X-ray Fluorescence Technique Research Articles

Validation of the analytical method using the energy dispersive X-ray fluorescence technique (EDXRF) for application in pharmaceutical sciences

The determination of impurities in raw materials intended for the production of pharmaceutical products is important to guarantee the quality of the final product, as well as to avoid damage to health. Metallic impurities can exhibit toxic effects even at low concentrations and so permissible levels are defined by the regulatory agencies and pharmacopeias. However, few methods are presented in official compendia in Brazil. In this sense, fast, sensitive, and precise techniques such as the energy dispersive X-ray fluorescence technique (EDXRF) must be evaluated for the analysis of metals in materials for pharmaceutical use. This way, therefore, there is the need to investigate the presence of contaminants and their concentration levels. The major goal of this research work was to validate a method for using the Energy Dispersive X-Ray Fluorescence (EDXRF) technique to identify and quantify the chemical composition of raw materials and pharmaceutical products. The methodology used was based on the selection of a microcrystalline cellulose matrix, which was spiked with two classes of contaminant elements, Class 1 (Cd, Pb, As, Hg) and Class 2A (Co, V, Ni) as defined by ICH guideline Q3D. The qualitative and quantitative analyses were carried out using the EDXRF technique, which proved to be quite effective and met all the validation parameters required in the mandatory official compendia (Resolution of the Collegiate Board (RDC) of Brazilian Health Regulatory Agency (Anvisa) nº 166, July 24, 2017), such as selectivity, linearity, precision, detection limit, quantification limit and robustness. This study showed that EDXRF can be used as a technique for detection and quantification of elemental impurities belonging to Class 1 and Class 2A.

Luminescence dating and firing temperature determination of ancient ceramics fragments from the Tunata-hill site in the Churajon archaeological complex in Arequipa, Peru

Ancient pottery fragments from the Tunata-hill site in Churajon archaeological complex, Arequipa, Peru, were dated by means of luminescence techniques such as thermoluminescence (TL) and optically stimulated luminescence (OSL) in order to provide absolute chronology. For TL, additive and regenerative methods were performed. For OSL a regenerative method was carried out for IRSL dating. A rigorous description of the study area and its context has been made. The ages of the samples were found to be between 0.50 ± 0.06 ky and 0.49 ± 0.03 ky for TL methods, and 0.49 ± 0.02 ky for OSL methods. On average, the estimated age by TL and OSL techniques is 490 ± 70 yr (1600 AD and 1460 AD). This means that Churajon ceramics under study would belong to the Late periods which corresponds to the Inca region, and the North sub-region of the Late Churajon phase, and the beginning of European colonization in Peru. X-ray fluorescence technique (XRF) analysis has shown the main presence of Fe (39.5%), Si (30.0%), and Al (10.4%) in fine pottery powder. Furthermore, the electron paramagnetic resonance (EPR) technique was used to study the firing temperature using the iron signal (Fe3+) as a firing temperature reference. The firing temperature of ceramics was found to be around 550 ± 50 °C.

Comparative study of pre-Hispanic and colonial adobes in Mexico. Preliminary inferences on the effects of the granulometric distribution and used recycled materials in the state conservation of earth architecture

The characterization of the pre-Hispanic and colonial adobes used in the construction of buildings in Mexico was carried out to know the differences between their processes and manufactures. The eight samples obtained correspond to adobe blocks 0.45 m long x 0.35 m wide and 0.12 m thick, which were part of the interiors of houses, the structure of fences, and hacienda galleys. These samples were investigated using X-ray Diffraction, X-ray Fluorescence, and Scanning Electron Microscopy techniques to determine the morphometry of the material and its chemical and mineralogical composition. Likewise, some analyzes were performed to determine their mechanical properties (simple compressive strength), physical properties (granulometry, solid density, cohesion, plasticity index, porosity, and moisture content), and biological (organic matter content). The results obtained in terms of the granulometric distribution indicate that pre-Hispanic adobe has a higher content of sand than silt-clay and gravel, while the colonial adobes present a low or null content of gravel with a higher content of silt-clays. Regarding the organic matter content, the colonial adobe presents the highest percentages compared to those of the pre-Hispanic adobes. Taking into account the above the pre-Hispanic adobes have better resistance and durability than colonial adobes due to their granulometric distribution, low organic matter content, good cohesion, high plasticity index, and the use of materials found in their natural environment, while the colonial used recycled materials, coming from the economic activity to which the hacienda was dedicated, for example, agriculture, mining, livestock, this has given rise to different manufacturing techniques and construction styles that reflect the state of conservation of buildings throughout the pre-Hispanic and colonial times. The granulometric distribution that pre-Hispanic adobe provides favorable physical and mechanical qualities for any construction technique, so it is recommended to use this formula to manufacture resistant and durable adobe.

