechanical properties. Water jet technique was used to cutting aluminum plates to the required dimensions before the nano-coating procedure. Multi-purpose fatigue apparatus has been adopted to apply tensile fatigue loading with zero stress ratios. High magnification camera with image j software has been utilized to measure the propagated crack lengths with the number of fatigue cycles. To inspection the quality, thickness uniformity and homogeneity of the nano-coating layer over specimen surfaces, EDXRF and FESEM techniques have been adopted in this study. Numerical simulation using ABAQUS 2021 programming was performed for the purpose of the results validation. The measured results offered a 25.9 %, 44.5 % and 47.9 % increasing in the hardness of the coated specimens using 1 g/l, 2 g/l and 3 g/l MWCNTs respectively. The modulus of elasticity produced an increasing of 26.7 %, 44.4 % and 46.3 % for the coated specimens using 1 g/l, 2 g/l and 3 g/l MWCNTs respectively. The nano-coating with 2 g/l MWCNTs produced more homogeneous, uniform thickness coating layer and fatigue crack growth resistance than that of the coated specimens using other concentrations of MWCNTs. The similarity in the crack growth behavior was the major outcome of the results validation from the fatigue tests and numerical simulation.

Air quality challenges in Central Asian urban areas: a PM2.5 source apportionment analysis in Dushanbe, Tajikistan.

This work presents the first comprehensive assessment of PM pollution sources in Dushanbe, Tajikistan. A total of 138 PM2.5 samples were collected during 2015-2016 and 2018-2019 and were analyzed through gravimetric, ED-XRF, and multi-wavelength absorption techniques. The results show that PM2.5 concentrations were substantially higher than the European annual limit value and WHO Air Quality Guidelines annual average value, with an average of 90.9 ± 68.5μgm-3. The PMF application identified eight sources of pollution that influenced PM2.5 concentration levels in the area. Coal burning (21.3%) and biomass burning (22.3%) were the dominant sources during the winter, while vehicular traffic (7.7%) contributed more during the warm season. Power plant emissions (17.5%) showed enhanced contributions during the warm months, likely due to high energy demand. Cement industry emissions (6.9%) exhibited significant contribution during the cold period of 2018-2019, while soil dust (11.3%) and secondary sulphates (11.5%) displayed increased contribution during the warm and cold months, respectively. Finally, waste burning (1.5%) displayed the lowest contribution, with no significant temporal variation. Our results highlight the significant impact of anthropogenic activities, and especially the use of coal burning for energy production (both in power plants and for residential heating), and the significant contribution of biomass burning during both warm and cold seasons.

Radiation grafting mediated tailoring of a mercury (Hg(II)) selective adsorbent “RAdMer”: Mechanistic insights, uptake performance and reusability evaluation in artificially contaminated groundwater

The presence of mercury (Hg(II)) in water bodies poses a pressing threat not only to aquatic life forms but also human health. This work proposes the fabrication of a novel thiol (-SH), amine (–NH–) and carboxylic (-COOH) group containing trifunctional adsorbent based on a radiolytically surface engineered biodegradable platform for selective sequestration of Hg(II) from aqueous media. Polyacrylonitrile (PAN) was gamma radiolytically incorporated onto cotton fabric via Radiation Induced Graft Polymerization (RIGP) process, followed by chemical conversion of the nitrile groups using dl-Cysteine as the trifunctional agent. The developed adsorbent RAdMer was characterized by FTIR, TGA, SEM-EDX, EDXRF, XRD, CHNS, 13C NMR and XPS techniques, and tested for Hg(II) removal in batch and continuous flow adsorption modes. Adsorption kinetics and equilibrium characteristics were validated using various theoretical models as well column adsorption models. Density Functional Theory (DFT) calculations performed to determine the complexation mechanism revealed the binding to be occurring predominantly in a 1:2 metal to ligand ratio with calculated binding affinity of −19.63 kcal.mol−1. RAdMer demonstrated fast uptake kinetics with over 60 % of total Hg(II) adsorption occurring within the first 30 min, while peak adsorption capacity was calculated at 174.3 mg.g−1. Moreover, RAdMer could be reused for >5 iterative cycles using an optimized HCl-Thiourea eluent system. Acting upon the UNOs SDG6 principle of providing “clean water and sanitation for all”, RAdMer efficiency was demonstrated with Hg(II) spiked ground water samples to successfully achieve the WHO permissible limit of <1.0 μg.L−1, and can therefore be potentially upscaled as an efficient methodology for remediation of Hg(II) ions in contaminated water.