Structural characterization of ultrathin diamond-like carbon overcoats for high areal density magnetic recording

This paper reports a comprehensive study on chemical structures of ultrathin diamond-like carbon (DLC) overcoats for high areal density magnetic recording. The DLC overcoats were fabricated in a range of thicknesses between 0.5 and 5.0 nm with Si interlayer on NiFe substrates using a pulsed filtered cathodic vacuum arc (PFCVA) technique. The overcoat thicknesses were accurately determined by high–resolution transmission electron microscopy and wavelength dispersive X-ray fluorescence techniques. The surface morphology, chemical composition, microstructure, and tribological properties were systematically investigated by atomic force microscopy, X-ray photoelectron spectroscopy, near-edge X-ray absorption fine structure, Raman spectroscopy techniques, and a reciprocating wear test. The results showed that the surface morphologies of DLC overcoats were atomically smooth with a root mean square surface roughness below 0.23 nm. The DLC overcoats had high sp3 bonds fraction. However, as the overcoat thickness was thinner than 1 nm, the sp2 bonds fraction suddenly increased resulting in a significant increase in the coefficient of friction. The obtained results demonstrated the limitation of the thickness of the DLC overcoat fabricated by the PFCVA technique as a protective coating for high–density magnetic storage devices.

High-temperature mass spectrometric study and modeling of ceramics based on the Al2 O3 -SiO2 -ZrO2 system.

Materials based on the Al2 O3 -SiO2 -ZrO2 system are promising for a wide range of high-temperature technological applications, such as thermal barrier coatings in the aviation and space industry or advanced materials in nuclear power reactors. Experimental studies of the ceramics based on this system by the Knudsen effusion mass spectrometric (KEMS) method are of significant interest in designing technological processes for the synthesis and exploitation of the Al2 O3 -SiO2 -ZrO2 materials. Samples of ceramics in the Al2 O3 -SiO2 -ZrO2 system, including the Al2 O3 -ZrO2 and SiO2 -ZrO2 binaries, were prepared by solid-state synthesis. Analysis of the samples was performed by X-ray fluorescence and diffraction techniques. The vapor composition and thermodynamic properties of the components in this system were determined by KEMS. The derived thermodynamic functions were optimized within the generalized lattice theory of associated solutions (GLTAS). In the temperature range 1900-2600 K, the SiO, Al,AlO, Al2 O, ZrO, ZrO2 , and O vapor species were identified over the samples in the systems under study. For the thermodynamic properties to be determined correctly, the samples of the Al2 O3 -SiO2 -ZrO2 system had to be vaporized at temperatures less than 2000 K, where data could be obtained only for the SiO species. The SiO2 activities obtained were taken as the experimental basis for the modeling within the GLTAS approach. This allowed evaluation of the component activities and excess Gibbs energy, and assessment of the relative number of bonds of different types. At 1920 K, the Al2 O3 -SiO2 -ZrO2 system is characterized by negative deviations of its thermodynamic properties from the ideal behavior. The consistency of the obtained modeling results was illustrated by comparison of the values derived from the data for the ternary and the boundary binary systems and thereby indicates the reasonable uniformity of the energy parameters of the lattice model derived in the calculations, which may be used in further modeling of multicomponent systems.

Analysis of the practices and technologies used for the treatment of brominated plastics of WEEE in Guadalajara city, Mexico

The increase in waste electrical and electronic equipment (WEEE) has become an attractive waste for the recycling industry, mainly due to the high volume found in the waste flow that can be transformed into other products. The purpose of this study is to investigate the treatments applied to WEEE brominated plastics in companies of recycling in the Metropolitan Area of Guadalajara (MAG), Mexico, and the compa­rison with international guidelines. The information-gathering was obtained through interviews and visits; fourteen companies dedicated to the field of recovery, treatment and/or recycling of electronic waste were identified. Only seven companies allowed the study to be carried out, and only five companies provided plastics samples. Eighty-six samples of different kinds of plastics were obtained and analyzed using the Han­dheld X-ray fluorescence (HXRF) technique, and the atypical cases have undergone an analysis of X-ray photoelectron spectroscopy (XPS) and X-ray energy dispersive spectrometer (EDS). Bromine was the predominant element in the samples analyzed, which sometimes exceeded the permissible limits of the European Directive 4 to 10 times, meaning that the concentration ranges go from 10000 to 39500 mg/kg. It was identified bromine as a chemical precursor of flame retardants, which is prohibited by international agreements because they cause damage to the environment and public health. As a result, the companies dedicated to the treatment and/or recycling of plastics from WEEE do not follow the practices and technologies used internationally. However, considering the circular economy, this is relevant to establish limits of traces of contaminants in recycled plastics.

Characterization of suspended particulate matter using cascade impactor and X-ray fluorescence

Atmospheric pollution has become one of the biggest environmental and public health problems in large urban centers. The process of industrialization and urbanization of large cities together with population growth and motorized transport has caused an increase in the level of air pollution in these places. Thus, this work approaches the characterization of suspended particulates in the surroundings of the Duque de Caxias Refinery (REDUC) from the identification of the chemical elements present using the X-ray fluorescence technique - XRF. A PIXE 8-stage impactor was used to collect the particulate material (aerodynamic diameters of 16 – 0.12 µm). On the other hand, the experimental measurements of XRF were performed using a commercial system ARTAX 200 (Bruker) and under the following conditions: voltage of 45 kV, current of 500 µA, acquisition time of 300 s and no filter in the incident X-ray beam. The study allowed estimating the dimensions of the particulate materials, identifying the chemical elements present and pointing out possible sources, from samples collected in three residential points that are in the surroundings of REDUC in the region of Campos Elísios. The X-ray fluorescence technique proved to be efficient and it was possible to detect the following chemical elements: Silicon, Sulfur, Chlorine, Potassium, Calcium, Titanium, Manganese, Iron, Nickel and Zinc. Correlations were observed between some elements making it possible to identify possible sources of pollution.

Multielement analysis in beer cans using X-ray fluorescence

In this study the elemental concentrations of twenty-three beer cans of different brands and nationalities were determined using X-ray fluorescence technique. Beer cans from Brazil (20 beer cans), Germany, the United Kingdom and Colombia were analyzed, totalizing 15 different breweries. It was possible to calculate the concentration of 15 elements in the beer cans samples: Mg, Al, Si, S, Cl, V, Cr, Mn, Fe, Ni, Cu, Zn, Ga, Zr and Pb. The results showed that aluminum concentrations ranged from 94 % to 96 %. Other's elements can be considered trace elements, being the highest concentrations of them for Mg (approximately 2%) and Mn (approximately 1%). Some elements showed differences between cans from different nationalities, with Zn being much higher in samples from Brazil. The Zr element showed similarities between German and UK beer cans. In addition, the beer can sample from Colombian had lower concentrations of Cl and Ga. This study shows that the values found are comparable to those found in the literature and that the concentrations of some trace elements in beer cans may represent signs of impurities brought during the recycling process.

Using X‐ray fluorescence to examine ancient Maya granite ground stone in Belize

AbstractWhile ubiquitous among ancient Maya sites in Mesoamerica, archaeological analysts frequently overlook the interpretive potential of ground stone tools. The ancient Maya often made these heavy, bulky tools of coarse‐grained, heterogeneous materials that are difficult to chemically source, unlike obsidian. This paper describes an application of handheld, energy‐dispersive X‐ray fluorescence (XRF) to provenance ground stone artifacts (tools and architectural blocks) composed of granite: a nonhomogenous, phaneritic stone. We present a multicomponent methodology that independently tested whole‐rock, thin‐sectioned, and powdered samples by petrographic microscope, conventional, lab‐based XRF, and portable XRF units, which yielded comparable results. After establishing distinct geochemical signatures for the three geographically restricted granite plutons in Belize, we devised a field‐based XRF application on a whole rock that could replicate the compositional readings of lab‐based XRF on powdered materials with sufficient accuracy and reliability. We applied this multishot XRF technique to granite ground stone items from a range of ancient Maya sites throughout Belize; we discuss two specific case studies herein. Our results underscore the widespread potential of multishot XRF applications for determining the provenance of coarse‐grained, heterogeneous rock materials. These results can help push the boundaries from one‐dimensional, functional explanations of ground stone items to their social and ideological dimensions, alongside deeper understandings of granite resource management.