Vibrational spectroscopic, crystallographic, and microscopic investigation on the Aioun El Atrouss diogenite

AbstractDiogenites are thought to have originated from asteroid 4 Vesta asteroid, and it has been previously shown that they mostly consist of orthopyroxene, chromite, and olivine minerals. In this study, the Aioun El Atrouss (AAT‐1) diogenite was analyzed by vibrational spectroscopic (FT‐IR and micro‐Raman), EDXRF, and XRD techniques. AAT‐001 is mainly composed of pyroxene and with lesser olivine. XRD investigation confirmed magnetite, kamacite, ilmenite, and albite. A troilite‐orthopyroxene intergrowth was revealed by XRF. The olivine composition was estimated to be approximately Fo66 by Raman olivine characteristic doublets. Pyroxenes in AAT‐01 were found to be En80Fs20. Finally, approximate peak shock pressure of more than 86 GPa for AAT‐1 was suggested based on previous hypervelocity impact experiments on olivine.

CellUSorb: A high-performance, radiation functionalized cellulose based adsorbent for Uranium (VI) remediation in ground water

A state of the art, phosphate functionalized cotton cellulose based green U(VI) adsorbent has been synthesized via single step, 60Co gamma radiation mediated simultaneous irradiation grafting process, wherein bis(2-methacryloxyethyl) phosphate (B2MEP) was grafted onto cotton cellulose fabric. Samples were characterized using 13C NMR, FTIR, EDXRF, XRD and SEM techniques. Poly(B2MEP)-g-cellulose adsorbent (CellUSorb) was tested for removal of Uranyl (U(VI)) ions from water, adsorption capacities being 79.9 mg.g−1 and 135.9 mg.g−1 in batch and column modes, respectively. The equilibrium adsorption data were analyzed using Langmuir, Freundlich and Redlich-Peterson isotherm models, and kinetic data using pseudo first order, pseudo second order, intra-particle diffusion and Boyd’s models. The adsorbent viability was enhanced through regeneration achieved using ammonium oxalate as eluent, ensuring reusability for five cycles with < 20 % attrition loss/cycle. A standalone, portable water treatment set up, housing a ∼ 100 g CellUSorb cartridge (maximum theoretical U(VI) adsorption capacity ∼ 27,200L for [U(VI)] = 500 µg.L−1), has been conceptualized, fabricated and successfully tested for U(VI) removal to < 30 µg.L−1 (WHO permissible limit) from contaminated water. With potential upscaling for large scale, onsite U(VI) remediation, CellUSorb is a promising prospect that spotlights the role of cellulose in accomplishing UNO’s Sustainable Development Goal of “clean water for all” (SDG6).

Analysis of coal ash samples from thermal power plants of India for their gallium content using NAA and EDXRF techniques

Coal fly ash (CFA) is an important secondary source for the recovery of gallium (Ga) which has a high potential for its wide applications in many strategic fields such as cellular communications and direct broadcast satellite.Various coal fly and bottom ash samples obtained from thermal power plants located in different parts of India were investigated for their gallium content using NAA and EDXRF techniques. The concentration of gallium in NIST SRM 1633b CFA is not available in NIST certificate and hence was established using k0 based IM-NAA method along with the other certified elements like As, Ce, Co, Eu, Fe, K etc. In addition, the gallium concentration in the NIST SRM was also obtained by relative NAA using Ga2O3 as a standard towards the validation of IM-NAA. Using the NIST SRM, the gallium content in the ash samples of Bituminous coal collected from South Central and Eastern India was found to be from 17.2 to 47.9 mg/kg whereas the same was 6.3–33.3 mg/kg for the ash samples of Lignite coal collected from the South-Central India and Western India. The gallium concentrations obtained by NAA in coal ash samples were compared with another non-destructive assay technique, i.e. EDXRF and the results are found to be in good agreement. These samples were proved to be a potential secondary source of gallium, available in India.