Study of Ni/AlN/Ni waveguide system for 8.05 keV incident energy

Ni/AlN/Ni waveguide system provides intensity enhancement by a factor of ~30 at 8.05 keV photon energy. In the present study, the effect of deviation of structural parameters (thickness of each layer) along with the surface-interface properties on electric field intensity (EFI) inside an ion beam sputter deposited Ni/AlN/Ni waveguide is investigated. EFI calculations are performed using structural parameters obtained from X-ray reflectivity (XRR) measurements performed using Cu-Kα source. Deposited waveguide structure provides intensity enhancement (~26) slightly lower than optimized value (~30). Furthermore, temporal stability of the structure is investigated using combined XRR and grazing incidence X-ray fluorescence (GIXRF) techniques (at 15 keV photon energy) after about 15 months. Some structural changes are observed which, however, do not lead to further decrease in intensity enhancement inside the waveguide, making it suitable for applications at 8.05 keV photon energy.

The Potential Of Acid Mine Drainage Formation At Bukit Besi, Dungun, Terengganu

Acid mine drainage (AMD) at Bukit Besi is often accompanied by high concentrations of various heavy metal such as iron, lead, copper, zink, cadmium, manganese, nikel, and arsenic. The samples were collected from active mining site at Cheng Yu, Bukit Besi. The physical and chemical tests used are ion chromatography (IC) and inductively coupled plasma (ICP) test, toxicity characteristic leaching procedure (TCLP), and clay mineralogy using XRF (X-ray fluorescence) and XRD (X-ray diffraction) techniques. Static test which is acid-base counting are used to predict the potential of AMD. The water analysis showed a very acidic water with pH < 3.5 with high concentration of heavy metals like Fe (822.03 mg/L) and sulfate (4455.87 mg/L). Acid-bases rock calculation shows highly significant results which have high potential of acid production (9.5 to 155.0 kg CaCO3/ton). The results from physical and chemical analysis show Bukit Besi area is potentially exposed to formation of acid mine drainage.

Evaluation of urban tree barks as bioindicators of environmental pollution using the X-ray fluorescence technique

Some chemical elements released in nature due to anthropogenic actions are harmful to living beings, and finding efficient and low-cost ways to measure their presence is a challenge. The major goal of this work was to use the barks of urban trees as bioindicators of the presence of these elements. For this purpose, tree barks of sixteen individual trees were collected, including Ipê (Bignoniaceae Family); Sibipiruna (Fabaceae Family); Pine (Pinaceae Family), in the city of Sorocaba, SP, Brazil, in three different districts. Two samples, one of Ipê and another of Sibipiruna, collected in the Mata Atlântica forest in Juquitiba, SP, Brazil, were used as control samples. They were also analyzed; six soil samples were collected in the same places as the tree barks in Sorocaba. The samples were analyzed using the Energy Dispersion X-Ray Fluorescence Spectroscopy technique. The elements studied ranged from Al to Bi. The results were submitted to univariate and multivariate statistical analysis showing that Sibipiruna presented a high concentration of the element Ca. At the same time, Ipê and Pine showed high concentrations of K. In the identified elements, the probable sources of contamination were pointed out, such as elements from the dust of braking automobiles (Al, Si, S, Ti, Fe, Cu, and Ba), elements from the paint used to paint the asphalt (Si, Ca, Cr and Pb) and elements from the tire tread wear (Al, S, Ca and Zn). From the analysis of soil samples and trees, it was found that there was high pollution by the element Pb in the specimens collected in front of the old Saturnia battery factory, located in the district of Éden in the city of Sorocaba, SP, Brazil (Coordinates: Lat 23K253141 m E; Long 23K7405583 m S).

Predicting cumulative lead (Pb) exposure using the Super Learner algorithm

Chronic lead (Pb) exposure causes long term health effects. While recent exposure can be assessed by measuring blood lead (half-life 30 days), chronic exposures can be assessed by measuring lead in bone (half-life of many years to decades). Bone lead measurements, in turn, have been measured non-invasively in large population-based studies using x-ray fluorescence techniques, but the method remains limited due to technical availability, expense, and the need for licensing radioactive materials used by the instruments. Thus, we developed prediction models for bone lead concentrations using a flexible machine learning approach--Super Learner, which combines the predictions from a set of machine learning algorithms for better prediction performance. The study population included 695 men in the Normative Aging Study, aged 48 years and older, whose bone (patella and tibia) lead concentrations were directly measured using K-shell-X-ray fluorescence. Ten predictors (blood lead, age, education, job type, weight, height, body mass index, waist circumference, cumulative cigarette smoking (pack-year), and smoking status) were selected for patella lead and 11 (the same 10 predictors plus serum phosphorus) for tibia lead using the Boruta algorithm. We implemented Super Learner to predict bone lead concentrations by calculating a weighted combination of predictions from 8 algorithms. In the nested cross-validation, the correlation coefficients between measured and predicted bone lead concentrations were 0.58 for patella lead and 0.52 for tibia lead, which has improved the correlations obtained in previously-published linear regression-based prediction models. We evaluated the applicability of these prediction models to the National Health and Nutrition Examination Survey for the associations between predicted bone lead concentrations and blood pressure, and positive associations were observed. These bone lead prediction models provide reasonable accuracy and can be used to evaluate health effects of cumulative lead exposure in studies where bone lead is not measured.

The New Markers of Early Obesity-Related Organ and Metabolic Abnormalities.

The objective of our study was to identify new markers related to excessive body adiposity and its early consequences. For this purpose we determined serum FGF-19 and FGF-21 concentrations in obese rats, whose role in the pathogenesis of obesity is not yet established. In addition, a total reflection X-ray fluorescence technique was applied to determine the elemental chemistry of certain tissues affected by obesity. Next, the new biochemical and molecular parameters were correlated with well-known obesity-related markers of metabolic abnormalities. Our obese rats were characterized by increased calorie consumption and body adiposity, hypercholesterolemia, elevated levels of liver enzymes and FGF-21, while the level of FGF-19 was reduced. Strong relationships between new hormones and established metabolic parameters were observed. Furthermore, we demonstrated that obesity had the greatest effect on elemental composition in the adipose tissue and liver and that rubidium (Rb) had the highest importance in distinguishing the studied groups of animals. Tissue Rb strongly correlated with both well-known and new markers of obesity. In conclusion, we confirmed serum FGF-19 and FGF-21 as useful new markers of obesity-related metabolic alternations and we robustly propose Rb as a novel indicator of excessive body adiposity and its early consequences. However, further investigations are encouraged to address this clinical issue.

Characterization of PM2.5 in Coastal Urban Area, Northwest Morocco: Seasonal Variations, Elemental Composition and Source Apportionment

Sale, located along the Atlantic Ocean, is the third-largest city in Morocco. The Bouregreg river separates Sale from Rabat (Morocco’s capital city). This City is characterized by a high demographic density. Their main air pollution sources are traffic, ocean, potteries, fishing, domestic heating, and artisanal activities. Ambient PM2.5 particles were collected in an urban area of Sale City (Morocco) from July 2018 to July 2019. The sampling was carried out using a Dichotomous sampler and the Total X-Ray Fluorescence technique (TXRF) was used to evaluate the elemental composition of the collected filters. In this paper, chemical characterization, and source apportionment of PM2.5 were investigated. The results showed that the PM2.5 mass concentrations vary, during the sampling period, from 3.08 µg/m3 to 49.48 µg/m3 with an average of 17.30 µg/m3. The highest values were observed in winter while the lowest in summer. The influence of atmospheric transport scenarios on the levels of PM was carried out using air mass back-trajectories, using the HYSPLIT™ model. This study allowed identifying four main clusters arriving at our receptor site in Sale City: Iberian Coast (24%), Near Atlantic Ocean (33%), Local (28%), and Oceanic (15%). For seasonal variations of metal concentrations, K, Ca, V, Mn, Fe, Ni, Cu, Zn, As, Sr, Ba, and Pb exhibited their highest concentrations during winter while Ti and Cr, their highest concentrations were observed during Autumn. The Enrichment Factor (EF) analysis showed that Ti, Sr, Mn, K, Ca, and Ba are mainly originated from airborne dust with EF < 10, V, Cu, Cr have both natural and anthropogenic sources with 10 < EF < 100, while Ni, Zn, and Pb were mainly from anthropogenic source with EF > 100. Five factors were selected in Positive Matrix Factorization (PMF) model’s analysis: crustal contribution, road dust, brake wear, heavy oil combustion, and exhaust vehicle emissions. Their contributions to PM2.5 were 5%, 53.6%, 20.1%, 14.3% and 7%, respectively. Road dust and vehicle exhaust sources showed the highest contribution in winter; while soil dust, brake wear, and oil combustion sources contributed the most in summer. The present study could be considered as the first source apportionment study on PM2.5 fractions carried out in Sale City, Morocco.