Extraction and Purification of Phosphorus from the Ashes of Incinerated Biological Sewage Sludge

Phosphorus depletion represents a significant problem. Ash of incinerated biological sewage sludge (BSS) contains P, but the presence of heavy metals (e.g., Fe and Al) is the main issue. Based on chemical characterization by SEM-EDS, ED-XRF and ICP-OES techniques, the characteristics and P content of bottom ash (BA) and fly ash (FA) of incinerated BSS were very similar. On BA, P extraction carried out in counter- current with an S:L ratio of 1:10 and H2SO4 0.5 M led to better extraction yields than those of a similar test with H2SO4 1 M and an S:L ratio of 1:5 (93% vs. 86%). Comparing yields with H2SO4 0.5 M (S:L ratio of 1:10), the counter-current method gave better results than those of the crossflow method (93% vs. 83.9%), also improving the performance obtained with HCl in crossflow (93% vs. 89.3%). The results suggest that the purification of the acid extract from heavy metals with pH variation was impractical due to metal precipitation as phosphates. Extraction with H2SO4 and subsequent treatment with isoamyl alcohol represented the best option to extract and purify P, leading to 81% extraction yields of P with low amounts of metals.

Immobilization of crystalline Fe2O3 nanoparticles over SiO2 for creating an active and stable catalyst: A demand for high temperature sulfuric acid decomposition

To address the issues of catalytic activity and stability of the promising Fe2O3/SiO2 catalyst for sulfuric acid decomposition, Fe2O3 was immobilized on SiO2 support by polyol, solvothermal and wet-impregnation methods and examined. The different methods yielded catalysts with varying crystal structure, porosity, morphology and redox properties which were investigated by XRD, Mössbauer spectroscopy, N2-BET surface area, SAXS, ED-XRF, HR-TEM, TPR/O and XPS techniques. The effect of the properties on the activity and stability was evaluated in a fixed-bed reactor and a structure-activity correlation was established. Above 750 °C the catalytic activity followed the order polyol > wet impregnation ∼ solvothermal. Stability of the sample prepared by polyol method was ascertained by 100 h experimental run at 800 °C. The higher activity and stability of the Fe2O3/SiO2 catalyst (polyol) is ascribed to the development of crystalline α-Fe2O3 dispersed phase, higher pore confinement, better support-active phase interactions and higher degree of reduction.

Leaching of platinum group metals from spent automotive catalysts using organic acids

An efficient and environmentally friendly new process is described for the recovery of platinum group metals from spent automotive catalysts. The process consists of the application of mechanical processing followed by heat treatment and leaching, with the aim of reducing the use of acids that can have adverse effects in the environment. The extraction of PGMs was carried out using HCl associated with malic, formic, and citric acids. Evaluation was made of the effects of parameters including acid concentration, volumes of inorganic and organic acids, solid to liquid (S/L) ratio, and extraction time. The automotive catalyst powders were characterized using XRD, SEM/EDS, particle size distribution, and EDXRF techniques. The spent automotive catalysts contained reasonable concentrations of Pt and Pd. Over 90% of the Pt and Pd could be recovered in a leaching process using 6 M HCl, S/L ratio of 1:30, and 20% (v/v) citric acid. The findings showed that citric acid can be used in the recovery of PGMs from spent automotive catalysts, decreasing the use of aggressive and corrosive acids often employed in the recovery of these metals. Hence, the addition of organic acids can contribute to efficient and environmentally friendly processes for the recovery of Pt and Pd.

Předběžná zpráva o výzkumu jeskyně Švédův stůl v Moravském krase v roce 2019

Švédův Stůl Cave in the Moravian Karst has been excavated several times since Martin Kříž started the first excavation in 1886. Two parts of the site were re-excavated in 2019. The primary aim was to conduct classical as well as innovative and experimental sedimentological and geoarchaeological investigations of sediments from the discarded spoil heap outside the cave entrance (trench C–D). Intact sediments with a small number of lithic artefacts and a large number of animal bones were also excavated during the 2019 excavation (trench A–B) located under the trench excavated by Bohuslav Klíma’s team in the 1950s. An attempt is being made using pXRF, benchtop ED-XRF and ITRAX techniques to link some of the sedimentary material in the spoil heap (C–D) with the stratified sediments in trench A–B. Animal bones and lithic artefacts were found in both trenches. Numerous samples were collected for geoarchaeological, palaeoenvironmental and dating analyses and the results will be published in upcoming publications.

Zirconium Alginate Beads: A Renewable Source for the Biosorption of Fluoride from Contaminated Ground Water

In view of the fluoride induced toxic effects on human health; an effective and simple biosorption method was developed for fluoride laden groundwater using zirconium alginate beads. The various parameters affecting the batch adsorption in fluoride spiked groundwater such as initial fluoride concentration (2.5-10 mg/L), residence time (10-120 min) and pH (5, 7, 9) were studied. The fluoride concentration in the solutions was measured by spectrophotometry at 550 nm using in-house developed zirconyl-xylenol orange complex reagent. The biosorbent was characterized with techniques such as X-ray diffraction (XRD), Fourier transform infrared Spectroscopy (FTIR), scanning electron microscopy (SEM) and energy dispersive X-ray fluorescence (EDX). At pH 5, 7 and 9; fluoride removal of 90.5, 46.6 and 88.8% by the biosorbent was noted in groundwater spiked with 10 mg/L of fluoride, within 30 min. Thus, the zirconium alginate beads were found to be potential biosorbents for remediation of groundwater contaminated with fluoride. Further studies are going on to find out the reusability of the developed biosorbent at field conditions. The biosorption mechanism was derived from sorption studies, FTIR, SEM and EDXRF techniques.

Studying the link between physiological performance of Crotalaria ochroleuca and the distribution of Ca, P, K and S in seeds with X-ray fluorescence.

This study describes the use of X-ray fluorescence spectroscopy in Crotalaria ochroleuca seed technology. This work evaluated X-ray fluorescence techniques to estimate the physiological performance of different C. ochroleuca seed coat colours based on the concentration and distribution of Ca, P, K, and S in seed structures. The treatments consisted of seeds separated by coat colours (yellow, green, and red) and a control treatment (colour mix according to their natural occurrence in commercial lots), and was carried out in a completely randomized design, with four replications. The physiological performance was evaluated by analyzing the water content, germination, first germination count, germination speed index, electrical conductivity, seedling emergence, and seedling length and dry mass. X-ray fluorescence spectroscopy techniques were carried out with quantitative analyses (Ca, P, K, and S concentration in the seed coat and the whole seed) and qualitative analyses (macronutrient mapping). The EDXRF and μ-XRF techniques are efficient and promising to differentiate the physiological performance of C. ochroleuca seeds, based on the concentration and distribution of Ca, P, K, and S in different structures. Ca is predominant in the seed coat, and K, S, and P are found throughout the embryonic axis. Seeds of yellow and green coats have higher nutrients concentration and distribution in the embryonic axis, revealing high germinative capacity and physiological performance. Seeds of red coat have higher nutrients concentration in the seed coat and lower assimilation, showing less vigour, which interferes directly in the quality of commercial lots.

Ceramic resistors as optically stimulated luminescent retrospective dosimeters

Application of optically stimulated luminescence (OSL) as a retrospective dosimetric technique is studied using ceramic resistors available in commonly used instruments like personal computers, printers, household electronic appliances etc. In order to understand the OSL process the composition of the ceramic resistors was analysed using XRD, FTIR and ED-XRF techniques and it is found to have hydrated calcium aluminium silicate as the major constituent along with trace impurities for the origin of radiation induced OSL. The important retrospective dosimetric characteristics like its OSL sensitivity, reproducibility, OSL dose response and stability of the signal upon storage after exposure have been studied. The dose response was found to be linear from 100 mGy to 5 Gy. It is also observed that the OSL signal decreases by 30% in the first 3 days and thereafter there is negligible fading up to 30 days. The correlation between TL and OSL signals in the material was also studied. Using Single Aliquot Regenerative (SAR) technique, the dose was recovered with very good accuracy. These dosimetric studies showed that carbon film ceramic resistors have potential use as emergency dosimeter.