ROI-Finder: machine learning to guide region-of-interest scanning for X-ray fluorescence microscopy.

The microscopy research at the Bionanoprobe (currently at beamline 9-ID and later 2-ID after APS-U) of Argonne National Laboratory focuses on applying synchrotron X-ray fluorescence (XRF) techniques to obtain trace elemental mappings of cryogenic biological samples to gain insights about their role in critical biological activities. The elemental mappings and the morphological aspects of the biological samples, in this instance, the bacterium Escherichia coli (E. Coli), also serve as label-free biological fingerprints to identify E. coli cells that have been treated differently. The key limitations of achieving good identification performance are the extraction of cells from raw XRF measurements via binary conversion, definition of features, noise floor and proportion of cells treated differently in the measurement. Automating cell extraction from raw XRF measurements across different types of chemical treatment and the implementation of machine-learning models to distinguish cells from the background and their differing treatments are described. Principal components are calculated from domain knowledge specific features and clustered to distinguish healthy and poisoned cells from the background without manual annotation. The cells are ranked via fuzzy clustering to recommend regions of interest for automated experimentation. The effects of dwell time and the amount of data required on the usability of the software are also discussed.

Combined Focused Ion Beam – Scanning Electron Microscope and Synchrotron X-ray Fluorescence analysis of multi-solid and melt inclusions from the super-giant Grasberg Cu[sbnd]Au deposit, Indonesia

Previous studies of the mineralised quartz veins from the Grasberg CuAu deposit in Indonesia have shown that they contain multi-solid inclusions and silicate melt inclusions. The multi-solid inclusions exhibit salinities up to 75 wt% NaCl equiv. and ultrahigh homogenisation (Vapour + Liquid + Solid → Liquid) temperatures, up to 1281 °C, but the processes leading to their formation are poorly understood. To determine the composition of these inclusions they were analysed by Focused Ion Beam – Scanning Electron Microscope (FIB-SEM) and Synchrotron X-ray Fluorescence (SXRF) techniques. FIB-SEM analysis of two representative multi-solid inclusions (MSI) showed that they contain a large halite and a smaller sylvite crystal and mixed KFe chloride crystals. K-feldspar crystals occurring inside and outside the multi-solid inclusions indicate that they were trapped from a melt phase. The ore-mineral chalcopyrite was also identified in one inclusion. Opening the multi-solid inclusions under vacuum resulted in a coating enriched in Na, K, Fe and Cl that precipitated on the crystals and walls of the inclusions. FIB-SEM analysis of a coexisting silicate melt inclusion showed that it consisted mainly of a devitrified glass with approximately K-feldspar composition that also contained small crystals of iron oxide. Further milling of the melt inclusion exposed a CuFe-rich silicate mineral. SXRF analysis of another multi-solid inclusion indicated that Br and Zn occur in the aqueous phase whereas K, Ca, Fe, Pb and Mn are hosted by solid phases within the inclusion.Modelling of mineralisation processes demonstrate that a supercritical, intermediate density fluid (with ~5 wt% NaCl) underwent an initial pressure drop causing phase separation and the formation of a vapour-rich fluid and a small fraction of brine, which led to the formation of salt hydrates, salt melts or both within the MSI. The coexistence of silicate melt inclusions and the occurrence of hematite and, K-feldspar in MSI suggest that a coeval silicate melt is also associated with mineralisation at the Grasberg deposit. The high salinity, multi-solid inclusions and melt inclusions form early in the vein paragenesis and record the origin and initial processes of ore deposition. Furthermore, the high metal-bearing capacity of salt melts suggests that the observation of coexisting silicate and salt melts may indicate the presence of a fertile mineral system.

Toxic Metals in Some Decorative Cosmetics and Nail Products

Cosmetic marketing is one of the most profitable and fast increasing markets in Kurdistan Region of Iraq. In recent years, the use of cosmetics has witnessed a rapid increase, especially with the emergence of social media and its impact on this trade. The market is full of different cosmetic brands and nail products. Moderate and low-quality brands of cosmetic samples that available in the local markets were selected to investigate their heavy metals and chemical composition. Samples from face foundation, eye shadow, and nail polish products were taken and examined to evaluate the concentration of metals, that is, Hg, Pb, Cd, As, Mn, Cr, Ni, Co, Fe, Zn, Cu, and Al ions, using X-ray diffraction and X-ray fluorescence techniques. The examination results show high concentrations of Fe and Al metals in the lipstick samples whereas the Hg, Cd, Cr, and Ni were out of detection limit. Moreover, the results show contamination of Hg heavy metal in one of the examined nail polishes brands, whereas the rest of foundation and eye shadow samples show a higher concentration of Al and Fe. Curcumin, as a natural bio-friendly chelate, has been used to deplete metal ions using ultraviolet-visible Spectrophotometer.

Screening of Soybean, Common Bean and Maize on Nickeliferous Soils from Mafic Rocks

In this study, nickeliferous soils' effects on grain legume and cereal growth as well as their potential to accumulate nickel and related micronutrients were examined. A completely randomized block design with six repetitions was set up. Samples were collected from eight points and the experiment was conducted for six weeks at the University of Man. In order to fill a plastic container, eight soil samples were used. The soil humidity was controlled with SONKIR MS02 multimeter. Common bean (Phaseolus vulgaris), soybean (Glycine max), and maize (Zea mays) were the test plants. Each soil sample was air dried and sieved with a 2 μm mesh. The X-ray fluorescence (XRF) technique was used to carry out a chemical analysis. Statistica 7.1 was used to conduct statistical analysis like the ANOVA and correlation test. At Moyango, the soil was developed on dunite. The soil had a colour varying from 7.5YR6/2 to 10YR5/6.). The dominant oxides found were Fe2O3, SiO2, and P2O5 with wt% > 7. The soil Ni was negatively correlated with K, Ca and, V. The soils had significant effect on soybean, common bean, and maize growth. However, the negative effect was more on common bean. The lowest soybean plant’s heights were observed on plant grown on soil from the mining site. The soil had a significant effect on soybean Ni, V, Mn, and Co content. Soybean plant Ni contents were 9.20 and 7.31 wt%, respectively from plants grown on soils M1 and M2. The content of Ni in soil had significant effect on plant growth, specifically it has reduced the height of grain legumes. From the results observed, maize should be the one most suitable for cultivation in the vicinity of the Ni mining region of Foungouesso-Moyango. Further investigation is needed with more test plants to prevent population health.

Multimodal X-ray nano-spectromicroscopy analysis of chemically heterogeneous systems.

Understanding the nanoscale chemical speciation of heterogeneous systems in their native environment is critical for several disciplines such as life and environmental sciences, biogeochemistry, and materials science. Synchrotron-based X-ray spectromicroscopy tools are widely used to understand the chemistry and morphology of complex material systems owing to their high penetration depth and sensitivity. The multidimensional (4D+) structure of spectromicroscopy data poses visualization and data-reduction challenges. This paper reports the strategies for the visualization and analysis of spectromicroscopy data. We created a new graphical user interface and data analysis platform named XMIDAS (X-ray multimodal image data analysis software) to visualize spectromicroscopy data from both image and spectrum representations. The interactive data analysis toolkit combined conventional analysis methods with well-established machine learning classification algorithms (e.g. nonnegative matrix factorization) for data reduction. The data visualization and analysis methodologies were then defined and optimized using a model particle aggregate with known chemical composition. Nanoprobe-based X-ray fluorescence (nano-XRF) and X-ray absorption near edge structure (nano-XANES) spectromicroscopy techniques were used to probe elemental and chemical state information of the aggregate sample. We illustrated the complete chemical speciation methodology of the model particle by using XMIDAS. Next, we demonstrated the application of this approach in detecting and characterizing nanoparticles associated with alveolar macrophages. Our multimodal approach combining nano-XRF, nano-XANES, and differential phase-contrast imaging efficiently visualizes the chemistry of localized nanostructure with the morphology. We believe that the optimized data-reduction strategies and tool development will facilitate the analysis of complex biological and environmental samples using X-ray spectromicroscopy techniques.