Applications of Raman spectroscopy in art and archaeology

Applications of Raman spectroscopy in art and archaeology

Green extraction of Niobium and Tantalum from Kenticha Tantalite ore using 1-Ethyl-3-Methyl Imidazolium Chloride ionic liquid

The decomposition of the Ethiopian Kenticha tantalite ore was studied using the KOH fusion and H2O leaching system at 400 0C for a 1 h reaction time. The experimental results obtained showed that 27 wt% of Ta2O5 was mainly transformed into insoluble KTaO3, not to be KNbO3, and as well, into the dissolved liquor containing 94.73 vol% of Nb2O5 and 75.80 vol% of Ta2O5. The observations, supported by the EDXRF, XRD, and ICP-OES techniques, showed that the ratio of the dissolved mixture of Nb and Ta metal ions was beneficial to the solvent extraction from both Ta2O5 and Nb2O5. Niobium and tantalum were extracted from their neutralized alkaline dissolved and hydrolyzed solution by a new process using the EMIC/AlCl3 ionic liquid as the extractant using selective stripping, precipitation, and calcination of a highly crystalline pure 99.84 wt% of Nb2O5 and amophours 90.81 wt% of Ta2O5. The compositions of the dissolved metal ions and solids were analyzed by the ICP-OES, EDXRF, XRD, and FT-IR techniques.

Contribution of flyash from coal-fired thermal power plants to uranium contamination of ground water

The elemental concentration of uranium in flyash and coal samples has been investigated using EDXRF and WDXRF techniques. To check the contribution of flyash to uranium contamination of ground water in the Malwa region of Punjab, the flyash and coal samples are collected from Guru Nanak Dev Thermal Power Plant (GNDTPP) in the Bathinda district of Punjab state, India. It is found that uranium concentration in the flyash is below the detection limit of the XRF set up, i.e. ~ 1 ppm. It is concluded that uranium contamination in the ground water of Malwa region is not due to the Thermal Power Plant.

Evaluation of energy dispersive scanning electron microscopy and X-ray fluorescence techniques for analysis of compost quality

The ED-XRF and SEM-EDS techniques are significant in analysis of compost quality and can be used as an alternative for AAS.

Comparison of the analytical performance of EDXRF and FAAS techniques in the determination of metal species concentrations using protocol 3050B (USEPA)

ABSTRACTSediments are active environmental compartments capable of interchanging the chemical species with the water column, degrading their quality and influencing the toxicity of the matrix. The average concentrations of sediment-associated metallic species have been used to evaluate the extent of their contamination. The approaches used have progressed considerably over the last few decades and different instrumental techniques have been employed in quali-quantification of metal compounds associated with sediments. This study aimed to evaluate the accuracy of the technique of Energy Dispersive X-Ray Fluorescence Spectrometry (EDXRF) performed on the equipment Shimadzu (model Rany, Series EDX-720) in the validation process, adopting as reference the technique of Flame Atomic Absorption Spectroscopy (FAAS), appliance GBC (model Avanta) to quantify the species: Zn, Fe, Ni, Cu, Pb and Cr in solution, in chemically available fraction (3050B Protocol-United States Environmental Protection Agency), extracted from sediments of the River Barigüi, metropolitan region of Curitiba, southern Brazil. The samples were collected according to the clean techniques protocols. The analytical figures of precision, accuracy and determination limit of the method were evaluated using the two techniques separately and on the same samples. Statistically significant differences were observed between the two methods.

Elemental and spectroscopic characterization of plasters from Fatih Mosque-Istanbul (Turkey) by combined micro-Raman, FTIR and EDXRF techniques

The characterization of the plasters and coloring agents of the wall paintings of Fatih Mosque have been performed using combined micro-Raman, FTIR and EDXRF techniques. The investigations show that the plaster used on the walls has mixed gypsum–lime binders. Cinnabar {HgS}, lead red {Pb3O4} and hematite {α-Fe2O3} were identified in the red surfaces. Blue color is attributed to ultramarine blue {Na8–10Al6Si6O24S2–4}. Green color is assigned to mixtures of green earth, copper phthalocyanine {Cu(C32Cl16N8)} and brochantite {CuSO4·3Cu(OH)2}. Strontium yellow {SrCrO4} and zinc white {ZnO} were also used to ensure the color tone. The results provide a basis for future restoration of wall paints.